Method of marking materials

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of marking materials with coded microparticles. Described is a method of marking materials with coded microparticles, characterised by that the coded microparticles used are obtained (i) through polymerisation of at least one water-soluble monoethylene unsaturated monomer in the presence of at least one ethylene unsaturated monomer containing at least two double bonds in a molecule, through reverse suspension polymerisation of water in oil, where the suspension agent used is doped nanoparticles, or (ii) emulsion polymerisation of water-insoluble monoethylene unsaturated monomers containing 0-10 wt %, in terms of the mixture of monomers, of at least one ethylene unsaturated monomer containing at least two double bonds in a molecule, where the emulsifying agent for stabilising the dispersion phase is in form of doped nanoparticles, or (iii) polymerisation of at least one ethylene unsaturated monomer and a copolymerisable dye containing an ethylene unsaturated double bond and, if needed, agglomeration of these particles, where during polymerisation in accordance with (i) and (ii), nanoparticles used are radioactively doped or doped with at least one dye and one compound from the group of rare-earth elements of the periodic table. Described also are materials containing coded microparticles for marking, obtained using the described method. The invention describes use of coded microparticles obtained using the described method.

EFFECT: novel method of marking materials.

14 cl, 1 tbl, 14 ex

 

The invention relates to a method of labeling materials encoded microparticles.

From US-A-3772099 known method of encoding explosives using inorganic phosphor, and fine commercially available phosphor and fine phosphor, doped, at least one element of the group of the lanthanoids of the Periodic system, are mixed, for example, with an aqueous solution of potassium silicate, a mixture of dried, crushed and sieved. The size of the particles formed in this way conglomerate ranges from 0.5 to 0.7 mm, while the particle size of the phosphors is from 6 to 8 μm. This conglomerate can, for example, carefully mixed with the explosive in the manufacture of dynamite. Already in 0.01 wt.% enough for marking explosives. Marked thus explosives may - even after the detonation on the basis of samples taken can be determined by means of emission lines, which emit coded phosphors, for example, irradiated with ultraviolet radiation. Because of the different doped phosphors there are a large number of possibilities of combinations, so you can determine the manufacturer, year, month, and week of manufacture explosives, labeled accordingly several doped phosphor is mi.

From US-A-4390452 known encoded microparticles intended for retrospective identification of substances containing such microparticles. The encoded microparticles are obtained by consecutive application in accordance with DE-A-2651528 visually distinct layers of paint on the carrier film and by obtaining on the surface of the material by means of diazotization of a very thin layer, in which the irradiation of UV-rays that pass through the containing microdata positive and get on this layer, after the manifestation contain numbers and symbols that can be decrypted by means of a microscope. From the applied layer is made of microparticles, the size of which does not exceed 1000 μm, having two flat parallel surfaces, which contain printed numbers and symbols. Microparticles used for labeling substances, such as explosives, with the purpose of the retrospective recognition of the origins and characteristics of the product.

WO-A-03/044276 relates to protective paper and protective products that contain at least one safety element based on the at least one photoluminescent segment, which can be at least partially placed in a paper product, 30-99 wt.% consisting of dry fibers and 70-1 wt.% of the filler. The safety element may, for example, b is to be obtained by coloring media of cellulose fibers photoluminescent paint. Photoluminescence becomes visible when the safety element is irradiated with radiation, the wavelength of which ranges from 200 to 500 nm.

From WO-A-03/052025 known containing nanoparticles printing ink for inkjet printers or printers on the piezoelectric elements. The diameter of the nanoparticles is from 1 to 1000 nm, they have a crystalline structure. They mainly consist of alloyed metal salt, for example nanoparticles from YVO4doped iridium, or LaPO4doped with cerium. The nanoparticles can be doped by several elements, such as LaPO4doped with cerium and terbium. Using such ink banknotes that are printed on these printers can, for example, be protected from forgery.

From WO-A-02/46528 known method of applying a protective marking as a coating on a substrate, such as paper, ceramic or polymer, and the binder layer contains a fluorescent microparticles with a diameter of 0.2 to 2 μm and optical distinguish them from individual particles with a diameter from 10 to 20 μm. When considering the naked eye the floor seems solid, however, with a strong increase in individual particles of color distinguished from particles with a diameter from 0.2 to 2 microns.

From US-B-6620360 a method of obtaining a multilayer microparticles for marking and further identifier is tion substances, containing these microparticles. Microparticles are obtained by successive deposition of several thin and visually discernible marking layer on a flat substrate, and the thickness of the marking layer after solidification should be less than 4.5 μm to 1 μm before applying the next layer. Then flat substrate is removed, and the material of the marking layer is crushed to obtain powder.

From US-B-6455157 known to use at least two different groups of microparticles for labeling of products, each microparticle group has several layers of paint, forming a code. Using these microparticles possible hierarchical coding products, so you can identify the manufacturer and the number of the labeled product.

B.J.Battersby, G.A.Lawrie. A.P.R.Johnston and Mthai in Chem. Commun., 2002, 1435-1441 reported optical encoding colloidal suspensions of fluorescent dyes, crystals and metals. So, for example, colloids with a diameter of from 3 to 6 μm optical mark by soaking fluorescent dyes or complex related lanthanides. Another type of marking colloids consists in soaking the zinc sulfide, cadmium-containing-selenide nanocrystals, or electrochemical deposition of metal ions in the voids of the colloids. Colloids can, for example, to distinguish the other is from each other using a fluorescent microscope or cytometer.

The present invention is the task of developing other ways of marking materials.

The task according to the invention is solved with a method of marking material encoded microparticles in the case of the use of microparticles obtained:

(i) polymerization of at least one water-soluble monoethyleneglycol monomer in the presence of at least one ethyleneamine monomer containing at least two double bonds in the molecule by reverse suspension polymerization of water in the oil, and as a suspending agent used doped nanoparticles,

(ii) emulsion polymerization of water-insoluble monomethylethanolamine monomers comprising from 0 to 10 wt.%, in terms of the mixture of monomers, at least one ethyleneamine monomer containing at least two double bonds in the molecule, and as an emulsifier to stabilize the dispersed phase using doped nanoparticles,

(iii) polymerization of at least one ethyleneamine monomer capable of copolymerization of dye containing Ethylenediamine double bond, and, if necessary, the agglomeration of these particles or

(iv) the agglomeration of at least two different groups of microparticles, characterized its the th absorptive capacity, emission and/or scattering of electromagnetic radiation, up to units, the average particle diameter ranging from 300 nm to 500 μm.

When carrying out polymerization according to (i) and (ii) use, for example, radioactively doped nanoparticles or nanoparticles, doped, at least one dye or one compound from the group of rare earth elements of the Periodic system.

The average diameter of the polymer particles obtained by polymerization according to (i)is, for example, from 0.1 to 1000 μm, preferably from 0.5 to 50 μm. Most often, the average diameter obtained according to (i) of the microparticles is from 1 to 20 μm. Getting granular polymers by the method of inverse suspension polymerization of water in oil (GSP), which as a suspending agent used doped nanoparticles, for example described in US-A-2982749, from column 1, line 21 to column 6, line 34. Examples of such suspendida agents having a low hydrophilic-lipophilic balance (HLB value below 7, preferably below 4)are modified silanes of finely dispersed silicic acid (silanized silica, bentonite or clay treated with Quaternary ammonium compounds, and organic nanoparticles, such as partially from sulphonated polyvinylformal or modified dimethylaminopropane of hlorvinilovye. To determine the HLB values are referred to the publication W..Griffin, Journal of Society of Cosmetic Chemist, vol. 1, 311 (1950).

Other nanoparticles, which can be used as suspendida agents are caso3, BaSO4, barium titanate, SiO2, oxides, sulfides, phosphates and pyrophosphates of alkali-earth or transition metals, in particular zinc oxide, titanium dioxide, iron oxide (goethite, hematite), iron sulfide and barium pyrophosphate, and polymer particles such as polystyrene or polyacrylate, a mixture of two or more nanoparticles, for example a mixture of zinc oxide and titanium dioxide. The average diameter of the nanoparticles is, for example, from 5 to 500 nm, usually from 20 to 300 nm.

The method of stabilization of emulsions, colloidal particles, and also other suspendresume agents for cap described in the publication R.Aveyard, B.P.Binks and J.H.Clint, Advances in Colloid and Interface Science, vol 100-102, str-546 (2003). In addition, reference is made to the publication .Vignati and R.Piazza, Langmuir, Vol.19, No.17, 6650-6656 (2003) about the Pickering emulsions. The nanoparticles used in OSB to get used according to the invention microparticles, before polymerization alloyed dye, preferably a fluorescent dye, a rare earth element of the Periodic system or its connection or a radioactive compound or a radioactive element. For this relatively small if the ESCWA substances, to identify alloyed particles through the identification of their absorption, emission and/or scattering of electromagnetic radiation has become possible. Preferred are nanoparticles, doped, at least one fluorescent dye, such as polystyrene nanoparticles with the average diameter of which is from 20 to 300 nm, and a fluorescent dye, silicon nanoparticles, average diameter ranging from 20 to 100 nm, and at least one fluorescent dye. In addition, when implementing the BSA for stabilization of the emulsion can be used silica particles having the above diameter, doped with lanthanum, and/or terbium and/or cerium.

Examples of dyes that may be used according to the invention, are:

(a) water-insoluble dyes:

Floral 7GALambdachrome® No. 5550
(Lambda Chrom Laser Dyes company
Lambda Physik GmbH
Hans-Böckler-Str. 12, Göttingen)
Coumarin 47CAS No. 99-44-1
Coumarin 102 CAS No. 41267-76-9
Coumarin 6NCAS No. 58336-35-9
Coumarin 30CAS No. 41044-12-6
The fluorescein 27CAS No. 76-54-0
UraninCAS No. 518-47-8
Bis-MSBCAS No. 13280-61-0
DCMCAS No. 51325-91-8
Crazily purpleCAS No. 41830-80-2
Phenoxazone 9CAS No. 7385-67-3
HITCICAS No. 19764-96-6
I R 125CAS No. 3599-32-4
I R 144CAS No. 54849-69-3
HDITCICAS No. 23178-67-8
Carbonsteel 7Lambdachrome® No. 4220 (Lambda Physik GmbH)
Carbonsteel 3Lambdachrome No. 4350 (Lambda Physik GmbH)

(b) water-soluble dyes:

td align="left"> CAS No. 64339-18-0
RhodamineCAS # 81-88-9
Rhodamine 101
Rhodamine 6GCAS No. 989-38-8
Diamond sulfateabilifyCAS No. 2391-30-2
Rhodamine 19CAS No. 62669-66-3
Rhodamine 110CAS No. 13558-31-1
SulforhodamineCAS No. 2609-88-3
Nile blueCAS No. 53340-16-2
OxazinCAS No. 62669-60-7
Oxazin 1CAS No. 24796-94-9
HIDCICAS No. 36536-22-8
CryptocyanineCAS No. 4727-50-8
Furan 1Lambdachrome ® No. 4260 (Lambda Physik GmbH)
Stilbene 3Lambdachrome ® No. 4200 (Lambda Physik GmbH)
DASBTILambdachrome ® No. 5280 (Lambda Physik GmbH)

(C) reactive dyes:

DACITC*CAS No. 74802-04-3
DMACA, SE*CAS No. 96686-598
5-FAM, SE*CAS No. 92557-80-7
FITC 'Isomer I'*CAS No. 3326-32-7
5-TRITC; G isomer*CAS No. 80724-19-2
*) these dyes react with, for example, NH-groups

In order in accordance with the method GSP to get a practically water-insoluble polymer particles, the solubility of the polymers in water is <1 g/l, preferably <0.1 g/l at 20°C), according to (i) soluble in water monomethylethanolamine monomers are subjected to copolymerization with monomers containing at least two double bonds in the molecule. Examples of the water-soluble monomers are Ethylenediamine3-C6-carboxylic acids, such as acrylic, methacrylic, crotonic, maleic, Takanawa, vinylmania and etakrinova acid, and acrylamide-2-methyl-propanesulfonate, vinylsulfonate, styrelseledamot, vinylcarbazole and vinylphosphonic acid. Ethylenediamine acid can be used in partially or completely neutralized by bases, alkali or alkaline earth metal, or ammonia, or aminovymi compounds form. Preferred as the neutralizing agent used solution e is whom soda, a solution of sodium hydroxide or ammonia. Other suitable water-soluble monomers are acrylamide and methacrylamide. The monomers can be used alone or in mixture, as well as together with <20 wt.% water-insoluble monomers, such as Acrylonitrile, Methacrylonitrile or esters of acrylic and methacrylic acid.

The examples used in the GSP as a cross-linking agent monomer with at least two double bonds are N,N'-methylenebisacrylamide, divinylbenzene, divinities, esters of acrylic and methacrylic acid and at least diatomic alcohols, such as ethylene glycol, propylene glycol, butyleneglycol, hexanediol, glycerin, pentaerythritol and sorbitol, and alkylene glycols, molar mass MNwhich is from 100 to 3000, in particular polyethylene glycol and copolymers of ethylene oxide and propylene oxide. Preferred crosslinking agents are butanediol-1,4-diacrylate, butanediol-1,4-dimethacrylate, hexanediol-1,6-diacrylate, hexanediol-1,6-dimethacrylate, simple di - and triallylamine ether of pentaerythritol or a simple trailerby ether of sorbitol. When implementing BSA cross-linking agents are used, for example, in amounts of from 0.01 to 10 wt.%, preferably from 0.5 to 5 wt.%, in terms of the total amount of monomers used. Of course, in the implementation of gender is merisalo you can use two or more cross-linking agents.

In the implementation of BSA nanoparticles, doped, preferably a dye, for example, in amounts of from 0.01 to 20 wt.%, preferably from 0.1 to 5 wt.%, used as a stabilizer for emulsions. The resulting polymerization microparticles contain doped nanoparticles preferably on the surface. Microparticles can be separated from the suspension, for example, coagulation of the suspension or removal of volatile solvents.

Another method of receiving encoded microparticles is (ii) emulsion polymerization of water-soluble monomethylethanolamine monomers and from 0 to 10 wt.%, in terms of the mixture of monomers, at least one ethyleneamine monomer containing at least two double bonds in the molecule, and as an emulsifier to stabilize the dispersed phase also use doped nanoparticles in amounts used to make OSB according to (i). Doped nanoparticles are in or on the surface of the formed product of emulsion polymerization. Methods of emulsion polymerization are known. When this water-insoluble monomers will polimerizuet, for example, in the presence of radical initiators such as sodium persulfate, hydrogen peroxide or redox catalysts, to obtain t is ncoi dispersion polymers. To stabilize the emulsion used, as a rule, the connection, the HLB value of which is >7. Such compounds are, for example, With12-C18-alcohols, modified 5-50 moles of ethylene oxide per mole of alcohol, or salts of alkali metals and from sulphonated (>C12-alcohols with long chain. Emulsifiers, if necessary, use according to (ii). In the case of their number is, for example, from 0.1 to 10, preferably from 0.5 to 3 wt.%, in terms of subject to polymerization of the monomers.

Under water-insoluble monomers thus it is necessary to imply such Ethylenediamine compounds which form water-insoluble polymers. Solubility in water insoluble polymer is, for example, <1 g/l, more <0.01 g/L. Examples of such monomers are styrene, α-methylsterols, esters of acrylic and methacrylic acids and monohydroxy C1-C18-alcohols, preferably1-C4-alcohols, acrylamide, substituted C1-C20-alkyl groups and N-substituted methacrylamides, such as N-methylacrylamide, N-methylmethacrylate, N-ethylacetamide and N-athletically.

Water-insoluble monomers, if necessary, subjected to copolymerization with a small amount of water-soluble monomers and water-soluble mon the measures used in such quantity, that the resulting polymers are insoluble in water. If water-soluble monomers used for the modification of water-insoluble polymers, their number when carrying out emulsion polymerization is, for example, from 0.1 to 10, preferably from 0.2 to 5 wt.%. As the water-soluble monomers can be used is described in paragraph (i) monomers, such as, in particular, Ethylenediamine acid. The modification of the polymers can, for example, be necessary to introduce functional groups in the polymer to be used in sequential reactions.

In some cases, the required can be reduced solubility of the polymer in water and the enhancement of the mechanical properties of the products of polymerization. This is achieved through the implementation of polymerization of water-insoluble monomers in the presence of Ethylenediamine monomers containing at least two double bonds in the molecule. Such monomers, also referred to as cross-linking agents that have been specified above in paragraph (i). When carrying out emulsion polymerization according to (ii) they are used in the same quantities as in the implementation of the above-mentioned PCB. Examples of the crosslinked product of emulsion polymerization are polystyrenes, crosslinked divinylbenzene or balantiocheilos, as well as esters of acrylic and meth is krylovii acid, stitched pentaerythritol and/or pentaerythritoltetranitrate, such as cross-linked poly(n-butyl acrylate) or crosslinked poly(methyl methacrylate).

The average particle diameter of the polymer obtained by polymerization according to (ii)is, for example, from 10 nm to 1000 μm, preferably from 10 nm to 10 μm. Often he is from 500 nm to 30 μm, in particular from 1 to 20 μm. Obtained according to (ii) aqueous dispersions of polymers containing alloy nanoparticles microparticles dispersed in water. Doped microparticles can be obtained from aqueous dispersions of polymers by centrifugation or by destabilization of the dispersion by adding inorganic salts. Since the microparticles are in most cases used in dispersed form, then their separation from the aqueous dispersion plays a minor role.

The encoded microparticles are also radical polymerization according to (iii)at least one ethyleneamine monomer capable of copolymerization of dye containing Ethylenediamine double bond. Examples of such dyes containing one ethyleneamine communication are 4-(dicyanovinyl)julolidine (DCVW) and TRANS-1-(2'-methoxyphenyl)pyrene. These dyes may, for example, be used in the reverse suspension polymerization (i) and in emulsion polymerization (ii) as with the suits to encode the polymer particles. Especially in cases when the formation of polymer particles, the average diameter of which is 5 to 500 nm, priority for use of encoded microparticles may be agglomeration of particles to form aggregates, average particle diameter which is, for example, from 300 nm to 500 μm.

Encoded microparticles can be obtained according to (iv) agglomeration of at least two different groups of microparticles, notable for its absorption capacity, emission and/or scattering of electromagnetic radiation, up to units, the average particle diameter ranging from 300 nm to 500 μm, preferably from 400 nm to 20 μm. So, for example, silica particles, encoded fluorescent dye having an average diameter of from 5 to 500 nm, preferably from 20 to 100 nm, and cross-linked polystyrene modified with amino groups (using, for example, from 0.5 to 3 wt.% dimethylaminopropylamine in the polymerization of styrene), average particle diameter which is from 20 to 100 nm, doped with one of the above reactive dyes such as dye CAS # 96686-59-8, lead to the formation of the agglomerate, the average particle diameter is, for example, from 300 nm to 500 μm, preferably from 400 nm to 20 μm.

Preferred are encoded microparticles, the encoding of which the content is t, respectively, at least two different dye. To increase the amount of information used, for example, a mixture of two groups of encoded microparticles, the mixture contains one group of encoded microparticles and only one fluorescent dye and another group of encoded microparticles and the two differ from each other fluorescent dyes.

In addition, the amount of information can be improved also by using for marking materials a mixture of two groups of encoded microparticles, the mixture contains one group of encoded microparticles, for example, one fluorescent dye and another group of encoded microparticles and the two differ from each other reactive dyes. In addition, can be used, for example, a mixture of two groups of encoded microparticles, the mixture contains one group of encoded microparticles and one fluorescent dye and another group of encoded microparticles, and three or more different from each other and different from the dye groups And fluorescent dyes.

Another example of the labeling material is a mixture of two groups of encoded microparticles a and b, the mixture contains one group of encoded microparticles and two different fluorescent dyes, and another group In the coded microca the TCI and two deviating fluorescent dyes.

Another example of labeling is a mixture of two groups of encoded microparticles a and b, the mixture contains one group of encoded microparticles and two different fluorescent dyes, and another group of encoded microparticles, and three or more deviating fluorescent dyes. Another example is a mixture of two groups of encoded microparticles a and b, the mixture contains one group of encoded microparticles and three different fluorescent dyes and another group of encoded microparticles and three deviating fluorescent dyes.

Another example of coding is a mixture of five different groups of microparticles And-E, containing:

As a group of particles with three different dyes F1, F2 and F3

In the group of microparticles with dyes F1 and F2,

With a group of microparticles with dyes F1 and F3

D group of microparticles with dyes F4 and F5 and

E. the group of microparticles with dye F4.

In addition, an object of the present invention is the use of encoded microparticles obtained:

(i) polymerization of at least one ethyleneamine monomer in the presence of dyes and/or nanoparticles, if necessary, radioactively doped or alloyed with at least one dye or rare earth element of the Periodic system of the s to obtain microparticles, having an average diameter of 300 nm to 500 μm, or

(ii) agglomeration of at least two different groups of microparticles, varying absorptive capacity, emission and/or scattering of electromagnetic radiation, up to units, the average particle diameter ranging from 300 nm to 500 μm,

and always use a combination of at least two different groups of encoded microparticles, varying absorptive capacity, emission and/or scattering of electromagnetic radiation, for labeling materials.

Particularly preferably used microparticles encoded fluorescent dyes, as well as microparticles, coded reactive dyes. An important role is also played by microparticles encoded water-soluble dyes, and microparticles encoded water-insoluble dyes.

Identification of encoded microparticles possible using commercially available cytometric containing fluorescent spectrometer and/or photodetectors with appropriate filters. Identification of encoded microparticles is carried out, for example, by analyzing the fluorescence spectrum emitted by the radiation of selected wavelengths, and you can vary the wavelength causing the fluorescence emitted by the SV is the same. Suitable for the identification of encoded microparticles cytometry are, for example, cytometry company Partec GmbH Otto-Hahn-Str. 32, D-48161.

The above-described encoded microparticles used for marking materials, such as dispersions, coatings, paints, explosives, polymers, plant protection products, seeds, pharmaceutical products such as tablets, capsules, tinctures, or preparations containing the active substance, cosmetic products such as creams, lotions or shampoos, solutions, such as fuel and, in particular, oil, paper, in particular of packaging paper, banknote and security paper, and all marked objects, for example the chassis of the vehicle.

The invention also relates to materials containing encoded microparticles for labeling, we obtain:

(i) polymerization of at least one water-soluble monoethyleneglycol monomer in the presence of at least one ethyleneamine monomer containing at least two double bonds in the molecule by reverse suspension polymerization of water in the oil, and as a suspending agent used doped nanoparticles,

(ii) emulsion polymerization of water-insoluble monoethyleneglycol monomer and from 0 to 10 wt.%, in baresch the ones on the mixture of monomers, at least one ethyleneamine monomer containing at least two double bonds in the molecule, and as an emulsifier to stabilize the dispersed phase using doped nanoparticles,

(iii) polymerization of at least one ethyleneamine monomer capable of copolymerization of dye containing Ethylenediamine double bond, and, if necessary, the agglomeration of these particles or

(iv) the agglomeration of at least two different groups of microparticles, varying absorptive capacity, emission and/or scattering of electromagnetic radiation, up to units, the average particle diameter ranging from 300 nm to 500 μm.

If you combine the two groups of particles with different codes, get tool, via which you can make complex or hierarchical labeling. Of these mixtures, it is possible to extract a variety of information, analyzing them, for example, by fluorescence microscopy. Contained in mixtures of information to read on the basis of absorption, emission and/or spectrum of the dispersion of different fluorescent materials by known methods described, for example, in the literary sources of art.

So, for example, by combining different coded microparticles and the and by using multiple fluorescent substances for coding microparticles can accumulate a significant amount of information. If, for example, using coded so microparticles want to modify the marking of the product, on the basis of absorption, emission and/or spectrum of the scattering sample the labeled product can be recognized, for example, its manufacturer, place, date of manufacture and batch number.

When used as a coding means encoded microparticles, of course, must be compatible with the underlying coding materials, there are no required properties of the product, nor recognition of encoded microparticles should not be damaged.

EXAMPLES

Example 1

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
52,5 mgNaNO2
30 gillimitability
270 gmethylmethacrylate
0.06 gyellow fluorescent dye Gelb 083 (Lumogen® F)
15 ghexad the Cana

The mixture was dispersed for 30 min at a speed of 5000 rpm and then transferred to a 2 liter vessel with anchor stirrer. Type of 1.575 g of tert-butylperbenzoate and the tank is heated for 1 hour to 60°C. thereafter, the contents of the tank are heated for 2 hours to 70°C, then 30 min to 85°C and then at this temperature, allowed to stand for 1 hour. Add 7 g of a 10%aqueous solution of tert-butylhydroperoxide and within an hour, add a solution of 0.4 g of ascorbic acid in 20 g of water. In conclusion, the vessel is cooled to room temperature.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 2.0 μm and a narrow distribution of particle sizes with the monotony of 0.5, which is determined by the analysis of light scattering in the mie theory (analyzer type mastersizer company Malvern), and for particles selected index of refraction equal 1,49, and the index of absorption of 0. The solids content is 30,38 wt.%.

Example 2

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

441,45 gwater
45 gpolyvinyl alcohol (Mowiol® 15/79 (10% in water))
180 gCulminal® MHPC 100 (5% in water) methylhydroxypropylcellulose
52,5 mgNaNO2
30 gbutanediamine
270 gmethylmethacrylate
0.06 gyellow fluorescent dye Gelb 083 (Lumogen® F)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 2.6 μm and a narrow distribution of particle sizes with the monotony of 0.5. The solids content amounts to 29.6 wt.%.

Example 3

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpartially gidrauxilirovannogo polyvinyl alcohol (Mowiol® 40/88 (10% in water))
52,5 mgNaNO2
15 g illimitability
285 gmethylmethacrylate
0.01 gyellow fluorescent dye Gelb 083 (Lumogen® F)
0.01 gorange fluorescent dye (Lumogen® F Orange 240)
0.01 gred fluorescent dye (Lumogen® F - Rot 240)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with painted 3 fluorescent dye particles, and the particles have an average volume particle diameter of 1.8 μm and a narrow distribution of particle sizes with the monotony of 0.4. The solids content is 31.5 wt.%.

Example 4

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpartially gidrauxilirovannogo polyvinyl alcohol (Mowiol® 40/88 (10% in water))
52,5 mgNaNO2
30g illimitability
270 gmethylmethacrylate
0.06 gyellow fluorescent dye Gelb 083 (Lumogen® F)
0.03 gred fluorescent dye (Lumogen® F Red 300)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with painted 2 fluorescent dye particles, and the particles have an average volume particle diameter of 1.8 μm and a narrow distribution of particle sizes with the monotony of 0.5. The solids content is 31 wt.%.

Example 5

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
2.1 gNaNO2(2.5% in water)
30 gbutanediamine
270 gMatelot is crylate
0.09 gred fluorescent dye (Lumogen® F Rot 305)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 2.4 μm and a narrow distribution of particle sizes with the monotony of 0.5. The solids content is 33.4 wt.%.

Example 6

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
52,5 mgNaNO2(2.5% in water)
30 gillimitability
270 gmethylmethacrylate
0.03 gyellow fluorescent dye (Lumogen® F - Gelb 083)
0.06 gorange fluorescent dye (Lumogen® F Orange 24)
0.09 gred fluorescent dye (Lumogen® F - Rot)
15 ghexadecane

The mixture was dispersed for 60 min at room temperature at 6500 rpm and then transferred to a 2 liter vessel with anchor stirrer. Type of 1.575 g of tert-butylperbenzoate and the tank is heated for 1 hour to 65°C. thereafter, the contents of the tank are heated for 2 hours to 70°C, then 30 min to 85°C and then at this temperature, allowed to stand for 1 hour. Add 7 g of a 10%aqueous solution of tert-butylhydroperoxide and within an hour, add a solution of 0.4 g of ascorbic acid in 20 g of water. In conclusion, the vessel is cooled to room temperature.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter at 1.91 μm and a narrow distribution of particle sizes with the monotony of 0.5. The solids content amounts to 31.7 wt.%.

Example 7

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

502,7 gwater
30 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
120 gCulminal® MHPC 100 (5% in water)
methylhydroxypropylcellulose
52,5 mgNaNO2
120 gpotentialtarget
150 gmethylmethacrylate
30 gmethacrylic acid
0.06 gyellow fluorescent dye (Lumogen® F - Gelb 083)
0.015 ggidroaerodinamicheskogo ether
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 4.9 μm. The solids content amounts to 30.3 wt.%.

Example 8

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 g polyvinyl alcohol (Mowiol® 40/88 (10% in water))
2.1 gNaNO2(2.5% in water)
30 gillimitability
240 gmethylmethacrylate
30 gn-butyl acrylate
0.09 gred fluorescent dye (Lumogen® F Rot 305)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 2.1 μm and a uniformity of 0.4. Received 6 g coagulate the solids content of the dispersion are 29.9 wt.%.

Example 9

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

370,1 gwater
of 208.3 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
1,75 gNaNO2(2.5% in water)
25 gbutanediamine
225 gmethylmethacrylate
0.75 gethylhexylcarbonate
0.08 gred fluorescent dye (Lumogen® F Rot 305)
12.5 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 1.6 μm and a uniformity of 0.4. Received 6 g coagulate the solids content of the dispersion is 28.3 wt.%.

Example 10

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

0.09 g
450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
2.1 gNaNO2(2.5% in water)
1.35 gpotentialtarget
298,65 gmethylmethacrylate
red fluorescent dye (Lumogen® F Rot 305)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 1.9 μm and a uniformity of 0.5. The solids content of the dispersion amounts to 31.4 wt.%.

Example 11

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
2.1 gNaNO2(2.5% in water)
300 gmethylmethacrylate
0.09 gred fluorescent dye (Lumogen® F Rot 305)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 1, and the total number tert-butespecially divided into three equal parts. PE is a new part added at 60°C, the second part is at 65°C, and a third part at 70°C.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 1.5 μm and a uniformity of 0.4. Received 6 g coagulate the solids content of the dispersion is 31.3 wt.%.

Example 12

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
2.1 mgNaNO2
30 g1,4-potentialtarget
270 gmethylmethacrylate
0.09 gred fluorescent dye (Lumogen® F - Rot)
15 gvaseline oil (CAS 8042-47-5)

The mixture was dispersed for 30 min at room temperature at 5000 rpm and then transferred to a 2 liter vessel with anchor stirrer. Add 2.1 g of tert-butylperbenzoate and the tank is heated for 1 hour to 60°C. thereafter, the contents of the tank naked is ewout at least 2 hours to 70°C, then 30 min to 85°C and then at this temperature, allowed to stand for 1 hour. Add 7 g of a 10%aqueous solution of tert-butylhydroperoxide and within an hour, add a solution of 0.4 g of ascorbic acid in 20 g of water. In conclusion, the vessel is cooled to room temperature.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 1.2 μm and a wide distribution of particle sizes. The solids content is 27.6 wt.%.

Example 13

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
2.1 mgNaNO2
24 g1,4-potentialtarget
216 gmethylmethacrylate
0.09 gred fluorescent dye (Lumogen® F - Rot)
60 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out, as the description is about the case 12.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 1.2 μm. The solids content is 29,0 wt.%.

Example 14

A 2-liter tank with stirrer (diameter 5 cm) was placed a mixture of the following composition:

450 gwater
250 gpolyvinyl alcohol (Mowiol® 40/88 (10% in water))
2.1 mgNaNO2
30 g1,4-potentialtarget
270 gmethylmethacrylate
0.09 gred fluorescent dye (Lumogen® F - Rot)
15 ghexadecane

Emulsification of the mixture and the polymerization of the monomer is carried out as described in example 12.

Get the variance associated with colored fluorescent dye particles, and the particles have an average volume particle diameter of 1.2 μm. The solids content is 29,0 wt.%.

Examples for the application

The molar composition of paints for paper

In one-liter vessel on namenda stirrer, prepared, as shown in table 1, the molar paint. The pH values are about 9 and a viscosity adjusted to 1000 MPa·S.

Table
composition(1)(2)(3)(4)(5)(6)(7)
Caso3-Pigment (Hydrocarb 90)100,070,070,070,070,070,070,0
Clay-Pigment (Amazon 88)97,030,030,030,030,030,030,0
Dispersing agent (Polysalz S)45,30,030,030,030,030,030,03
NaOH25,00,05 0,050,050,050,050,05
Styrene-butadiene-binding Styronal® D80849,710,010,010,010,010,010,0
Thickener (Sterocoll®)40,50,300,300,300,300,300,30
Marking variance 130,91,00,50,20,10,0100,200
Marking variance 232,51,00,50,20,10,0100,400
Marking variance 331,11,00,5 0,20,10,0100.800 to

As adopted in the art the method of recording is given in the first column of the table below (1) the solids content of the used components. For each of the next six columns (2)-(7) are given for each example on the application of the relative concentrations based on 100 parts of pigment (in this case, Hydrocarbon 90 + Amazon 88).

As marking dispersion 1 used the dispersion obtained according to example 3.

Marking the variance 2 is obtained similarly to example 3, however, contains the same concentration of dye only the red fluorescent dye (Lumogen® F - Rot).

Paint paint is applied on the raw paper company Scheufelen using the squeegee, so that the applied weight was 15 g/m2.

Thus colored paper dried with a suitable drying apparatus. The naked eye cannot detect the marking paper with fluorescent labeled particles, but with the help of laser raster microscope we can uniquely determine all the types used for marking particles.

Marking paper size

Obtained according to the invention particles for labeling used in the surface treatment of paper. This marking is isperia 1, 2 and 3 are mixed with Basoplast® 400DS, standard dispersion of an acrylate copolymer and the mixture is kneaded in an aqueous solution of starch (the ratio of the synthetic product to starch is 1:100). The mixture contains from 8 to 15% solids, and in this form is applied in the form of a film on paper. The applied weight is 2 g/m2starch and 0.02 g/m2the polymer. Using a laser raster microscope could be unambiguously define all the types used for marking particles.

Marking coatings for films

In 1 kg of a 45%dispersion it acrylate Epotal®A 816 mixing 0.75 ml or 1.5 ml and 15 ml marking dispersion according to example 3 or similarly prepared dispersion and two-colored particles with the same total concentration of dye type Lumogen® F Red 300 or Lumogen® F Red 300 and Lumogen® F Orange 240 and the mixture through a pneumatic brushes apply to worr film (200 MB from ExxonMobil), which pre-electrically treated and covered with the first ground layer PU dispersion (Epotal® P 350). Using a laser raster microscope could be unambiguously define all the types used for marking particles.

1. The method of marking material encoded microparticles, characterized in that use encoded microparticles obtained
(i) polymerization of at least one vocarstvo is image monoethyleneglycol monomer in the presence at least one ethyleneamine monomer containing at least two double bonds in the molecule by reverse suspension polymerization of water in the oil, and as a suspending agent used doped nanoparticles, or
(ii) emulsion polymerization of water insoluble monomethylethanolamine monomers comprising from 0 to 10 wt.%, in terms of the mixture of monomers, at least one ethyleneamine monomer containing at least two double bonds in the molecule, and as an emulsifier to stabilize the dispersed phase using doped nanoparticles, or
(iii) polymerization of at least one ethyleneamine monomer capable of copolymerization of dye containing Ethylenediamine double bond, and, if necessary, the agglomeration of these particles,
moreover, when carrying out polymerization according to (i) and (ii) use nanoparticles, radioactively doped or alloyed, at least one dye or one compound from the group of rare earth elements of the Periodic system.

2. The method according to claim 1, characterized in that the average size of the polymer particles obtained by polymerization according to (i)is from 0.1 to 1000 microns.

3. The method according to claim 1, characterized in that the average particle diameter of the polymer, recip is controlled polymerization according to (i), is from 0.5 to 50 μm.

4. The method according to claim 1, characterized in that the average particle diameter of the polymer obtained by polymerization according to (i), is from 1 to 20 microns.

5. The method according to claim 1, characterized in that the average size of the polymer particles obtained by polymerization according to (ii)ranges from 10 nm to 1000 μm, preferably from 10 nm to 10 μm.

6. The method according to claim 1, characterized in that the average size of the polymer particles obtained by polymerization according to (ii)ranges from 500 nm to 30 μm.

7. The method according to claim 1, characterized in that the average size of the polymer particles obtained by polymerization according to (ii)ranges from 1 to 20 microns.

8. The method according to one of claims 1 to 7, characterized in that the quality of encoded microparticles using at least two different groups of microparticles, notable for its absorption capacity, emission and/or scattering of electromagnetic radiation.

9. Materials containing encoded microparticles for marking received
(i) polymerization of at least one water-soluble monoethyleneglycol monomer in the presence of at least one ethyleneamine monomer containing at least two double bonds in the molecule by reverse suspension polymerization of water in the oil, and as a suspending agent used Leger the bathrooms nanoparticles, or
(ii) emulsion polymerization of water insoluble monomethylethanolamine monomers comprising from 0 to 10 wt.%, in terms of the mixture of monomers, at least one ethyleneamine monomer containing at least two double bonds in the molecule, and as an emulsifier to stabilize the dispersed phase using doped nanoparticles, or
(iii) polymerization of at least one ethyleneamine monomer capable of copolymerization of dye containing Ethylenediamine double bond, and, if necessary, the agglomeration of these particles,
moreover, when carrying out polymerization according to (i) and (ii) use nanoparticles, radioactively doped or alloyed, at least one dye or one compound from the group of rare earth elements of the Periodic system.

10. The use of encoded microparticles obtained
(i) polymerization of at least one water-soluble monoethyleneglycol monomer in the presence of at least one ethyleneamine monomer containing at least two double bonds in the molecule by reverse suspension polymerization of water in the oil, and as a suspending agent used doped nanoparticles, or
(ii) emulsion polymerization is not rastvorimyv water monomethylethanolamine monomers, including from 0 to 10 wt.%, in terms of the mixture of monomers, at least one ethyleneamine monomer containing at least two double bonds in the molecule, and as an emulsifier to stabilize the dispersed phase using doped nanoparticles, or
(iii) polymerization of at least one ethyleneamine monomer capable of copolymerization of dye containing Ethylenediamine double bond, and, if necessary, the agglomeration of these particles,
when carrying out polymerization according to (i) and (ii) use nanoparticles, radioactively doped or alloyed, at least one dye or one compound from the group of rare earth elements of the Periodic system having an average diameter of 300 nm to 500 μm,
and in each case use a combination of at least two different groups of encoded microparticles, notable for its absorption capacity, emission and/or scattering of electromagnetic radiation, for labeling materials.

11. The use of claim 10, wherein the applied microparticles encoded fluorescent dyes.

12. The use of claim 10, wherein the use of microparticles, coded reactive dyes.

13. The use of claim 10, characterized those who, that apply microparticles encoded water-soluble dyes.

14. The use of claim 10, wherein the use of microparticles, coded not water-soluble dyes.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: present invention pertains to new photochromic monomers

Alk=CH3-C10H21 X=Cl, Br, I, F, NH2, CH2OH, CH2Cl, CH2Br, CHO, CO2H, method of obtaining them, photochromic polymers- polyazomethines, which are reversibly photocontrolled due to introduction into their structure, of dihetarylenthane class photochromic fragments.

EFFECT: obtaining new photochromic photocontrolled polymers for designing new information technologies.

8 cl, 25 dwg, 15 ex

FIELD: nonferrous metallurgy industry; aircraft industry; other industries; production of the heat-resistant alloys on the basis of the nickel.

SUBSTANCE: the invention is pertaining to the dispergated coloring agents intended for the ink-jet recording. The invention describes the dispergated coloring agent containing the coloring agent and the pseudo-finely-dispergated particles of the polarizable polymer having the dimension less, than the particles of the coloring agent. In the dispergated coloring agent the coloring agent itself and the particles of the polarizable polymer are attached to each other. At that the pseudo-finely-dispergated particles of the polarizable polymer contain the interpolymer consisting of the monomeric components containing, at least, one type of the hydrophobic monomer and, at least, one type of the hydrophilic monomer, where the hydrophobic monomer contains, at least, the monomer having the methyl group in α - position and the radically-polymerizable non-saturated double bond. The invention also describes the method of production of the indicated dispergated coloring agent and the water ink produced on its basis. The presented dispergated coloring agent has the high stability for a long time and practically in the absence of the surface-active substance or the dispergator. The ink produced on its basis has stability of blowout in the ink-jet printing method.

EFFECT: the invention ensures, that the ink produced on the basis of the presented dispergated coloring agent has the high stability of blowout in the ink-jet printing method.

20 cl, 14 dwg, 7 tbl, 15 ex

FIELD: chemistry of polymers, leather industry, chemical technology.

SUBSTANCE: invention relates to a method for preparing polymeric products that are used in processes for dressing leather or fur, in treatment and disinfection of natural and sewage waters. Method for preparing polymeric products involves the hydroxymethylation reaction of polyhexamethylene guanidine chloride with formaldehyde and arylation reaction of prepared product with aromatic compound comprising o-amino- or o-hydroxy-groups. The hydroxymethylation reaction is carried out in the presence of acetic acid or formic acid up to formation of trimethylol derivative of polyhexamethylene guanidine chloride. In some cases the arylation product is subjected for complex formation with transient metal salt or azo-coupling reaction with diazonium salt taken among group including sulfanilic acid, naphthionic acid, j-naphthyls, p-nitroaniline, 2,6-dichloro-4-nitroaniline. Invention provides simplifying, accelerating and enhancing the effectiveness of process in dressing leathers with derivatives of polyhexamethylene guanidine showing tanning effect, staining properties, flocculating capacity and high antibacterial activity.

EFFECT: improved preparing method.

3 cl, 1 tbl, 9 ex

The invention relates to the production of dye sintanol used for processing leather and fur
The invention relates to the production of the tanning agent used in the production of leather and fur

The invention relates to organic chemistry and is a new polymer-based 5,5'-methylenebisacrylamide aldehyde and diamine fluorophore General formula:

[=F=CH-C6H40-CH2-C6H40-CH=n,

where n= 6-9,

< / BR>
The claimed connection most effectively can be used as fluorescent additives in liquid and solid scintillators as active element in laser technology

The invention relates to the field of organic dyes, in particular to a method of obtaining polimerisation dyes containing in the molecule fragments of the polymer, i.e

The invention relates to the production of organic dyes, in particular to methods for oligomeric dyes primarystring

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of producing oligomers and a method of producing composite materials therefrom. Described is a method of producing styrene oligomers, homologues thereof, methylmethacrylate or mixture of acrylic and methacrylic esters, involving heating a monomer to 70-98°C for 15-60 minutes in the presence of a radical polymerisation initiator in amount of 0.001-0.5 wt % of the monomer until achieving viscosity of 500-2500 mPa·s, and then cooling and adding a polymerisation inhibitor in amount of 0.0005-0.05% of the weight of the monomer. Described also is a method of producing composite materials, characterised by that the oligomer produced using the above described method is mixed with a polymerisation initiator taken in amount of 0.1-4% of the mass of the oligomer and a mineral and/or polymer filler taken in amount of 60-90% of the reaction mass, followed by pressing and/or solidification of the obtained mass at temperature 10-100°C.

EFFECT: shorter oligomerisation time and obtaining an oligomer with longer storage time, obtaining composite material with improved physical-mechanical and technological parametres.

3 cl, 1 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to compositions prepared from polyesters and polyamides for making articles such as sheets, films, fibres, bottles and articles made via pressure casting. The composition contains crystallisable polyester and polyamide dispersed in the polyester. The polyester consists of 85% acid fragments obtained from terephthalic acid, 2,6-naphthalene dicarboxylic acid and diesters thereof. The polyamide consists of a repeating link of aminocaproic acid and a repeating A-D link. A is a residue of adipic acid, isophthalic acid, terephthalic acid, 1,4-cyclohexane dicarboxylic acid or naphthalene dicarboxylic acid or mixtures thereof, and D is a residue of m-xylene diamine, p-xylene diamine, hexamethylene diamine, ethylene diamine or 1,4-cyclohexane dimethyl amine or mixtures thereof. The polyamide has triamine content after hydrolysis less than 0.22, and content of carboxyl outside the range of 20-80% of total amount of terminal groups.

EFFECT: invention enables to obtain partitioned. granules without increasing relative viscosity and without gel formation.

14 cl, 2 tbl, 4 dwg, 16 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of recuperating unreacted monomers contained in a stream of residual gas formed during synthesis of a copolymer of vinyl ester and ethylene. Described is a method of producing copolymers containing vinyl ester or ethylene or ethylene unsaturated monomers via radical emulsion or suspension polymerisation in an aqueous medium at absolute pressure between 5 and 100 bars. At the end of polymerisation, the reaction mixture is throttled with reduction of its absolute pressure to 0.1-5 bars. Unreacted monomers are recuperated from the residual gas through multi-step fractionated condensation with deep cooling. At the first condensation step, water vapour is condensed at temperature ranging from -90 to -60°C, and at the third condensation step, ethylene is condensed at temperature ranging from 140 to 100 °C.

EFFECT: design of a method which enables extraction of valuable substances from the formed residual gas, where the said substances can be cheaply recycled.

9 cl, 2 dwg, 1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method for producing acrylate latex. Described is a method of producing acrylate latex, involving emulsion copolymerisation of acrylic monomers with ethylene-unsaturated comonomers in the presence of an emulsifying agent, characterised by that the emulsifying agent used is a cation-active emulsifying agent of cetyl pyridinium chloride or cetyl pyridinium bromide. Copolymerisation is carried out under the effect of gamma-radiation with power between 0.02 and 0.099 Gy/s until attaining absorbed dose of 3-4 kGy with monomer degree of conversion not lower than 99.8%.

EFFECT: obtaining aggregation- and sedimentation-resistant cation-active acrylate latex with positively charged latex particles.

3 cl, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method for producing acrylate latex. Described is a method of producing acrylate latex, involving emulsion copolymerisation of acrylic monomers with ethylene-unsaturated comonomers in the presence of an emulsifying agent, characterised by that the emulsifying agent used is a cation-active emulsifying agent of cetyl pyridinium chloride or cetyl pyridinium bromide. Copolymerisation is carried out under the effect of gamma-radiation with power between 0.02 and 0.099 Gy/s until attaining absorbed dose of 3-4 kGy with monomer degree of conversion not lower than 99.8%.

EFFECT: obtaining aggregation- and sedimentation-resistant cation-active acrylate latex with positively charged latex particles.

3 cl, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: wall has a layer which contains a polyamide dispersed in a crystallisable polyester and an agent which reduces interphase tension, selected from a group comprising lithium sulphoisophthlate and lithium sulphobenzoic acid. The polyamide contains a product of reacting aminocaproic acid with itself, or a product of reacting A-D, where A is a residue of adipinic, isophthalic, terephthalic, 1,4-cyclohexane dicarboxylic, resorcinol dicarboxylic or naphthalene dicarboxylic acid or mixtures thereof, and D is a residue of m-xylenediamine, n-xylenediamine, hexamethylenediamine, ethylenediamine or 1,4-cyclohexane dimethylamine or mixtures thereof. The polyester contains 85% links obtained from terephthalic acid or dimethyl ester of terephthalic acid. The wall does not contain cobalt compounds.

EFFECT: invention enables to obtain packed articles with high interphase bonding strength and low turbidity.

38 cl, 8 tbl, 5 dwg, 9 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a polymer dispersion which does not contain water and a volatile organic solvent, meant for preparing lubricant compositions for glass fibre and glasing glass fibre and structures from such fibres, particularly nets and fabric. The disclosed dispersion contains a product of polymerisation of at least one vinyl monomer in the presence of a radical initiator in a dispersion organic reaction medium represented by siloxanes, having at least one epoxy group in the terminal position. The dispersion contains 20-70 wt % polymer in form of fine, essentially spherical particles with size less than 40 mcm.The invention also discloses a method of preparing the dispersion, lubricating and glasing compositions, as well as glass fibre coated with said compositions.

EFFECT: dispersion has high polymer content and is stable in usual storage conditions.

28 cl, 1 tbl, 35 ex

FIELD: chemistry.

SUBSTANCE: invention can be used in chemical industry. The apparatus for polymerisation of olefins, particularly ethylene, has a gas-phase reactor with a fluidised layer, a gas recirculation line connected to the reactor for outlet and recirculation of the stream of recirculation gas; and a cyclone 3. The cyclone 3 has an upper section 3a, having an inlet opening 4 lying eccentrically relative the central axis, a middle section 3b, adjacent to the upper section 3a and a lower section 3c for outlet of solid particles released from the recirculation gas, which is adjacent to the middle section 3b. Inside the upper section 3a and part of the middle section 3b there is a vertical cylindrical pipe 5, which continues downwards and serves for outlet of the recirculation gas with low content of particles.

EFFECT: invention ensures good separation of finely dispersed particles from recirculation gas, while preventing accumulation of hot fine polymer particles.

10 cl, 2 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing perfluorinated polymers with sulfo-groups and is used in production of proton conducting ion-exchange membranes. The method involves copolymerisation of tetrafluoroethylene with perfluoro(3,6-dioxa-4-methyl-7-octene)sulfonylfluoride in the medium of an organic solvent - perfluoromethyl diethylamine at temperature 50°C and pressure 2.5-5 atm. The initiator used is bis(perfluorocyclohexanoyl)peroxide.

EFFECT: invention solves the problem of increasing molecular weight of a copolymer of tetrafluoroethylene with perfluoro(3,6-dioxa-4-methyl-7-octene)-sulfonyl fluoride and replacing the ozone-depleting solvent with an environmentally safe solvent.

2 dwg, 1 tbl, 13 ex

FIELD: chemistry.

SUBSTANCE: method is realised via copolymerisation of tetrafluoroethylene (TFE) and perfluro(3,6-dioxy-4-methyl-7-octene)sulfonylfluoride (FS141) in a medium of organic solvent. Copolymerisation is carried out in a medium of solvent - 1,2-dichlorohexafluorocyclobutane (RC 316) at pressure 2.5-5 atm using bis(perfluorocyclohexanoyl)peroxide as an initiator.

EFFECT: low explosion hazard of the process and replacement of the ozone-decomposing solvent by an environmentally safe solvent.

1 cl, 1 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of producing oligomers and a method of producing composite materials therefrom. Described is a method of producing styrene oligomers, homologues thereof, methylmethacrylate or mixture of acrylic and methacrylic esters, involving heating a monomer to 70-98°C for 15-60 minutes in the presence of a radical polymerisation initiator in amount of 0.001-0.5 wt % of the monomer until achieving viscosity of 500-2500 mPa·s, and then cooling and adding a polymerisation inhibitor in amount of 0.0005-0.05% of the weight of the monomer. Described also is a method of producing composite materials, characterised by that the oligomer produced using the above described method is mixed with a polymerisation initiator taken in amount of 0.1-4% of the mass of the oligomer and a mineral and/or polymer filler taken in amount of 60-90% of the reaction mass, followed by pressing and/or solidification of the obtained mass at temperature 10-100°C.

EFFECT: shorter oligomerisation time and obtaining an oligomer with longer storage time, obtaining composite material with improved physical-mechanical and technological parametres.

3 cl, 1 tbl, 10 ex

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