Pressure sensitive adhesives containing polymeric surface-modified nanoparticles

FIELD: chemistry.

SUBSTANCE: invention relates to pressure sensitive adhesives, suitable for use on a wide variety of substrates, including both high surface energy and low surface energy substrates. Pressure sensitive adhesives comprise an acrylate polymer and surface-modified nanoparticles. The surface-modified nanoparticles comprise a nanoparticle comprising a silica surface and surface modifying groups, covalently bonded to the silica surface of the nanoparticle. At least one surface modifying group is a polymeric silane surface modifying group. At least one surface modifying group is a non-polymeric silane surface modifying group.

EFFECT: disclosure also provides a method of preparing pressure sensitive adhesives, including exposing them to UVA and UVC radiation.

21 cl, 2 dwg, 12 tbl

 

SCOPE

[0001] the Present disclosure relates to curable pressure adhesives containing surface-modified nanoparticles with a polymeric silane surface-modifying substances.

Summary of the INVENTION

[0002] Briefly, on the one hand, the present disclosure provides a curable pressure adhesive containing an acrylic polymer and surface-modified nanoparticles. Surface-modified nanoparticles include nanoparticles comprising silicon surface, the polymer silonovoy surface-modifying group, and the polymer silonovoy surface-modifying group. Both silane surface-modifying group, polymer and a polymer covalently linked to the silicon surface of the nanoparticle.

[0003] In some embodiments, the acrylate polymer comprises the reaction product of one or more methacrylate monomers, and at least one monomer vinylcarbazole acid. In some embodiments, the polymeric silane surface modifying group consisting of methacrylate repeating units. In some embodiments, the polymeric silane surface modifying group has a repeating unit vinylcarbazole acid.

[0004] In some embodiments, the polymeric silane surface-mo�oficerowie group consists of, at least one of dialkoxy alkyl silane and dialkoxy aryl silane. In some embodiments, the ratio of the molar percent of the polymeric surface-modifying substance to the polymeric surface-modifying substance is between 95:5 and 50:50, e.g., between 80:20 and 60:40, inclusive.

[0005] In some embodiments, polymeric surface-modifying substance has a functional group capable of forming cross-links with the acrylate polymer. In some embodiments, cured under pressure adhesive has a composition and a curing agent and/or tackifiers.

[0006] on the other hand, the present disclosure provides a method of producing cured under pressure adhesive, consisting of treatment of the mixture of the first methacrylate monomer, vinylcarbazole acid, the first photocatalyst and the surface-modified nanoparticles of ultraviolet radiation in spectrum "A" is sufficient for partial polymerization of the first methacrylate monomer and vinylcarbazole acid with the formation of the partially polymerized mixture, add the hardener and the second photocatalyst to the partially polymerized mixture to form a coating, the coating on a substrate, and exposure of the substrate to ultraviolet radiation in spectrum "A" for the formation of glue, utverjdaemogo� under pressure. In some embodiments, the method consists of exposure to ultraviolet radiation spectrum for curing under pressure adhesive for the purpose of binding the polymeric surface-modifying substance with an acrylate polymer.

[0007] the above summary of the present disclosure are not intended to describe each variant of the present invention. The details of one or more examples of the invention are also described in this description below. Other features, objects and advantages of the present invention will be clearly listed in the description and claims.

BRIEF description of the DRAWINGS

[0008] FIG. 1 shows a histogram showing the performance of exfoliation of the adhesive compositions of the set of data N from the stainless steel substrate with high surface energy. [0009] FIG. 2 shows a histogram showing the performance of exfoliation of the adhesive compositions of the set of data N from polypropylene substrates with low surface energy.

DETAILED DESCRIPTION

[0010] typically, the adhesive compositions, e.g., adhesives, curing under pressure (CODE), including acrylic adhesives, are widely known. It is also known the use of additives to modify the properties of adhesive compositions, such as tackifiers, plasticizers and fillers. However, despite the fact that the individual components f�of raly adhesive composition may be known, the choice of specific combinations of components and their relative amounts with the objective of achieving specific requirements necessary for the end user, remains a challenge.

[0011] Also known is the use of surface-modified nanoparticles in resins, including thermosetting resins. It was assumed that surface-modified nanoparticles may be embedded in CODE. However, like any other potential additives, the choice of specific nanoparticles, surface-modifying substances and their amounts, as well as formulation development of such surface-modified nanoparticles in the adhesive composition remains a challenge.

[0012] One problem faced by the developers of adhesive compositions, is the desire to create a solid cured under pressure adhesive for use on a wide range of substrates, including substrates with high surface energy and substrate with low surface energy. Generally, substrates with low surface energy is defined as a substrate having a surface energy less than 37 Dyne/cm, such as polypropylene and polyethylene (e.g., the high-density polyethylene). Generally, substrates with high surface energy is defined as a substrate having a surface energy of more than 37 Dyne/cm, e.g., more than 200 �ina/cm, including, e.g., aluminum, glass and stainless steel.

[0013] in Addition to improving strength with a wide range of substrates, the formulator of adhesive compositions must also take into account the influence of other properties of the adhesive composition, such as grip strength. Grip strength is often measured by determining the strength of the adhesive in shear. For example, the addition of tackifiers can increase the adhesion (e.g., pull strength), but often weakens the force of adhesion (e.g., the shear strength).

[0014] In General, the present disclosure describes cured under pressure adhesive compositions consisting of silica nanoparticles surface modified with a polymer, a chemically active or inactive Milanovich functional groups. Surface-modified nanoparticles dispersed in acrylic adhesive composition.

[0015] typically, the acrylic adhesive composition comprises an acrylic polymer consisting of the reaction product mixture of the first methacrylate monomer and vinylcarbazole acid. As used herein, the term "methacrylate" refers to acrylate or methacrylate. For example, the term "butylmethacrylate" refers to acrylate or butylmethacrylate. In some embodiments, the mixture may also contain a crosslinking agent.

[0016] the Alkyl group of the first meta�of relata contains from 4 to 18 carbon atoms. In some embodiments, the alkyl group contains at least 5 carbon atoms. In some embodiments, the alkyl group contains not more than 8 carbon atoms. In some embodiments, the alkyl group of the first methacrylate contains eight carbon atoms, e.g., isooctylphenyl and/or diethylhexylphthalate.

[0017] Examples vinylcarbazole acids that can be used in some embodiments of the present disclosure, include acrylic acid, methacrylic acid, taconova acid, maleic acid, fumaric acid and beta-carboxymethylcel.

[0018] In some embodiments, the acrylic copolymers of the present disclosure contain at least 2 percent by weight, and in some embodiments not less than 3 mass percent vinylcarbazole acid of the total weight of alkyl methacrylates and vinylcarbazole acids. In some embodiments, the acrylic polymer contains not more than 10 mass percent, and in some embodiments, not more than 8 mass%, and, in some embodiments, not more than 5 mass percent vinylcarbazole acid. In some embodiments, the acrylic polymer contains no more than 3-5 percent by weight, inclusive, vinylcarbazole acid, of the total weight of alkyl methacrylates and vinylcarbazole acids. In General, acrylic adhesive compositions containing such high levels vinylcarbazole� acid, considered capable of adhesion to the substrates with high surface energy, such as, e.g., stainless steel.

[0019] In some embodiments, the acrylic copolymers of the present disclosure contain less than 2 percent by weight, e.g., less than 1 mass%, vinylcarbazole acid, of the total weight of alkyl methacrylates and vinylcarbazole acids. In some embodiments, the acrylic copolymer contains not more than 0.3-1.5 mass%, e.g., from 0.5 to 1 mass%, inclusive, vinylcarbazole acid, of the total weight of alkyl methacrylates and vinylcarbazole acids.

[0020] In some embodiments, the mixture may contain one or more additional monomers, including one or more additional alkyl methacrylates. In some embodiments, an alkyl group of at least one alkyl methacrylate containing not more than 4 carbon atoms. In some embodiments, an alkyl group of at least one alkyl methacrylate containing 4 carbon atoms, e.g., butylmethacrylate. In some embodiments, an alkyl group of at least one alkyl methacrylate contains 1-2 carbon atoms, e.g., methyl and/or ethyl.

[0021] In some embodiments, can be used non-polar alkyl methacrylate. As used herein, non-polar monomer is a monomer whose homopolymer has a par�meter solubility, measured by way of Federal not exceeding 10.50. The use of non-polar monomer improves the adhesion of the surface with low energy with the glue. It also improves the structural properties of the adhesive composition (e.g., force of adhesion). Examples of suitable non-polar monomers and the solubility parameter for Faders ((cal./cm3)1/2include 3,3,5 cyclohexyl acrylate (9.35), trimethylcyclohexyl acrylate (10.16), isobornyl acrylate (9.71), N-octyl acrylamide (10.33), butyl (9.77) and their combinations.

[0022] Photopolymerized composition may contain a curing agent for the expansion of the forces of adhesion of the resulting adhesive substances or articles. Suitable hardeners include hydrogen outlet CARBONYLS such as anthraquinone and diphenylmethan, and their derivatives, as disclosed in U.S. patent No. 4181752, and multifunctional acrylates such as 1,6-hexandiol diacrylate, the trimethylolpropane triacrylate and 1,2-propylene glycol diacrylate and acrylates are disclosed in U.S. patent No. 4379201. Other suitable curing monomers include polymeric multifunctional methacrylates, eg.. the polyethylene oxide diacrylate or a polyethylene oxide dimethacrylate; polyvinyl hardeners, such as substituted or unsubstituted divinylbenzene; and difunctional urethane acrylates such as "EBECRYL" 270 and "EBECRYL" 230 (ur�anew acrylates with an average molecular weight, accordingly, in the 1500 and 5000, supplied by UCB from G. Smyrna, GA), and combinations thereof. Suitable hardeners, also playing the role of photocatalysts are replaced by the chromophore halomethyl-C-triazine disclosed in U.S. patents Nos. 430590 and 4329384.

[0023] In some embodiments, the CODE of the present disclosure may have the General composition additives, such as tackifiers and plasticizers. Typically, plasticizers are materials that are compatible with the acrylic copolymer to which they are added, and having a glass transition temperature (TC) exceeding Those of acrylic copolymer. On the contrary, a plasticizer compatible with the acrylic copolymer, but has a lower TC TC acrylic copolymer. Despite the fact that the actual Vehicle varies depending on the formulation of an acrylic copolymer, usually TC acrylic copolymer does not exceed -20°C, e.g., less than -30°C, less than -40°C, or even below -50°C.

[0024] In some embodiments, the adhesive compositions of the present disclosure include at least one plasticizer. Examples of plasticizers with high Those include terpenes, alifaticheskii - or aromatic-modified hydrocarbon, C5-C9, and esters of rosin. Examples of plasticizers with low include Those serpentinely resins, terpenes, alifaticheskii - or aromatic-modified hydrocarbon, C5-C9, and the ether� rosin.

[0025] typically, the adhesive compositions of the present disclosure are vulcanized by using actinic radiation, e.g., ultraviolet light (UV). In some embodiments, can be used the UV radiation spectrum. In some embodiments, the UV radiation spectrum "C" can be used alone or in combination (e.g., series) with UV radiation spectrum. As used herein, the UV radiation spectrum "A" refers to actinic radiation having a wavelength of from 320 to 390 mm. As used herein, the UV radiation spectrum "C" refers to actinic radiation having a wavelength of from 250 to 260 mm.

[0026] typically, photocatalytically included in UV-curable formulations. The photocatalysts suitable for use in the present invention include ventinove esters, substituted ventinove ethers, such as benzoin methylether or benzoin isopropylated, substituted acetophenone, such as 2,2-dimethoxy-1,2-diphenylethan-1-he; 2,2,-diethoxy-acetophenone and 2,2-dimethyl-acetophenone; substituted alpha-ketols such as 2-methyl-2-hydroxy propiophenone; aromatic chloride sulfonyl such as 2-naphthalene sulfonyl chloride; photoactive oximes, such as 1-phenyl-1,2-propandiol-2-(0-ethoxycarbonyl)oxime; substituted triazine, and oligomeric photosensitizers, such as� oligomeric 2-hydroxy-2-methyl-1-[4-methylvinyl)phenyl]-1-acetone (available on the market as ESACURE KIP 150" from Sartomer company, Exton, PA), and mixtures thereof. In some embodiments, the preferred photocatalysts include 2,2-dimethoxy-1,2-diphenylethan-1-he (supplied by Ciba Additives under the trademark IRGACURE 651, and Sartomer company, Exton, Pennsylvania, under the name ESACURE KB-1), IRGACURE 184 (Ciba), DAROCUR2959 (Ciba) and DAROCUR 1173 (Ciba).

[0027] the Acrylic adhesive composition of the present disclosure contain surface-modified nanoparticles. As a rule, "surface-modified nanoparticles" means particles from the surface of application, attached to the surface at the nanometer level basis. In some embodiments, the framework is essentially spherical. In some embodiments, the basics are relatively similar in the primary particle size. In some embodiments, the basics have constrained the distribution of particle size. In some embodiments, the base is almost completely compressed. In some embodiments, the base amorphous. In some embodiments, the base esotropia. In some embodiments, the particles are, largely, not agglomerated. In some embodiments, the particles are, to a large extent, not connected, unlike, for example, fumed or colloidal silicon dioxide.

[0028] As used herein, the term "agglomerated" is a description of a weak Association of primary particles, usually held�x them together by charge or polarity. Agglomerated particles can usually be broken down into smaller structures by, for example, the shear stresses that occur during the dispersion of agglomerated particles in a liquid.

[0029] In General, the terms "United" or "connections" are the description of the strong connection of primary particles often bound together by, for example, residual chemical treatment, covalent chemical bonds, or ionic chemical bonds. Further destruction of the joints on the smaller patterns it is very hard to achieve. United particles, as a rule, don't break up into smaller structures by, for example, the shear stresses that occur during the dispersion of agglomerated particles in a liquid.

[0030] As used herein, the term "silicon nanoparticle" refers to a nanoparticle that is attached to the silicon surface at the nanometer level basis. This includes the basics of the nanoparticles mainly composed of silicon, and the basis of nanoparticles containing other inorganic (e.g., metal oxides) or organic bases having a silicon surface. In some examples, the base consists of metal oxide. Can be used any known metal oxide. Examples of metal oxides include the oxides of silicon, titanium, aluminum, zirconium, vanadium, chromium, antimony, zinc, oxide�, eriya, and mixtures thereof. In some embodiments, the base consists of a nonmetal oxide.

[0031] typically, the silicon nanoparticles have an average diameter bases less than 200 nm, e.g., less than 100 nm. In some embodiments, the silicon nanoparticles have an average diameter of not less than 5 nm, e.g., not less than 10 nm. In some embodiments, the silicon nanoparticles have an average diameter of the basics from 50 to 100 nm inclusive. In some embodiments, the silicon nanoparticles have an average diameter of bases 10 to 30 nm, inclusive.

[0032] Despite the possibility of using other methods, such as titration and light scattering, the particle size is related to the present paper, based on transmission electron microscopy (TEM). Using this technology, which collected THE images of the nanoparticles and to determine the size of each particle was used for image analysis. After this was determined, the distribution of particle size based on account, by counting the number of particles having a size falling in each of the predefined number of discrete ranges of particle sizes. After that, it was calculated the particle size. One such method is described in the Provisional application U.S. 61/303,406 ("Polymodal dispersion of nanoparticles", Thunhorst, etc.), filed February 11, 2010, and referred to herein as a "Procedure translucent� electron microscopy".

[0033] the Procedure for transmission electron microscopy. To measure particle size and size distribution of particles, a colloidal solution of nanoparticles dissolved by taking 1 or 2 drops of colloidal solution and its mixing with 20 ml of deionized distilled water. Dissolved samples were treated with ultrasound (ultrasonic cleaner, Mettler Electronics Corp., Anaheim, California) for 10 minutes, and a drop of diluted sample was placed on a copper TEM grid with a cell in 200 mesh together with the carbon / farmerboy film (Product 01801, company Ted Pella, Inc. Redding, California), and dried under atmospheric conditions.

[0034] the Dried samples were photographed using a transmission electron microscope (TEM) (HITACHI H-9000NAR, Hitachi, Ltd., Tokyo, Japan) at a voltage of 300 kV with magnifications in the range from 10 to 50 thousand times thousand times, depending on the size of the particles in each sample. The pictures were taken using the "Gatan Digital Micrograph" and a camera with a CCD (894 ULTRASCAN, the company Gatan, Inc., Pleasanton, CA). Each sample has a calibrated scale mark.

[0035] the particle Size was measured using a single line through the center of each particle, thus, the measurement is based on the assumption that the particles are spherical. If a particular particle was not spherical, Lee�Oia measurements were carried out using the longest axis of the particle. In each case, the number of measurements performed on individual particles, has exceeded the preset value in the test procedure ASTM E122 standard of error of 5 nm.

[0036] Kushina on the market for silicon dioxide include supply companies Naico Chemical Company, NAPERVILLE, Il (for example, NALCO 1040, 1042, 1050, 1060, 2326, 2327 and 2329); Nissan Chemical America Company, Houston, Texas (e.g., SNOWTEX-ZL, -OL, -O, -N, -C, -20L, -40, and -50); Admatechs Co., Ltd., Japan (for example, SX009-MIE, SX009-MIF, SC1050-MJM, and SC1050-MLV); Grace GmbH & Co. KG, worms, Germany (e.g., products under the designation LUDOX, e.g., P-W50, P-W30, P-X30, P-T40 and P-T40AS); Akzo Nobel Chemicals GmbH, Leverkusen, Germany (e.g., products under the designation LEVASIL, eg., 50/50%, 100/45%, 200/30%, 200A/30%, 200/40%, 200A/40%, 300/30% and 500/15%; and Bayer Materialscience AG, Leverkusen, Germany (e.g., products under the name DISPERCOLL S (e.g., 5005, 4510, 4020 and 3030).

[0037] the Nanoparticles used in the present disclosure, have the treated surface. As a rule, substances for surface treatment of the silicon nanoparticles are organic in nature, with a first functional group capable of covalent chemical compound with the surface of the nanoparticles, wherein the substance attached surface treatment that modifies one or more properties of the nanoparticle.

[0038] the Substance surface treatment often include more than one functional group capable of coupling with the surface of the nanoparticles. For example, al�hydroxy groups are shared by the first functional groups, capable of reaction with the free silanol groups on the surface of silicon nanoparticles, forming a covalent bond between the substance surface treatment and the surface of silicon dioxide. Examples of substances surface treatment having multiple alkoxy groups include tralkoxydim (e.g., isooctyl trimethoxysilane). In some embodiments, the substances of surface treatment have no more than three functional groups for coupling with the base.

[0039] In some embodiments, the substance surface treatment also includes one or more additional functional groups, providing one or more additional required properties. For example, in some embodiments, the additional functional group can be selected to provide the required degree of compatibility between the surface-modified nanoparticles and one or more additional components of the resin system, e.g., one or more curable resins and/or active diluents. In some embodiments, the additional functional group can be selected to modify the rheology of the resin system, e.g., increasing or decreasing the viscosity, or ensure non-Newtonian rheological characteristics, e.g., thixotropy (shear thinning).

[0040] In some�, where, options, at least part of the surface-modified nanoparticles can be reactive. Thus, at least some of the surface-modified nanoparticles of at least one of the materials of surface treatment used to modify the nanoparticles comprises a second functional group capable of interacting, e.g., the formation of cross-links, with one or more materials in the composition of the formulation adhesive cured under pressure.

[0041] In the adhesive compositions of the present disclosure, at least it changes the surface of the nanoparticles is not polymeric. Typically, the polymer material surface treatment does not have any polymerized or polymerized with repetitive elements. In some embodiments, the polymer material surface treatment have a molecular weight of less than 1500 g/mol, e.g., less than 1000 g/mol, e.g., less than 500 g/mol. Examples of polymeric substances of surface treatment include dialkoxy alkyl silanes (e.g., isooctyl trimethoxysilane) and dialkoxy aryl silanes.

[0042] In addition to the polymer material surface treatment, surface-modified nanoparticles are modified with at least one polymer material surface treatment.

As a rule, "polymer surface-modify�group" consists of polymerized or copolymerizing recurring items. As used herein, the term "polymeric surface-modifying group" refers to both groups of the polymer surface with a lower molecular weight having from 2 to 20 repeating elements and the polymeric surface-modifying groups with higher molecular weight, having 21 or more repetitive elements.

[0043] In some embodiments, polymeric surface-modifying substance is less than 10 repetitive elements, e.g., 5-9 repetitive elements, inclusive. In some embodiments, polymeric surface-modifying substance is at least 10 duplicate items. In some embodiments, the polymeric substance change surface has at least 10 to 20 repetitive elements, inclusive. In some embodiments, polymeric surface-modifying substance has at least 100 repetitive elements, e.g., from 100 to 200 repeating elements, inclusive. In some embodiments, polymeric surface-modifying substance has no more than 500 repeated elements, e.g., 300 duplicate items, or even not more than 200 duplicate elements.

[0044] In some embodiments, polymeric surface-modifying groups have the molecular weight of at least 500 g/mol, e.g., at least 100 g/mol, eg., at least 1500 g/mol, e.g., not less than 2000 g/mol, or even at least 2500 g/mol. In some embodiments, the molecular weight of the polymeric surface-modifying group can be up to 30000 g/mol, or even 50000 g/mol. However, in some embodiments, the molecular weight of the polymeric surface-modifying group may be not more than 30000 g/mol, e.g., not more than 10,000 g/mole, or even no more than 6000 g/mol. For polymeric surface-modifying substance, the molecular weight is calculated as described in the present document, the order of Calculation Molecular Weight Polymeric Silane.

[0045] In some embodiments, one or more polymeric substances changes the surface can be reactive. That is, polymeric surface-modifying substance comprises a functional group which reacts, e.g., forms a cross connection with the acrylate copolymer. In some embodiments, the functional group contains a group that produce hydrogen. In some embodiments, the group that produce hydrogen, contains benzophenone.

[0046] In some embodiments, acrylate copolymer, and polymeric surface-modifying group contains at least one methacrylate and at least one vinylcarbazole acid. In some embodiments, a component of the�options acrylate adhesive polymer and surface-modifying substances are similar, i.e. they contain similar methacrylate monomer (monomers) and vinylcarbazole acid (acid). In some embodiments, acrylate adhesive and polymer substance change surface may have different components. For example, in some embodiments, the acrylate polymer or polymer substance change surface may include different or additional methacrylate monomer (monomers), e.g., not polar methacrylate.

[0047] Regardless of whether similar or different methacrylate monomers and/or vinylcarbazole acid, in some embodiments, the mass percentage of vinylcarbene in each component may be the same or different. For example, in some embodiments, the acrylate polymer contains WAPmass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid monomers and methacrylate acrylate polymer, and a polymeric silane surface modifying group contains WOSmass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid monomers and methacrylate acrylate polymer is a polymer silonovoy surface-modifying group.

[0048] In some embodiments, the ratio of WOS/WAPis between 0.8 and 1.2, inclusive. For such systems, in which W OS/WAPclose to 1, the polymeric surface-modifying substance is likely to be compatible with the acrylate polymer. In some embodiments, the ratio of WOS/WAPless than 0.5 or more than 2, e.g., less than 0.2 or more than 5, or even less than 0.1 or higher than 10. For such systems, in which the ratio of WOS/WAPfar from 1, the polymeric surface-modifying substance is likely to be less compatible with the acrylate polymer. Of course, the degree of compatibility or incompatibility depends on other factors, such as the identity between the methacrylate monomers used in the acrylate polymer and the polymeric silane, and the difference in their respective content vinylcarbazole acid.

[0049] Examples

isobutylacetate
Table 1
Description of materials used in the preparation of examples
ComponentDescriptionSource
AAacrylic acid
IOAisooctadecyl
IBOA
BAn-butyl acrylate
1-6512,2-dimethoxy-2-phenylacetophenone (photosensitizer IRGACURE 651)CIBA Corporation Tarrytown, NY
1-1841-hydroxycyclohexyl benzophenone, (photosensitizer IRGACURE 184)CIBA Corporation Tarrytown, NY
VAZO 672,2'-azobis(2-methylbutyronitrile), (thermal catalyst of free radicals VAZO 67)E. I. du Pont de Nemours and Company, Wilmington. Delaware
F85glycerine ester of hydrogenated rosin (tackifiers FORAL 85)Hercules Incorporated, Wilmington, Delaware
R6108Hydrocarbon resins (tackifiers REGALREZ 6108)Eastman Chemical Company, Kingsport, Tennessee
SNP-75Aqueous colloidal Sol of silicic acid (40,0% solids) with an average particle size of 75 nanometers (nm) (NALCO 2329)Nalco ompany of Naperville, Illinois
SNP-20Aqueous colloidal Sol of silicic acid (41,1% solids) with an average particle size of 20 nanometers (nm) (NALCO 2327)Nalco Company of Naperville, Illinois
IOTMSIsooctylmercaptoacetate
MPTMS(3-mercaptopropyl) trimethoxysilane (MPTMS, the agent transfer chain)Aldrich Chemical Company, Inc., Milwaukee, Wisconsin
1M2P1-methoxy-2-propanol
ABPAlloxanthine, copolymerizing benzophenones hardener.
TRZ2,4-bis(trichloromethyl)-6-6(4-methoxyphenyl)-SIM-triazine, hardener

[0050] test Methods

[0051] the Procedure for testing the strength of the peel. Peel resistance at 90° of the sample film from stainless steel (HC), polypropylene (PP) or high density polyethylene (HDPE) was measured in the following manner that substantially conforms to the test procedure described in method F (Ed. 05/07) �peeling resistance of the adhesive tape, pressure sensitive" Council on adhesive tape, pressure sensitive PSTC-101. The test was conducted at a temperature of 23°C (73°F) and a relative humidity of 50% (RH).

[0052] the Sample tape with adhesive transfer was cut off at about 1.27 cm wide and about 20 cm in length with the drill samples. Cut the sample was applied with its adhesive side facing down and in length on the surface of the measuring panel length of 12.5 cm and a width of 5 cm was Applied the sample was smoothed on a test panel using a light pressing thumb and cut along the panel. The antiadhesive material was carefully separated to open the other side of the adhesive layer. A strip of aluminum foil width 1,59 cm, length about 20 cm and a thickness of 50 micrometers was located in the center of the adhesive layer along the open on the test panel, completely covering the opened adhesive layer, with the rest of the length as the length from one edge of the test panel. Test panel with an aluminum plate on the adhesive layer was double-laminated rubber roller weighing 2 kg at a rate of 61 cm/min.

[0053] For the 15-minute results, the samples subsequently were in a state of equilibrium within 15 minutes at a temperature of 23°C and a relative humidity of 50%. For a 72-hour results, the samples subsequently were compiled�anii equilibrium within 72 hours at 23°C and a relative humidity of 50%.

[0054] After equilibration, the samples were placed in a test fixture a test of strength on peeling angle of 90° (or test device shear/peeling. Model 3M90, purchased from Instrumentors, Incorporated, Strongsville, Ohio; or the device for tensile testing INSTRON Model 4465, purchased from INSTRON, Norwood, mA). The protruding portion of the aluminum foil was fixed in the clamps of the tester adhesion and peeling resistance was measured at a speed of exfoliation at 30.5 cm/min. Was evaluated by at least two test samples with the results obtained in ounce-force/inch, which were used to calculate the average efforts of exfoliation. It was converted to Newtons per decimeter (N/DM).

[0055] the Procedure for the verification of shear strength."Time shear strength", a measure of the ability of pressure sensitive tape to remain adhered to the substrate at an elevated temperature under constant load applied in a direction parallel to the tape surface and the substrate was evaluated as follows, which is broadly in line with the methodology of the tests described in the methodology Council for adhesive tape, pressure sensitive PSTC-107 Ed. 10/30, "shear Strength pressure sensitive adhesive tape". Procedure "B".

[0056] the Sample �patients under stood with adhesive transfer was placed on a flat surface outdoor adhesive layer up. A strip of aluminum foil with a width of 2.54 cm and a length of about 10 cm was applied to the surface of the adhesive layer, speaking at length about 5 cm from the edge of the adhesive surface. The resulting adhesive layer with an aluminum plate was, with the drill samples, cut into test pieces of a width of 1.27 cm and a length of about 10 cm. the Antiadhesive material was carefully separated from the test sample opposite to the aluminum foil, opening the test surface of the adhesive layer. Approximately 3.8 cm long test piece was covered with adhesive side facing down and in length on the surface of a test panel of stainless steel dimensions 7.6 cm in length and 5.1 cm in width, with the remaining length of the test piece projecting beyond one edge of the panel. For cutting the test piece along the length of the test panel in 2.54 cm, was used by the cutting device (Shear pipe shaver, if a Device Model SCF-100 purchased from Chem Instruments Incorporated, of Fairfield, Ohio). The test sample was double-laminated rubber roller weighing 2 kg at a rate of 61 cm/min. Aluminum hook was fixed on the protruding end of the test piece so that when you dangling on the hook of the weight is evenly distributed over the sample.

[0057] the Test panel with test sample�m and a hook was placed on an adjustable stand with a timer located in such a way that the panel deviated from the vertical by 2 degrees, with protruding downward extremity with a hook angle of 178 degrees to the test panel. Adjustable stand with timer included hanging rack and stop switches associated with the timer. Weight weight of 500 or 1000 grams was neatly hung on the hook, and the timer was set to zero. Adjustable stand with timer was located inside a temperature-controlled at 23°C and a relative humidity of 50%, and in an oven with forced air supply set at 70°C or 149°C. If the weight was falling before the expiration of 10,000 minutes, the time before the fall of the weights recorded in the minutes. For samples whose weight does not fall, and she acted after 10,000 minutes, and the time of shear was observed as 10000+ minutes. "Shearing strength" was calculated as the average between the two test panels and was recorded in minutes.

[0058] the Procedure for determining percent solids. Mass percentage of solids surface-modified nanoparticles in the solution was determined by gravimetric method: the Sample was placed on an aluminum dish and weighed. After drying for 3 hours at a temperature of 120°C, the sample was re-weighted. To calculate the mass percent solids was used for the weight change.

[009] the calculation of the molecular weight of the polymeric silane. The molecular weight of the polymer Milanovich surface-modifying substances was calculated according to the following equation:

Mn=mn*f*I+x*CTA

where Mn = the molecular mass, g/mol; m = mass of the monomer, g;

f = efficiency of the catalyst;

x = the effectiveness of the agent transfer chain (CTA);

n = the number of catalyzing substances per mole of catalyst;

I = moles of catalyst, and

CTA = moles of the agent transfer chain.

[0060] Preparation Milanovich Functional Polymers P1-P7.

[0061] Various silane functional polymers with predetermined molecular weights were prepared as follows: compounds Milanovich functional polymers are shown in Table 2A were prepared by polymerization of a solution in ethyl acetate ("EthAc").

[0062] In a glass bottle were charged monomer (monomers) acrylate and (3-mercaptopropyl) trimethoxysilane. The mixture was diluted with ethyl acetate to 35-40 percent by weight solids and added 0,0385 grams thermal catalyst VAZO 64. The solution was purged with nitrogen for 20 minutes and then closed and placed in a bath with a constant temperature of 6°C with mild stirring for 24 hours. The resulting silane-functional polymers are shown in Table 2b.

Table 2A
The compositions Milanovich functional polymers P1-P7
I. D.IOA (g)IBOA (g)AA (g)BA (g)ABP (g)MPTMS (g)EthAc (g)
P11821.4932
P218-2--0.09932
P318-2-0.0611.4932
P43.34 0.1616.5-1.4932
P53.3416.50.16--1.4932
P616.782.50.8--4.56150
P716.782.50.8--0.71150

Table 2b
Polymeric silane surface-modifying substance P1-P7
RoomMonomersThe mass ratioMM (g/mol)Recurring items (*) Reactivity
P1IOA:AA90:10300017No
P2IOA:AA90:1030,000173No
P3IOA:AA:ABP9010:0.1300017Yes
P4WA:SA:AA82.516.7:0.8300015No
P5IBOA:IOA:AA82.516.7:0.8300012No
P6IBOA:IOA:AA82.516.7:0.8500019No
P7/td> IBOA:IOA:AA82.516.7:0.830,000115No

(*) assessment based on the calculated molecular weight based on the assumed stoichiometric structure of the polymeric surface-modifying substances.

[0063] Preparation of modified nanoparticles (MNP).

[0064] the Nanoparticles of silicon dioxide, modified with the help of Isooctylmercaptoacetate (IOTMS).

[0065] a Series of nanoparticles of silicon dioxide, modified with the help of Isooctylmercaptoacetate, polymeric surface-modifying substance, was prepared as shown in Table 3, in the following manner: the aqueous colloidal Sol of silicic acid (SNP-20 or SNP-75) was dissolved in 1M2P. A solution of IOTMS in 1M2P was slowly added over 20 minutes to the dissolved solutions of nanoparticles of silicon dioxide. The mixture was further diluted with an additional amount of 1M2P, and then heated at 80°C for 24 hours. After disconnecting the source of heating, the reaction mixture was cooled to room temperature. To modified particles was added to the IOA monomer, and the resulting mixture was placed in a vacuum to remove all 1M2P and solvent ethyl acetate. The resulting modificarea�nye nanoparticles were obtained in the range from 25 to 100 percent by weight solids, depending on the remaining amount of monomer IOA. Materials with 100% solids were immediately used to prevent agglomeration. Materials that contain some residual amount of monomer IOA, were used within 1-2 days.

[0066] the Nanoparticles of silicon dioxide, modified with Milanovich Functional Polymers P1-P7.

[0067] a Series of nanoparticles of silicon dioxide, modified through IOTMS and Milanovich functional polymer was prepared as shown in Table 3, in the following manner: the Aqueous colloidal Sol of silicic acid (SNP-20 or SNP-75) was dissolved in 1M2P. The required volume of solution IOTMS diluted in 1M2P, and a solution of silane modified polymer (P1-P7) in ethyl acetate were slowly added over 20 minutes to a previously dissolved solu silicic acid. The resulting mixture was further diluted with an additional amount of 1M2P, and then heated at 80°C for 24 hours. After disconnecting the source of heating, the reaction mixture was cooled to room temperature. To modified particles was added to the IOA monomer, and the resulting mixture was placed in a vacuum to remove all 1M2P and solvent ethyl acetate. The resulting modified nanoparticles were obtained in the range from 25 to 100 percent by weight solids, depending on the remaining volume of the IOA monomer. Materials with 100% solids were immediately used to prevent agglomeration. Materials containing a residual amount of the monomer were used within 1-2 days.

Table 3
Surface-modified nanoparticles of silicon dioxide (SNP 20 and SNP-75)
Room MNP1M2PSNPIOTMSSilane modified polymer
(g)(mm)(g)(G)Molar %Room(g)Molar %
1200201005.97100--0
225020100 4.7880P625.120
312520501.7960P625.140
425020502.3980P787.120
5200751001.41100--0
6200751001.1280P13.620
71007540 0.4580P214.420
87075400.4580P33.020
97075400.4580P43.4320
107075400.4580P53.1320
1120075501.1380P65.9120
122007550 0.8460P611.840
1325075501.1380P741.020

[0068] the Resulting modified nanoparticles were mixed in an acrylic syrup copolymers to obtain compositions curable pressure adhesive properties with high shearing strength and peeling.

[0069] the Procedure for preparation of the CODE.

[0070] Step 1. By mixing acrylate monomer components of the adhesive composition (i.e. itachinaruto (IOA) and acrylic acid (AA), the photocatalyst and the surface-modified nanoparticles (MNP) was prepared partially polymerized mixture. For each sample, the amounts of the monomers are shown in percent by weight, based on the total weight of monomers. Volume IOA includes all residual monomers IOA that are present in the component of surface-modified nanoparticles. Volumes of other components (e.g., catalyst and MNP), shown in mass parts per hundred parts by weight of monomers. Thereafter, the mixture was deactivated by bubbling in gaseous and�PTA within 5 to 15 minutes. Thereafter, an inert mixture was exposed to UV radiation spectrum "A" two 350BL lamps (supplied by Osram Sylvania, Danvers, mA) to create a partially polymerized syrup covering the mixture with a viscosity of about 2000 CPS (cps) (less than 2 minutes). At the moment the syrup was filed with the air to stop the polymerization, leading to formation of a partially polymerized syrup.

[0071] Stage 2. Further, for the purpose of education covering the composition, the partially polymerized syrup were added additional components. For each sample data of the components shown in the mass parts from one hundred parts by weight of the monomers used for preparation of the partially polymerized syrup from Step 1. After that, the mixture was gently shaken or laminated for forming a uniform covering of the whole.

[0072] Step 3. The resulting cover composition was coated on a high release side differential siliconized release substrate of Kraft paper coated with bar notched for the formation of continuous cloth of thickness about 0,051 mm (0.002 inch). Thereafter, the coating was exposed to UV radiation spectrum "A" 350BL lamps (supplied by Osram Sylvania, Danvers, mA) in deactivated nitrogen Atmos�'ere for the formation of vulcanized tape with adhesive anti-adhesive transfer to the substrate. The UV radiation spectrum "A" was measured with a UV radiometer PowerMAP purchased from the company, EIT Incorporated, sterling, VA.

[0073] Step 4. Additionally, in some examples, the resulting tape with adhesive transfer was also exposed to UV radiation spectrum "C" with the use of germicidal lamps with a diameter of 1.6 cm and a power of 20 watts (supplied by Voltarc Technolgies, Inc., Waterbury, Connecticut) is deactivated in a nitrogen atmosphere for education completed tape with adhesive transfer. The UV radiation spectrum "C" was measured with a UV radiometer PowerMAP purchased from the company, EIT Incorporated, sterling, VA.

[0074] the data Set "A". Reference example REF-A1, Examples A1 to A3 and Comparative examples CE-A1 CE-A3. The adhesive substance from the data Set "A" were based on the adhesive composition of 90:10 IOA:AA, including hardener, combined with nanoparticles, modified with the use of compatible, inert polymer ligament (90:10 IOA:AA, 3000 MM). The adhesive compositions were vulcanized only with the help of UV radiation spectrum "A".

[0075] Samples were prepared according to the Procedure of preparation of the CODE. In Step 1, the partially polymerized solution was prepared from 90 mass % to the IOA, 10 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. The type and amount of modified nanoparticles are summarized in Table 4. In Phase 2 were d�Balleny 0.10 parts per hundred hardener TRZ and an additional 0.16 parts per hundred of the photocatalyst (I-651. In Stage 3, the intensity of the UV radiation spectrum "A" was 160 millijoules per square centimeter. Vulcanized-curable pressure adhesives were evaluated at the Time of shearing strength at 149°C to HC with a mass of 1000 g, 15-minute test for peel resistance on HC, and 72-hour test for peel resistance to HC, as described in the above test methods. The results are shown in Table 4.

Table 4
The composition and results for data Set "A"
EXAMPLEMNPResults for stainless steel (HC)
RoomParts per hundredNP:P (*)Shift(+), (min)15 min exfoliation
(N/DM)
72 hours of exfoliation
(N/DM)
REF-A1No014486146
A1MNP-6 580:2010000+98208
A2MNP-61080:2010000+122180
A3MNP-61580:2010000+94160
CE-A1MNP-55100:010000+90209
CE-A2MNP-510100:010000+81218
CE-A3MNP-515100:0530788171
(*) The ratio of the molar percent of the polymeric surface-modifying substances(IOTMS) to polymeric surface-modifying substance.
(+) Shift at 149°C with a load of 1000 g

[0076] As shown in Table 4, the use of compatible, inert surface-modifying substances provided the necessary combination of superior qualities shear at high temperature, 15-minute and 72-hour exfoliation.

[0077] the data Set. Reference example REF-B1, Example B1 and Comparative example CE-B1. The adhesive substance from the data Set "B" were based on the adhesive composition 94:6 IOA:AA, including hardener, combined with nanoparticles, modified with the use of compatible, inert polymer ligament (90:10 IOA:AA). The adhesive compositions were vulcanized only with the help of UV radiation spectrum "A".

[0078] Samples were prepared according to the Procedure of preparation of the CODE. In Step 1, the partially polymerized solution was prepared from 94 mass % IOA, 6 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. The type and amount of modified nanoparticles are summarized in Table 5. In Step 2 were added 0.10 parts per hundred hardener TRZ and an additional 0.16 parts per hundred of the photocatalyst (I-651. In Stage 3, the intensity of the UV radiation spectrum "A" was 160 millijoules per square centimeter. Vulcanized-curable pressure adhesives were evaluated at the Time of shearing strength at 149°C to HC with g�for a mass of 1000 g, The 15-minute test for peel resistance on HC, and 72-hour test for peel resistance to HC, as described in the above test methods. The results are shown in Table 5.

Table 5
The composition and results for data Set "B"
EXAMPLEMNPResults for stainless steel (HC)
RoomParts per hundredNP:P(*)Shift(+), (min)15 min exfoliation (N/DM)72 hours of peeling (N/DM)
REF-B1No07491109
B1MNP-61080:2056179156
CE-B1MNP-510 100:013773153
(*) The ratio of the molar percent of the polymeric surface-modifying substances (IOTMS) to polymeric surface-modifying substance.
(+) Shift at 149°C with a load of 1000 g

[0079] As shown in Table 5, the use of compatible, inert surface-modifying substances provided the necessary combination of superior qualities shear at high temperature, 15-minute and 72-hour exfoliation.

[0080] the data Set "C". Reference example REF-C1, Examples C1-C3 and Comparative examples CE-C1 CE-C3. The adhesive substance from the data Set "C" were based on the adhesive composition of 93.5:6.5 to IOA:AA with tackifiers, including hardener, combined with nanoparticles, modified with the use of a compatible inert polymer ligament (90:10 IOA:AA, 3000 MM for MNP-6 and 30000 MM for MNP-7). The adhesive compositions were vulcanized only with the help of UV radiation spectrum "A".

[0081] Samples were prepared according to the Procedure of preparation of the CODE. In Step 1, the partially polymerized solution was prepared from a mass of 93.5 % IOA, of 6.5 mass % AA and 0,040 parts per hundred of the photocatalyst (I-184. The type and amount of modi�tirovannyh nanoparticles are summarized in Table 6. In Step 2 were added 0.15 parts per hundred hardener TRZ and an additional 0.35 parts per hundred of the photocatalyst (I-184. Phase 2 was also added tackifiers F85 (10 parts per hundred). In Stage 3, the intensity of the UV radiation spectrum "A" was 426 millijoules per square centimeter. Vulcanized-curable pressure adhesives were evaluated at the Time of shearing strength at 23°C and 50% relative humidity at HC with a mass of 1000 g, 15-minute test for peel resistance to HC and HDPE, and 72-hour test for peel resistance to HC and HDPE, as described in the above test methods. The results are shown in Table 6.

Table 6
The composition and results for data Set "C"
EXAMPLEMNPShift (+)Peel (N/DM)
RoomParts per hundredNP:P(*)NS (min)15 min, HC72 hours, HC15 min, HDPE72 �Asa, HDPE
REF-C1No010000+58942527
C1MNP-61080:2010000+661342935
C2MNP-61580:2010000+811202931
C3MNP-71080:2010000+571032939
CE-C1MNP-510100:0689972128 2731
CE-C2MNP-515100:02630771322734
(*) The ratio of the molar percent of the polymeric surface-modifying substances (IOTMS) to polymeric surface - modifying substance.
(+) Shear at 23°C with a load of 1000 g

[0082] As shown in Table 6, compared with nanoparticles, modified only with the help of the polymeric surface-modifying substances (CE-C1 and CE-C2), the use of compatible, inert surface-modifying substances provides an improved 15-minute and 72-hour peeling resistance on substrates with high surface energy (stainless steel), and on substrates with low surface energy (HDPE), without deterioration of shear strength.

[0083] the data Set "D". Reference example REF-D1, Examples D1-D3 and Comparative examples CE-D1 - CE-D3. The adhesive substance from the data Set "D" were based on the adhesive composition of 90:10 IOA:AA, including the hardener. The adhesive compositions contain nanoparticles modified with either a compatible or reactive with a compatible inert polymer linkages. The adhesive compositions were vulcanized by using UV radiation spectrum "A" (Phase 3) and UV spectrum of "C" (Step 4).

[0084] Samples were prepared according to the Procedure of preparation of the CODE. In Step 1, the partially polymerized solution was prepared from 90 mass % to the IOA, 10 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. The type and amount of modified nanoparticles are summarized in Table 7. In Step 2 were added 0.10 parts per hundred hardener TRZ and an additional 0.16 parts per hundred of the photocatalyst (I-651. In Stage 3, the intensity of the UV radiation spectrum "A" was 160 millijoules per square centimeter. In Step 4, the intensity of the UV radiation spectrum "C" was 47 millijoules per square centimeter. Vulcanized-curable pressure adhesives were evaluated at the Time of shearing strength at 149°C to HC with a mass of 1000 g, 15-minute test for peel resistance on HC, and 72-hour test for peel resistance to HC, as described in the above test methods. The results are shown in Table 7.

Table 7
The composition and results for data Set "D"
EXAMPLEMNP Shift (+)Peel (N/DM)
RoomParts per hundredNP:P (*)ReactivityHC (min)15 min, HC72 hours, HC
REF-D1No0-10000+91147
D1MNP-6580:20No10000+69207
D2MNP-61080:20No10000+78197
D3MNP-61580:20No10000+75172
D4MNP-8580:20Yes10000+76199
D5MNP-81080:20Yes10000+73221
D6MNP-81580:20Yes10000+54168
CE-D1MNP-55100:0No10000+84196
CE-D2MNP-510100:0No10000+97201
CE-D3MNP-515100:0 No10000+60205
(*) The ratio of the molar percent of the polymeric surface-modifying substances (IOTMS) to polymeric surface-modifying substance.
(+) Shift at 149°C with a load of 1000 g

[0085] the data Set "E". Reference example REF-E1, Examples E1 and E2 and Comparative example CE-E1. The adhesive substance from the data Set "E" were based on the adhesive composition 94:6 IOA:AA, including the hardener. The adhesive compositions contain nanoparticles modified with either a compatible reactive, or with a compatible inert polymer linkages. The adhesive compositions were vulcanized by using UV radiation spectrum "A" (Phase 3) and UV spectrum of "C" (Step 4).

[0086] Samples were prepared according to the Procedure of preparation of the CODE. In Step 1, the partially polymerized solution was prepared from 94 mass % IOA, 6 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. The type and amount of modified nanoparticles are summarized in Table 8. In Step 2 were added 0.10 parts per hundred hardener TRZ and an additional 0.16 parts per hundred of the photocatalyst (I-651. In Stage 3, the intensity of the UV radiation spectrum "A" was 160 millijoules per square centimeter. In Step 4, the intensity of Wisliceny spectrum "C" was 47 millijoules per square centimeter. Vulcanized-curable pressure adhesives were evaluated at the Time of shearing strength at 23°C on HC with a mass of 1000 g, 15-minute test for peel resistance on HC, and 72-hour test for peel resistance to HC, as described in the above test methods. The results are shown in Table 8.

td align="center"> No
Table 8
The composition and results for data Set "E"
EXAMPLEMNPShift (+)Peel (N/DM)
RoomParts per hundredNP:P (*)ReactivityHC (min)15 min, HC72 hours, HC
REF-E1No0-10000+72126
E1MNP-61080:2010000+73144
E2MNP-81080:20Yes10000+80173
CE-E1MNP-510100:0No10000+77169
(*) The ratio of the molar percent of the polymeric surface-modifying substances (IOTMS) to polymeric surface-modifying substance.
(+) Shear at 23°C with a load of 1000 g

[0087] the data Set "F". The reference examples REF-REF F1 and-F2, and F1-F4. This set of data shows that the use of different polymer bundles and the matrix CODE may provide an advantageous balance of properties. Adhesives REF-F1 and Examples F1 and F2 were based on the adhesive composition 904:10 IOA:AA, including the hardener. Typically, the adhesive compositions with a high content of acrylic acid are considered suitable for use on substrates with high top�ostroy energy. Adhesives REF-F2 and Examples F3 and F4 were based on the adhesive composition of 99.1:0.9:20.0 IOA:AA:IBOA with tackifiers, including the hardener. Typically, the adhesive compositions with a very low content of acrylic acid are considered suitable for use on substrates with low surface energy. The adhesive compositions of Examples F1-F4 contained nanoparticles, modified with associated reactive polymer ligaments. The adhesive compositions were vulcanized only with the help of UV radiation spectrum "A".

[0088] Samples were prepared according to the Procedure of preparation of the CODE. For the Reference example REF-F1 and Examples F1 and F2 in Phase 1, partially polymerized solution was prepared from 90 mass % to the IOA, 10 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. The type and amount of modified nanoparticles are summarized in Table 9. In Step 2 were added 0.16 parts per hundred of the photocatalyst (I-651, and in Stage 3, the intensity of the UV radiation spectrum "A" was 169 millijoules per square centimeter.

[0089] For Reference example REF-F2 and Examples F3 and F4 in Step 1, the partially polymerized solution was prepared from 99,1 mass % IOA, a 0.9 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. The type and amount of modified nanoparticles are summarized in Table 9. In Step 2 were added 0.17 parts per hundred hardener TRZ, advanced�enforcement of 0.20 parts per hundred of the photocatalyst (I-651 and 20.0 parts per hundred monomer IBOA. It was also added 28.8 parts per hundred of hydrocarbon resin R6108. In Stage 3, the intensity of the UV radiation spectrum "A" was 631 millijoules per square centimeter.

[0090] the Cured curable pressure adhesives were evaluated during shear at 70°C on HC with a mass of 1000 g, 15-minute and 72-hour test for peel resistance on a substrate with high surface energy (i.e. stainless steel), and a substrate with low surface energy (i.e., polypropylene) were measured as described in the above test methods. The results are shown in Table 9.

td align="center"> MNP-9
Table 9
The composition and results for data Set "F"
EXAMPLEMNPShift(+)Peel (N/DM)
RoomParts per hundredNP:P (*)NS (min)15 min, NS72 hours, NS15 min, PP72 hours PP
REF-F1 No010000+841322028
F1MNP-101080:2010000+881912040
F2MNP-91080:2010000+951492225
REF-F2No0-115477946274
F3MNP-101080:2010000+62864575
F41080:2010000+691097582
(*) The ratio of the molar percent of the polymeric surface-modifying substances (IOTMS) to polymeric surface-modifying substance.
(+) Shear at 70°C with a load of 1000 g

[0091] In the examples with the matrix CODE, suitable for the surface with VPE (Examples F1 and F2), the addition of nanoparticles surface-modified with polymer ligaments having poor compatibility with CODE that provided improved 15-minute and 72-hour peeling resistance with stainless steel, the substrate with VPE, without prejudice to shear. In addition, the use of polymer ligaments (MNP 10) which includes a monomer with a high Tc (IBOA, Tc is equal to 104°C), provided excellent peeling resistance of the polypropylene (PP), a substrate with low surface energy, compared to a bunch of similar compatibility (MNP-9), but which includes a monomer with a low Tc (VA, Those equal to 49°C).

[0092] In some examples, a matrix CODE, suitable for surfaces with NPE (Examples F3 and F4), the addition of nanoparticles with a surface modi�tirovannoj using polymer ligaments, having good compatibility with CODE, improved shear strength. The excellent results of the peel strength on stainless steel and polypropylene were obtained using polymer ligaments, which includes a monomer with a low Tc (silane polymer MNP-9-82,5/16,7/0,8 BA/IOA/AA), compared with a polymeric binder comprising a monomer with a high Tc (silane polymer MNP-10-82,5/16,7/0,8 IBOA/IOA/AA).

[0093] the data Set "G". The adhesive compositions of the data Set "G" were based on the adhesive composition of 90:10 IOA:AA. We investigated the effects of including modified nanoparticles, including a curing agent in the matrix CODE and the use of UV radiation spectrum "C".

[0094] Samples were prepared according to the Procedure of preparation of the CODE. In Step 1, the partially polymerized solution was prepared from 90 mass % to the IOA, 10 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. Also there was added 10 parts per hundred of surface-modified, reactive, polymeric nanoparticles MNP-8. In Phase 2, were added photocatalyst I-651 and, optionally, a curing agent (hardener TRZ), as summarized in Table 10. All the samples were only solidified using UV radiation spectrum "A" (Phase 3). Thus, the reactive polymer ligaments modified nanoparticles were left without connections with the adhesive matrix. Some way�s were also subsequently solidified using UV radiation spectrum "C" (Stage 4), forming a connection of the reactive polymer ligaments modified nanoparticles with an adhesive matrix.

Table 10
Compositions adhesive compositions of the data Set "G"
EXAMPLEMNP (10 parts per hundred)TRZ (parts per hundred)I-651 (parts per hundred)UV-spectrum "A"
(MJ/cm2)
UV-spectrum "C"
(MJ/cm2)
REF-G1No00.151690
G1MNP-800.151690
REF-G2No00.1516947
G2MNP-800.1516947
REF-G3No0.100.161600
G3MNP-80.100.161600
REF-G4No0.100.1616047
G4MNP-80.100.1616047

[0095] the Cured curable pressure adhesives were evaluated at the Time of shear at a temperature of 23°C and 50% relative humidity at HC with a mass of 1000 g, 15-minute test for peel resistance on HC, and 72-hour test for peel resistance to HC, as described in the above test methods. The results are shown in Table 11.

Table 11
The adhesive properties of adhesive compositions of the data Set "G" on the stainless�ing steel
EXAMPLEThe cure in the CODEMNPCuring the UV-spectrum "C"Shift (+) (min)15 min exfoliation (N/DM)72 hours of peeling (N/DM)
REF-G1NoNoNo18862112
01NoYesNo19258120
REF-G2NoNoYes35261115
G2NoYesYes24448126
REF-G3YesNoNo1000+ 86146
G3YesYesNo10000+95195
REF-G4YesNoYes10000+91147
G4YesYesYes10000+73221
(+) Shear at a temperature of 23°C and 50% relative humidity with a load of 1000 g

[0096] the data Set "H". Reference example REF-H1, Samples H1-H3, and Comparative examples CE-H1-CE-H3. The adhesive substance from the data Set of "N" were based on the adhesive composition of 90:10 IOA:AA, including the hardener. Samples were prepared using nanoparticles of size 20 nm and 75 nm. The nanoparticles were modified by the use of inert polymer bundles with different ratios not polymeric to polymeric surface modification. The adhesive compositions have been solidified with the help�new York as UV radiation spectrum "A", and UV radiation spectrum "C".

[0097] Samples were prepared according to the Procedure of preparation of the CODE. In Step 1, the partially polymerized solution was prepared from 90 mass % to the IOA, 10 mass % AA and 0,040 parts per hundred of the photocatalyst (I-651. The type and amount of modified nanoparticles are summarized in Table 12. In Step 2 were added 0.15 parts per hundred of the photocatalyst I-651 and 0.10 parts per hundred hardener TRZ. In Stage 3, the intensity of the UV radiation spectrum "A" was 191 millijoules per square centimeter. In Step 4, the intensity of the UV radiation spectrum "C" was 60 millijoules per square centimeter.

[0098] Vulcanized-curable pressure adhesives were evaluated during shear at 70°C in stainless steel with a mass of 1000 g of 15-minute and 72-hour test for peel resistance on a substrate with high surface energy (i.e. stainless steel), and a substrate with low surface energy (i.e., polypropylene) were measured as described in the above test methods. The results are shown in Table 12 and summarized in Fig. 1 and 2.

/tr> 5000
Table 12
The composition and results for data Set "H"
P�EMER MNPShift(+)Peel (N/DM)
NSPP
RoomParts per hundredNP:P (*)MM (g/mol)HC (min)15 min72 hours15 min72 hours
REF-H1-0--10000+86922227
H1MNP-21080:20500010000+82993051
H2MNP-2580:205000 10000+761132944
H3MNP-22.580:20500010000+791112439
H4MNP-4580:2030,00010000+811062536
H5MNP-42.580:2030,00010000+71942337
H6MNP-3560:40500010000+791193050
H7MNP-32.560:40500010000+741132743
CE-H1MNP-15100:0-10000+701052027
CE-H2MNP-12.5100:0-10000+811042129
H8MNP-111080:20500010000+861122334
H9MNP-11580:2010000+771192436
H10MNP-112.580:20500010000+661022335
H11MNP-13580:2030,00010000+791082534
H12MNP-132.580:2030,00010000+851032734
H13MNP-12560:40500010000+8210444
H14MNP-122.560:40500010000+90962640
CE-H3MNP-55100:0-10000+721062630
CE-H4MNP-52.5100:0-10000+771182628

[0099] the Experts in this field will be obvious that the described invention can be made various changes and modifications, without departing from the scope of this invention.

1. Cured under pressure adhesive containing an acrylic polymer and surface-modified nanoparticles, where the surface-modified nanoparticles contain:
(a) a nanoparticle having to�annieway surface;
(b) a polymeric silane surface modifying group, and
(C) a polymeric silane surface modifying group;
where the polymeric silane surface modifying group and a polymeric silane surface modifying group covalently linked to the silicon surface of the nanoparticle, in this case,
acrylate polymer comprises the reaction product of one or more methacrylate monomers and at least one monomer vinylcarbazole acid, methacrylate monomers include a first methacrylate monomer where the alkyl group of the first methacrylate monomer contains from 4 to 18 carbon atoms, inclusive, and
vinylcarbazole acid is selected from the group consisting of acrylic and methacrylic acids.

2. Cured under pressure adhesive according to claim 1, characterized in that the acrylate polymer contains from 2 to 10 mass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid and methacrylate monomers.

3. Cured under pressure adhesive according to claim 1, characterized in that the acrylate polymer contains from 0.5 to 1.5 mass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid and methacrylate monomers.

4. Cured under pressure adhesive according to claim 1, characterized in that the polymer resin�Naya silane surface-modifying group consisting of methacrylate repeating units.

5. Cured under pressure adhesive according to claim 4, characterized in that the polymeric silane surface modifying group further has a repeating unit a vinyl carboxylic acid.

6. Cured under pressure adhesive according to claim 5, characterized in that the acrylate polymer contains WAPmass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid monomers and methacrylate acrylate polymer, and a polymeric silane surface modifying group contains WOSmass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid monomers and methacrylate acrylate polymer is a polymer silonovoy surface-modifying group, and the ratio of WOS/WAPis between 0.8 and 1.2, inclusive.

7. Cured under pressure adhesive according to claim 5, characterized in that the acrylate polymer contains WAPmass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid monomers and methacrylate acrylate polymer, and a polymeric silane surface modifying group contains WOSmass percent vinylcarbazole acid, based on the total weight of the monomers vinylcarbazole acid monomers and methacrylate acrylate polymer is a polymer silonovoy on�Ernesto-modifying group, and the ratio of WOS/WAPless than 0.5 or more than 2.

8. Cured under pressure adhesive according to claim 1, characterized in that the polymeric silane surface modifying group comprises at least 10 repeating units.

9. Cured under pressure adhesive according to claim 1, characterized in that the polymeric silane surface modifying group consists of no more than 200 repeating units.

10. Cured under pressure adhesive according to claim 1, characterized in that it is not a polymeric silane surface-modifying substance comprises at least one of tralkoxydim silane and tralkoxydim silane.

11. Cured under pressure adhesive according to claim 1, characterized in that the ratio of the molar percent of the polymeric surface-modifying substance to the polymeric surface-modifying substance is between 95:5 and 50:50, inclusive.

12. Cured under pressure adhesive according to claim 11, characterized in that the ratio of the molar percent of the polymeric surface-modifying substance to the polymeric surface-modifying substance is between 80:20 and 60:40, inclusive.

13. Cured under pressure adhesive according to claim 1, characterized in that the polymeric surface-modifying substance has a functional group capable of forming cross-links with the acrylate polymer�M.

14. Cured under pressure adhesive according to claim 13, characterized in that the functional group contains a group that produce hydrogen.

15. Cured under pressure adhesive in accordance with claim 14, characterized in that the group that produce hydrogen, contains benzophenone.

16. Cured under pressure adhesive according to claim 1, characterized in that it further comprises a curing agent.

17. Cured under pressure adhesive according to claim 1, containing from 5 to 20 mass parts, inclusive, of surface-modified nanoparticles to 100 parts by weight of acrylate polymer.

18. Cured under pressure adhesive according to claim 1, characterized in that it further comprises tackifiers.

19. The method of preparing the curable pressure adhesive consisting of
(i) treatment of the mixture of the first methacrylate monomer, vinylcarbazole acid, the first photocatalyst and the surface-modified nanoparticles of ultraviolet radiation in spectrum "A" is sufficient for partial polymerization of the first methacrylate monomer and a vinyl carboxylic acid with the formation of the partially polymerized mixture;
(ii) adding a curing agent and a second photocatalyst to the partially polymerized mixture to form a coating;
(iii) coating on a substrate, and
(iv) effect on the substrate of the ultraviolet radiation spectrum of ADL education of glue, cured under pressure, where the surface-modified nanoparticles contain:
(a) a nanoparticle having a silicon surface;
(b) a polymeric silane surface modifying group having a molecular weight of at least 1000 grams per mole, and
(c) not polymeric silane surface modifying group having a molecular weight less than 500 grams per mole,
where the polymeric silane surface modifying group and a polymeric silane surface modifying group covalently linked to the silicon surface of the nanoparticle.

20. A method according to claim 19, characterized in that the polymeric surface-modifying substance has a functional group capable of forming cross-links with the acrylate polymer.

21. A method according to claim 20, further comprising impact on cured under pressure adhesive UV radiation spectrum "C" for the purpose of binding the polymeric surface-modifying substance with an acrylate polymer.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to polymer chemistry and specifically to adhesive compositions based on a copolymer of butyl methacrylate and methacrylic acid, used for bonding different substrates (metal, wood, ceramic etc.). The adhesive composition contains (pts.wt) 20.0-30.0 copolymer of 95 wt % butyl methacrylate with 5 wt % methacrylic acid (BMK-5); 3.0-10.0 organic silane of formula (C2H5O)4-n-Si-[OSi(OC2H5)3]n, where n=0-2; 0.5-3.0 water; 2.0-10.0 aerosil and an organic solvent - 46.99-67.5.

EFFECT: use of the organic silane of given formula and water in the adhesive composition increases adhesive strength and heat resistance of the adhesive composition based on the BMK-5 copolymer.

2 tbl, 17 ex

FIELD: chemistry.

SUBSTANCE: described is an adhesive composition for gluing to metal, containing: (a) at least one methacrylate radical polymerisation monomer; (b) an ambient temperature radical polymerisation initiator system containing at least one oxidant and at least one reducing agent; (c) a photoinitiator; and (d) an epoxy compound; where the adhesive will at least partially solidify at temperature between 10 and 40°C through a radical polymerisation catalyst system which is activated at ambient temperature. Described also is a two-component curing adhesive for gluing to metal, containing: (a) a first component containing (i) at least one methacrylate radical polymerisation monomer, (ii) at least one reducing agent and (iii) a photoinitiator and (b) a second component containing an oxidant which is reactive at ambient temperature with respect to the reducing agent and forms free radicals capable of initiating radical polymerisation and facilitate chain growth, and an epoxy compound; where the adhesive will at least partially solidify at temperature between 10 and 40°C through a radical polymerisation system activated at ambient temperature.

EFFECT: obtaining an adhesive which does not require additional heat for initiating curing.

24 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: composition contains the following in wt %: 5-80 polyester A copolymer obtained as a result of condensation with itaconic acid; 5-80 (meth)acrylate homopolymer and/or copolymer B consisting of more than 50 wt % monomers of formula I where R1 denotes hydrogen or methyl and R2 denotes an alkyl residue, an aliphatic or aromatic residue with 1-5 carbon atoms and 10-80 graft copolymer from type A polymer and type B polymer (polymer AB). Polyester A has a straight or branched structure with OH number from 5 to 150 mg KOH/g, and acid number less than 10 mg KOH/g, and number-average molecular weight 700-25000 g/mol. Content of itaconic links in the polyester copolymer per total content of polycarboxylic acids ranges from 0.1 mol % to 20 mol %.

EFFECT: invention enables to obtain well compatible polymer structures which do not contain styrene or derivatives thereof, based on a polyester graft polymethacrylate copolymer.

17 cl, 3 tbl, 9 ex

FIELD: electricity.

SUBSTANCE: adhesive tape includes adhesive polymeric resin on acryl basis and conductive fillers. Adhesive polymeric resin includes polymer obtained by copolymerisation of alkyl acrylate monomer having C1-C14 alkyl group with polar copolymerised monomer. Conductive filler is chosen from the group consisting of precious metals, base metals, precious or base metals with coating from precious metals, precious and base metals with coating from base metals, non-metals with coating from precious and base metals, conductive non-metals, conductive polymers, and their mixtures. Conductive fillers are oriented in adhesive tape both on longitudinal and in transverse directions. Electrically conducting adhesive tape is obtained by mixing monomers for preparation of adhesive polymeric resin with conductive fillers. Mixture in the form of sheet is formed. Both surfaces of the sheet are illuminated with light in order to perform photochemical polymerisation of adhesive polymeric resin. Each surface of the sheet is illuminated with light of various intensity. Light is emitted selectively to some part of the sheet of surface. Adhesive tape has flexibility and more effective electric conductivity.

EFFECT: adhesive tape can be used in electronic components, as adhesive tape screening electromagnetic waves, which provides the possibility of easy attachment and detachment.

18 cl, 3 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: composition contains epoxy diane resin, oligoether acrylate, curing agent, initiator and solid filler. The filler is silica gel or aerosil. The initiator is in form of benzoin or dimethoxyphenyl acetophenone ethers. Oligoether acrylate is selected from a group of dimethacrylate ethers. The curing agent used is aliphatic or aromatic diamine and aliphatic or aromatic tertiary amine. The photocurable adhesive composition is obtained by mixing all components until their complete dissolution. The obtained mixture is put between glued surfaces and exposed to UV light for not less than 5 min. Further, thermal post-polymerisation is carried out at temperature not higher than 50°C, followed by cooling and holding. The invention is used in production of organic light-emitting diodes to prolong their service life.

EFFECT: good adhesion to glass, weather resistance, low chemical aggressiveness, high water resistance and crack resistance when pressed between glass plates.

8 cl, 3 tbl, 3 ex

FIELD: polymerization processes.

SUBSTANCE: invention relates to two-component composition used to initiate curing of one or more polymerizable monomers that are cured when affected by free radicals, which composition consists of organoborane-amino complex and an isocyanate capable of destroying organoborane-amino complex, wherein equivalent ratio of amine nitrogen atoms to boron atoms ranges from more than 4.0:1 to 20.0:1. In another embodiment of invention, subject of invention is two-component composition for use as sealing materials, coatings, primers for modifying polymer surfaces, and as molded resins, which composition consists of component 1: organoborane-amino complex wherein ratio of amine nitrogen atoms to boron atoms ranges from more than 4.0:1 to 20.0:1; component 2: one or more monomers, oligomers, or polymers having olefinic instauration, which are able of being subjected to free-radical polymerization; and effective amount of an isocyanate, which can initiate dissociation of complex to free borane for initiation of polymerization of one or more monomers, oligomers, or polymers having olefinic instauration, provided that complex dissociation initiator is stored separately from complex until initiation of polymerization becomes desirable. Such compositions are handling safe, i.e. they are not self-inflammable, stable at or near ambient temperature and so they do not initiate polymerization at or near ambient temperature in absence of complex dissociation initiator. Polymerized composition show good cohesion and adhesion strength. Described are polymerizable composition polymerization process, method of gluing two or more substrates using polymerizable composition; method of modifying polymer surface having low surface energy using polymerizable composition, as well as coating and laminate containing polymerizable composition.

EFFECT: enlarged resource of polymerizable compositions and expanded application areas thereof.

10 cl, 2 dwg, 4 tbl

The invention relates to adhesive compositions based on water dispersion of acrylic copolymer and can be used for gluing PVC materials (films, vacuum forming tiles and t

FIELD: chemistry.

SUBSTANCE: invention relates to silicon-acryl hybrid polymers, glue compositions, gluing when pressed, which contain hybrid polymers. Glues can be used in contact with skin and in manufacturing medical tapes and systems of transdermal delivery of medications. Hybrid polymer resulting from carrying out joint chemical reaction for silicon polymer component, which represents organodisubstituted polysiloxane, silicone resin component and acryl polymer component, obtained from mixture of polydimethylsiloxane mono(meth)acrylate monomer, with obtaining hybrid silicone-acrylate polymer, where acryl polymer component is covalently self-cross-linked with silicone polymer component and/or silicone resin component. Invention also relates to hybrid polymer, obtained as a result of carrying out joint chemical reaction for silicone polymer component, silicone resin component and acryl polymer component with obtaining hybrid silicone-acrylate polymer, where silicone resin component contains silicone resin, containing triorganosiloxy-units R3SiO1/2, where R represents organic group, and tetrafunctional siloxyl-units SiO4/2 with molar ratio in the range from 0.1 to 0.9 of R3SiO1/2 unit per each SiO4/2 unit, where acrylate polymer is obtained from monomers, selected from the group, including butylacrylate, 2-ethylhexylacrylate, isooctylacrylate, methylacrylate, methylmethacrylate, N-(tertiary)octylacrylamide, hydroxyethylacrylate, acrylic acid, hydroxypropylacrylate, hydroxypropylmethacrylate or their mixtures.

EFFECT: invention makes it possible to create glues, demonstrating wide range of characteristics with respect to gluing when pressed, in particular, high level of characteristics of detachment, adhesiveness and displacement.

10 cl, 2 dwg, 4 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to an adhesive which is suitable for use with low-surface energy materials. The adhesive contains an acrylic copolymer, an adhesive reagent with a high glass transition point (Tg) and an adhesive reagent with a low glass transition point. The acrylic copolymer is a ternary copolymer of 2-ethylhexyl acrylate, butyl acrylate and acrylic acid. The adhesive reagents with a high glass transition point and a low glass transition point are terpenes, terpene-phenol-formaldehyde resins, rosin ester and modified C5-C9 aliphatic and aromatic hydrocarbons. Both adhesive reagents have Tg greater than Tg of the acrylic copolymer.

EFFECT: adhesive reagent with a high glass transition point has Tg of at least 20°C and the adhesive reagent with a low glass transition point has Tg of less than 0°C.

14 cl, 1 dwg, 10 tbl

FIELD: chemistry.

SUBSTANCE: described is a core-cladding emulsive polymerisate with an activator included in the core, which is obtained from polymerising a mixture containing: a) 5-99.9 wt % of one or more mono-functional (meth)acrylate monomers with water solubility of < 2 wt % at 20°C; b) 0-70 wt % of one or more monomers that copolymerisable with monomers a); c) 0-20 wt % of one or more compounds that are di- or multi-vinylenically unsaturated; d) 0-20 wt % of one or more polar monomers with water solubility of >2 wt % at 20°C, selected from (meth)acrylic acid and (meth)acrylamide, and c) 0.1-95 wt % of at least one activator. Wherein components a) to e) amount to 100 wt % of polymerisable components of the mixture, characterised by that e1) the activator is a compound of formula I where R1 is methyl; X is a linear alkanediiyl group with 1-18 carbon atoms; R2 denotes a hydrogen atom or a linear or branched alkyl residue with 1-12 carbon atoms; R3, R4, R5, R6 and R7 independently denote a hydrogen atom and that e2) the activator e) is covalently bonded to the emulsive polymerisate. Also described is a method of producing said emulsive polymerisate by "core-cladding" polymerisation in an aqueous emulsion, wherein components a) to e) at the first step are polymerised in form of a core, and then a mixture of components a) to d) are polymerised thereon as cladding in at least an additional step. Components a) to e) for the core and components a) to d) for the cladding are selected such that in the resultant polymerisate, the glass transition temperature of at least one cladding TGS is higher than the glass transition temperature of the core TGK, wherein the glass transition temperature of at least one cladding TGS is higher than 100°C, wherein the glass transition temperature TG is determined according to the EN ISO 11357 standard. Described is a two- or multi-component system with a controlled working life, which is curable at room temperature using a redox system of initiators containing A) 0.8-69.94 wt % emulsive polymerisate according to claims 1-7 or obtained by a method according to claim 8; B) 30-99.14 wt % of one or more ethylenically unsaturated monomers; C) 0.05-30 wt % peroxides; optionally D) 0-60 wt% unsaturated oligomers; E) 0.01-2 wt % polymerisation inhibitor; and optionally F) 0-800 pts.wt auxiliary substances and additives; wherein the sum of components A)+B)+C)+D)+E) is 100 wt %, and the amount of F) relates to 100 pts.wt of the sum A)+B)+C)+D)+E). Wherein component A) and component C) are stored together, and before applying the system, at least one component B) is stored separately from A) and C), wherein the capacity of the separately stored component B) to cause swelling of the polymerisate A) is so high that the activator of the polymerisate A) fixed in the polymer can react with component C), or component A), part of component B) and component DC) are stored together, wherein part of component B) is selected such that the capacity of component B) to cause swelling of the polymerisate A) is so low that the activator of the polymerisate A) fixed in the polymer cannot react with component C). Also described is use of said two- or multi-component system as a component part of substances, such as resins from unsaturated polyesters and vinyl esters or adhesive substances, cast resins, polymer coatings for floors and other reactive coatings, sealants, impregnating compounds, binding compounds, compounds for making artificial marble and other artificial stones, compounds for reactive concrete inserts, tooth filling compounds, porous plastic moulds for ceramic articles.

EFFECT: obtaining two- or multi-component systems that are curable at room temperature, the working life of which can be controlled in a wide range and which, nevertheless, are quickly and completely curable before a certain moment in time without requiring energy or an external mechanical pulse.

13 cl, 2 tbl, 19 ex

FIELD: chemistry.

SUBSTANCE: polymer type A is a copolyester obtained by cocondensation of unsaturated aliphatic dicarboxylic acids, selected from a group comprising fumaric acid, maleic acid, itaconic acid and esterifiable derivatives thereof, with polyols or lactones. Monomers which form type B polymer are selected from a group comprising methyl(meth)acrylate, ethyl(meth)acrylate, propyl(meth)acrylate, butyl(meth)acrylate and ethylhexyl(meth)acrylate. Type AB polymer is a graft copolymer of type A polymer and type B polymer and is a copolymer with polyester backbone chains and poly(meth)acrylate side chains.

EFFECT: mixture, which contains type A, B and AB polymers, has high compatibility of polymer components and is suitable for use as an adhesive, particularly a melt adhesive.

13 cl, 3 tbl, 14 ex

FIELD: chemistry.

SUBSTANCE: described is an adhesive composition for gluing to metal, containing: (a) at least one methacrylate radical polymerisation monomer; (b) an ambient temperature radical polymerisation initiator system containing at least one oxidant and at least one reducing agent; (c) a photoinitiator; and (d) an epoxy compound; where the adhesive will at least partially solidify at temperature between 10 and 40°C through a radical polymerisation catalyst system which is activated at ambient temperature. Described also is a two-component curing adhesive for gluing to metal, containing: (a) a first component containing (i) at least one methacrylate radical polymerisation monomer, (ii) at least one reducing agent and (iii) a photoinitiator and (b) a second component containing an oxidant which is reactive at ambient temperature with respect to the reducing agent and forms free radicals capable of initiating radical polymerisation and facilitate chain growth, and an epoxy compound; where the adhesive will at least partially solidify at temperature between 10 and 40°C through a radical polymerisation system activated at ambient temperature.

EFFECT: obtaining an adhesive which does not require additional heat for initiating curing.

24 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention discloses versions of water resistant, pressure sensitive adhesive acrylic polymers having volume-average particle size of at least 250 nm, formed during polymerisation in the presence of a surfactant in an emulsion of a mixture of monomers. Disclosed also are versions of labels having a frontal base and a pressure sensitive adhesive, which is one of the versions of the disclosed water resistant acrylic polymers.

EFFECT: disclosed polymers enable to obtain pressure sensitive acrylic based adhesives, which during coating and drying in form of a film become transparent and resistance to whitening when exposed to water.

44 cl, 1 dwg, 2 tbl, 16 ex

The invention relates to sealing compositions, in particular polyacrylate connecting the sealant composition of the copolymers and Acrylonitrile

The invention relates to a sticky water-based adhesive compositions based on acrylic copolymers, particularly to adhesives for adhesive tapes for paper, cardboard, plastic or metal bases, used for the manufacture of self-adhesive decorative and finishing materials, for gluing cardboard products on conveyor technology for labeling in paper, printing and other industries
The invention relates to adhesive substances, and more particularly to a method of manufacturing heat-sensitive adhesive compositions

FIELD: chemistry.

SUBSTANCE: invention can be used in paint industry. The method of producing an aqueous dispersion of silanised colloidal particles of silica in an aqueous medium involves mixing a) at least one silane compound with epoxy functionality, b) at least one silane compound without epoxy functionality, capable of modifying colloidal particles of silica, and c) colloidal particles of silica to form an aqueous dispersion of silanised colloidal particles of silica containing silane compounds from a) and b). The weight ratio of a) and b) to silica ranges from about 0.01 to 1.5.

EFFECT: invention increases stability of colloidal silica dispersions, water resistance and hardness of lacquer coatings.

13 cl, 15 tbl

FIELD: chemistry.

SUBSTANCE: solid particles are selected from a group consisting of corundum, fused corundum, sintered corundum, zircon corundum, silicon carbide, boron carbide, cubic boron nitride, diamond and/or mixtures thereof and have a physically applied coating. The coating contains at least one polyol.

EFFECT: invention improves processing properties of solid particles and reduces dust formation which occurs when processing solid particles.

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