Adhesive composition, method of treating reinforcing layers and method of producing reinforced polymeric products using said composition

FIELD: chemistry.

SUBSTANCE: invention relates to an adhesive composition in form of an aqueous dispersion with content of solid substance from 1 to 50 wt %, as well as to a method of treating reinforcing layers with said composition, particularly a cord for tyres, and to a method of producing reinforced polymeric products by treating reinforcing layers. The adhesive composition contains: (a) 0.001-5 mol epoxide compound with molecular weight 50-290 in a form dissolved in water, per 1000 g of the overall composition, (b) 0.1-20 wt % completely or partially blocked isocyanate in form of a solid substance, (c) 0.1-40 wt % resorcin-formaldehyde latex in form of a solid substance and (d) water.

EFFECT: preparation of an adhesive composition which can be used in form of a single-step system, having good wettability and good adhesion, and high rate of reaction with non-activated fibres, particularly on polyethyleneterephthalate fibres.

15 cl, 1 ex, 2 tbl

 

This invention relates to adhesive compositions for the treatment of reinforcing layers, which are used to obtain reinforced polymer products, the adhesive composition contains dissolved epoxy compound.

It is proved that when receiving fibre reinforced rubber products, it is preferable to use a binder to improve the adhesion between a reinforcing layer of fabric and rubber. The use of such a bonding agent is important, in particular in the field of cord for tires and other designed for heavy duty composite material with reinforcing fibers. The current level of technology, in particular for this application, it is known that compounds of synthetic fibers rubber products used resorcinol-formaldehyde-latex (RFL) system.

Thus, the process can be done or single-stage or two-stage method. In practice, it has been shown that only two-stage method substantially satisfactory results, particularly in the case of non-activated polyester fibers. In the two-stage procedure, first, in the first stage, carry out the activation of the fibers so that the latter were covered with an epoxy compound and/or isocyanate. Usually this is achieved through water dis is version, in which the isocyanate and/or epoxy compound is contained with a certain solids content. After this first stage, second stage, carry out the application of resorcinol-formaldehyde latex system. Using this two-stage method, the first stage ensure full activation of the fibers, so that the epoxy compound and/or isocyanate leads to the formation of active functional groups on the fiber surface, and the second stage can then be processed by latex. Processing RFL likewise carried out in a water dispersion.

However, the two-stage method is complicated from the point of view of process technology, as well as complex is the provision of two different dispersions and work with them.

Thus, attempts to carry out processing in the form of a one-step method were unsuccessful. Single-stage systems are described, for example, in US 2002/0122938, as well as in the US 3419450. In practice, however, it was impossible to carry out one-step impregnation, that is, the use of aqueous dispersions RFL, as well as epoxy compounds and isocyanate, even to the activated fibers. Activated fibers are fibers that have already been provided with a coating, such as epoxy compounds, immediately after fabrication. In the case shall the applications of these methods thus pre-activated fiber again handle any dispersion. In the US 2002/0122938 proposed to use a single-stage system, which also contains a special epoxy compound in addition to RFL and isocyanate. However, in the US 2002/0122938 epoxy compound is also found in the form of solids in the dispersion. The disadvantage of this single-stage system is that it cannot be applied to neaktivirovannye fibers, and that the results obtained with the already activated fibers, in particular in relation to wettability and adhesion, are unsatisfactory.

On this basis, the objective of the invention is to provide adhesive composition that can be applied in the form of a single-stage system; however, suggest that this adhesive composition has good wetting and good adhesion, and high speed of response to non-activated fibers, in particular fibers PET. Another objective of this invention is to offer an appropriate way of obtaining such a composition and to specify how to use it.

The task in relation to adhesive compositions are solved by the distinguishing signs on paragraph 1 of the claims, and in the way - with the help of distinctive signs on paragraph 13 of the claims. Dependent claims reveal preferential options for implementation of the invention.

Thus, the according to this invention proposed, the adhesive composition for one-step processing of reinforcing layers to obtain reinforced polymer products, in which the epoxy compound is contained in dissolved form with a concentration of from 0.001 to 5 mol per 1000 g of the total composition, while the isocyanate and RFL continue to be in the form of solids. The applicant was able to show that it is possible to work with such a composition in which the epoxy compound is present in dissolved form, in one way, and at the same time to achieve the advantages of the previous two-stage system, namely the selectivity in respect of the coating. However, the adhesive composition according to this invention not only leads to selective wetting, i.e. the first is the activation of the fiber, and then the subsequent application of solids contained in the dispersion, but when the adhesive composition according to this invention, in addition, achieve excellent adhesion to untreated polyester cords against rubber. In addition, it was shown that the application of the compositions of this invention is the reduction of penetration depth, so that it is possible to reduce the concentration of glue. The consequence of this is that covered cord has a lower stiffness and, therefore, better stability.

In the case of adhesive compositions according to this invention it is preferable that the concentration of the epoxy compounds ranged from 0.002 to 0.2 mol/1000 g of the total composition. Suitable epoxy to connect enemy, which are dissolved in the dispersion, are, in particular, those that have a molecular weight of from 50 to 2000. Particularly preferred are epoxy compounds with a molecular mass of from 50 to 1000, most preferred with a molecular mass of from 50 to 290, in particular, water-soluble polyglycidyl ethers, epoxy-Novolac resins, polyfunctional alkylene epoxy compounds, diglycine ethers and bisphenol-based resin. However, this invention also includes all epoxy compounds listed in EP 1221456 A1.

The adhesive composition according to this invention has a solids content of 1 to 50 wt.%, preferably from 1 to 30% wt. The size of particles present in the dispersion, that is, the isocyanate is less than 5 microns.

Thus, the proportion of solids in the dispersion is from 0.1 to 20% wt. isocyanate and 0.1 to 40 wt.%. RFL. Preferably the composition contains from 0.1 to 10% wt. isocyanate and from 10 to 25% wt. RFL in the form of solids.

In addition, it has been shown that the adhesive composition is the predominant, if the isocyanates used 4,4-diisocyanatobutane (DHS) and/or colorvision (TDI), and/or naphthylisocyanate (NIDS). However, the invention of course also includes all other known isocyanates that can be used is to use for the adhesive compositions of this type. In this respect, by means of example, reference is made to U.S. patent 2002/0122938 A1 and described there diisocyanates.

It was shown that in the isocyanates according to this invention are preferred blocking agents, in particular isocyanate blocking the lactam. Examples of these agents are ε-caprolactam, δ-valerolactam. However, this invention includes, of course, other known blocking agents. This oximes, for example, methylethylketoxime (butanonoxime), metiletilketoksim, cyclohexanone. Monophenol, such as phenol, resorcinol, cresol, trimethylphenol, tert-butylphenol. Primary, secondary and tertiary alcohols, ethers, glycols, light anal-forming compounds such as, for example, acetoacetic esters, acetylacetone, derivatives of malonic acid. Secondary aromatic amines. Imides, mercaptans, triazoles.

In the adhesive compositions of this invention can also achieve an additional increase in the reaction rate due to the fact that add the catalyst in the form of a metal link. Thus, as catalysts-metal compounds suitable compounds of such metals as sodium, potassium, cesium, strontium, silver, cadmium, barium, cerium, uranium, titanium, chromium, tin, antimony, manganese, iron, cobalt, Nickel, copper, zinc, lead, calcium and/or zirconium. If soy is inany preferred metals are zinc compounds. Thus, suitable compounds are zinc acetate, zinc sulfate, zinc carbonate, zinc oxide, zinc acetylacetonate and/or zinc chloride. Particularly preferred is zinc acetate. The catalyst is present in the dispersion in the dissolved form, with its concentration of from 0.0001 to 0.1 mol/1000 g of composition.

Resorcinol-formaldehyde-latex system (RFL), which is used according to this invention, is known in itself at this level of technology.

In addition, this invention relates to a method for processing reinforcing layers to obtain reinforced polymer products (paragraph 13 of the claims). In the case of the method according to this invention using the adhesive composition described herein previously. In the case of this method, the adhesive composition can also be prepared shortly before the planned application by mixing the individual components. Thus, no matter in what form are the individual components, that is, it is also possible to pre-mix two or more components.

However, in this invention it is essential that the adhesive composition was applied to one-step method, that is, all components must be present before treatment in the form of a water dispersion and/or solution. To achieve the technical result is insignificant, the extent to which this aqueous dispersion prepared in the form of a homogeneous composition for quite a long time to use individual components were mixed shortly before use.

In addition, the applicant was able to show that the adhesive composition according to this invention is suitable in particular for the processing of the raw polyester fibers. It was possible to achieve excellent rates of reaction, which were significantly higher speeds, previously known from comparative systems, and at the same time was obtained a good degree of wetting.

Hereinafter the invention is explained in more detail with reference to an example implementation.

Example

Was obtained adhesive composition for impregnation according to this invention, the composition of which is given in Table 1.

Table 1
The composition for one-step impregnation
The components of the composition for impregnationNumberThe solids content
Lactam blocked MDI29,35 g29,35 gby 5.87%
Polyglycidyl ether110,65 g10,65 g2,13%
RFL 2260,87 g60,00 g12,00%
Deionized water199,13 g
Total:500,00100,00 g20,00%
1present in dissolved form
223% in deionized water

Inactivated cord of PET processed simultaneously by the two-stage impregnation in a known manner and by impregnation according to this invention the composition shown in Table 1. In the case of the two-stage impregnation was applied composition known in the prior art. When you first impregnation as a blocked isocyanate used Grilbond®IL-6 50% F, and as the epoxy compound - Grilbond®G1701 EMS-Primid AG, Switzerland. The variance for the second stage was a product of condensation of resorcinol-formaldehyde resin and butadiene-styrene-vinylpyridine latex.

In Table 2 the comparison of the results of both impregnation.

Table 2
The two-stage impregnationOne-step impregnation
CompositionlL-6+ G17012,7%11,7%1
RFL6,3%15,8%1
PropertiesAdhesion255
1Gain impregnation: the amount of a binding agent for PET imaging after coating.
2Floor cord rubber: 1=0-20%; 2=20-40%; 3=40-60%; 4=60-80%; 5=80-100%.

1. The adhesive composition in the form of a water dispersion with a solids content of 1 to 50 wt.% for processing reinforcing layers to obtain reinforced polymer products containing
a) from 0.001 to 5 mol of epoxy compounds with molecular weight 50-290 in dissolved form per 1000 g of the total composition,
b) from 0.1 to 20 wt.% fully or partially blocked isocyanate in the form of solids,
C) from 0.1 to 40 wt.% the resorcinol-formaldehyde latex (RFL) in the form of solids,
g) water.

2. The adhesive composition according to claim 1, characterized in that the solid content in the society ranging from 5 to 30 wt.%.

3. The adhesive composition according to claim 1, characterized in that it contains from 0.002 to 0.20 mol of epoxy compounds in the dissolved form per 1000 g of the total composition.

4. The adhesive composition according to claim 1, characterized in that the epoxy compound selected from the group polyglycidyl ethers, epoxy-Novolac resins, polyfunctional alkilinity epoxy compounds, ethers of diglycine and bisphenol-A-based resins.

5. The adhesive composition according to claim 1, characterized in that it additionally contains as a catalyst of from 0.0001 to 0.1 mol of compound of the metal in the dissolved form per 1000 g of the total composition, with the specified connection metal is a compound of zinc selected from zinc acetate, zinc acetylacetonate, zinc oxide, zinc chloride, zinc carbonate and/or zinc sulfate.

6. The adhesive composition according to claim 1, characterized in that the isocyanate is blocked by the lactam.

7. The adhesive composition according to claim 1, characterized in that the isocyanate is chosen from 4,4-diisocyanate-difenilmetana (DHS) and/or colordistance (TDI) and/or afterdetente (NIDS).

8. The adhesive composition according to claim 1, characterized in that it contains additional additives and/or dispersing agents.

9. The adhesive composition according to claim 1, characterized in that it contains from 0.1 to 10 wt.% blocked or partially blocked isoci the Nata in the form of solids and 10 to 25 wt.% RFL in the form of solids.

10. The adhesive composition according to one of claims 1 to 9, characterized in that the diameter of the solid particles isocyanate is <5 μm.

11. The processing method of reinforcing layers, in particular cord for tires, for the production of reinforced polymer products, characterized in that the treatment is carried out, the adhesive composition in accordance with at least one of claims 1 to 10.

12. The method according to claim 11, characterized in that the handle inactivated cord for tires.

13. Method for the production of reinforced polymer products by processing the reinforcing layers, characterized in that the specified treatment is carried out, the adhesive composition in accordance with at least one of claims 1 to 10, which is obtained immediately before processing by mixing the individual components.

14. The method according to item 13, wherein the adhesive composition is prepared by mixing component (C) (RPL) with the structure already present in the form of a mixture of components (a), (b) and (d).

15. The method according to item 13 or 14, characterized in that the handle inactivated cord for tires.



 

Same patents:

FIELD: technological processes.

SUBSTANCE: invention is related to production technology of synthetic cord, in particular, to impregnation and thermal treatment of aramid cord, and may be used in tyre and rubber industry. Aramid cord of all brands is impregnated with latex-resorcin-formaldehyde or latex-resorcin-formaldehyde-soot compounds on the basis of latexes "ДБА"-1, "СКД"-1s and 5% solution of resin "СФ"-282, with concentration of 12-14%. Then cord is thermally treated to residual moisture of 0.5-1.0% at 120-140°C with load of 400-800 kg/cloth. Cord produced by this method is repeatedly impregnated and thermally treated according to the same modes.

EFFECT: simplified treatment of aramid cord; reduction of power inputs; improvement of its physical-mechanical properties and increase of operability of tyres and rubber items.

1 tbl

FIELD: fire-protection; oil-and-gas industries; petrochemical industry; production of the multilayer fire-protection materials.

SUBSTANCE: the invention is pertaining to the field of production of the multilayer fire-protection materials and may be used for manufacture of the special purpose fire-protective clothing for the workers acting in the highly inflammable aerosphere - the fire fighters, the employees of the refueling stations and in the oil-and-gas industries. The multilayer fire-protection material is made in the form of the packet containing the outer layer made out of the heat-resistant fibers, the intermediate thermo-insulating layer, the inner layer made out of the cotton fabric and the hydraulic insulating layer located between the intermediate thermo-insulating layer and the outer layer. The hydraulic insulating layer is made in the form of the polymeric composition consisting of (in mass shares): 60-75 - chlorosulfonated polyethylene, 25-40 - the chloroprene rubber, 5-100 - the mineral inactive filler, 0.5-15 - the fire-retardant agent, 1-10 - the vulcanization accelerators, 5-15 - the tri chloroethylphosfate and 200-400 - the dissolvent. As the mineral inactive filler may be used kaolin, as the fire retardant - antimony trioxide, as the vulcanization accelerator - magnesium oxide. As the dissolvent they may use the mixture of the butyl acetate and toluene taken in the ratio of 1:1. The produced multilayer fire-proof material has the high flame resistance and the flex stability, the low abradability of the hydraulic insulating layer and also stability of the vulcanization production process at the multilayer fire-protection material manufacture.

EFFECT: the invention ensures production of the multilayer fire-protection material, which has the high flame resistance, the flex stability, the low abradability of the hydraulic insulating layer and stability of the vulcanization production process at the multilayer fire-protection material manufacture.

5 cl, 1 tbl, 3 ex

FIELD: fire-protection; oil-and-gas industries; petrochemical industry; production of the multilayer fire-protection materials.

SUBSTANCE: the invention is pertaining to the field of production of the multilayer fire-protection materials and may be used for manufacture of the special purpose fire-protective clothing for the workers acting in the highly inflammable aerosphere - the fire fighters, the employees of the refueling stations and the oil-and-gas industry. The multilayer fire-protection material is made in the form of the packet containing the outer layer made out of the heat-resistant fibers, the hydraulic insulating layer, the intermediate thermo-insulating layer and the inner layer made out of the cotton cloth. The hydraulic insulating layer is applied on the outer surface of the outer layer and made in the form of the polymeric composition consisting of (in mass %): 80-95 - the chlorosulfonated polyethylene, 5-20 - the chloroprene rubber, 5-100 - the mineral inactive filler, 0.5-15 - the fire-retardant agent, 1-10 - the vulcanization accelerator and 200-400 - dissolvent. As the mineral inactive filler may be used kaolin, as the fire retardant - antimony trioxide, as the vulcanization accelerator - magnesium oxide. As the dissolvent they use the mixture of butyl acetate and toluene taken in the ratio of 1:1. The produced multilayer fire-protection material has the high flame resistance, the flex stability and the frost resistance, the reduced rigidity and high efficiency of manufacture.

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5 cl, 1 tbl, 3 ex

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2 tbl, 4 ex

FIELD: rubber industry.

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FIELD: fire-resistant materials.

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1 tbl, 7 ex

FIELD: general mechanical rubber goods and tires.

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1 tbl, 4 ex

FIELD: production of fireproof materials and protective textile materials possessing specific properties.

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1 tbl, 5 ex

FIELD: textile industry.

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4 dwg, 2 tbl, 3 ex

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The invention relates to the production of textile materials, coated, namely the production of fabrics, for the manufacture of sports goods

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3 cl, 4 tbl

FIELD: rubber industry.

SUBSTANCE: invention relates to technology of manufacturing rubber reinforcement cord. Cord coating composition comprises first rubber latex, phenol resin, and water-soluble resorcinol-formaldehyde condensation product. Weight percentages of first rubber, phenol resin, and condensation product based on solid components of composition lie in ranges: 30 to 95, 0.01 to 30, and 2 to 15, respectively. First rubber is a nitrile group-containing high-saturated polymer rubber characterized by iodine number 120 or lower. Water-soluble condensation product belongs to novolak type.

EFFECT: increased bend resistance and size stability at room temperature and high temperatures.

10 cl, 1 dwg, 6 tbl, 5 ex

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12 cl

Polymer composition // 2395542

FIELD: chemistry.

SUBSTANCE: invention relates to polymer compositions, particularly to rubber mixtures for making tyre treads and can be used in the tyre industry. The polymer composition contains the following components, in pts. wt: polybutadiene rubber SKD 20-30, polyisoprene rubber SKI-3 70-80, zinc oxide 4-5, technical carbon N339 50-55, oleic acid 1.5-2.0, sulphur 1.5-2.2, sulfenamide T 1.0-1.5, diaphene PP 1.0-1.5, Pikar hydrocarbon resin 2-3, oil PN-6s 10-15, Omsk-10 wax 1.5-2.0, acetonanyl N 1.5-2.0, santogard PVI 0.1-0.15, 3-15 mm long pieces of waste hybrid saturated cords 1.5-20.0.

EFFECT: increased extension elongation, bouncing elasticity and lower brittleness temperature.

2 cl, 4 tbl

FIELD: chemistry.

SUBSTANCE: present invention pertains to rubber industry, particularly to composite material based on rubber mixtures, containing methylstyrene and divinyl rubber, and can be used for making sluper and rail pad shock-absorbers of railway tracks. Compound contains the following components, wt %: crushed rubber coated polyamide cord with fibre length 10-15 mm-17.0-18.5, rubber compound based on methylstyrene and divinyl rubber, containing a vulcanising group and inactive technical carbon - 77-78, particulate filler material-granulated sphate spew from the stage of vulcanisation of the shock-absorber pads-2, granulated rubber crumbs - 2.0-3.5.

EFFECT: increase in the resources of working capacity of the cushion bolsters, friction coefficient on the steel per-unit-volume of resistance of the electric current.

2 tbl

FIELD: chemistry.

SUBSTANCE: present invention pertains to the technology of making chemical fibre, particularly to a two-stage method of saturating synthetic fibre. The fibre is first saturated with water, and then with resorcin-formaldehyde latex. The preliminary saturating mixture contains blocked isocyanate with at least, trifunctional isocyanate groups and latex, in which the weight ratio of the blocked isocyanate to the latex ranges from 9 to 0.7. The mixture also contains water, emulsifier and a 2-vinylpyridine copolymer. The composite product consists of rubber and fibre or cord. The fibre or cord has, on parts of the surface, (1) blocked isocyanate with trifunctional isocyanate groups, (2) resorcin-formaldehyde latex adhesive and (3) rubber compound, vulcanised in situ.

EFFECT: possibility of carrying out the fibre or cord saturation process for production of composite technological products in ecologically clean conditions without use of toxic substances, without reducing the quality of the product.

17 cl, 3 tbl, 2 ex

FIELD: rubber industry.

SUBSTANCE: invention relates to technology of manufacturing rubber reinforcement cord. Cord coating composition comprises first rubber latex, phenol resin, and water-soluble resorcinol-formaldehyde condensation product. Weight percentages of first rubber, phenol resin, and condensation product based on solid components of composition lie in ranges: 30 to 95, 0.01 to 30, and 2 to 15, respectively. First rubber is a nitrile group-containing high-saturated polymer rubber characterized by iodine number 120 or lower. Water-soluble condensation product belongs to novolak type.

EFFECT: increased bend resistance and size stability at room temperature and high temperatures.

10 cl, 1 dwg, 6 tbl, 5 ex

FIELD: mechanical rubber goods.

SUBSTANCE: invention, in particular, relates to a method for improving direct adhesion between adhesive-activated textile reinforcing material and activated rubber, to compositions of textile reinforcing materials, and to articles in the form of thread, cord, or cloth. Material is activated with gluing substance based on halohydroxyl or epoxide resin. As-deposited coating composition is fixed on material, imbedded into activated rubber, and cured at suitable temperature for suitable time. Coating composition contains at least one hydroxyl aromatic compound with at least two hydroxyl groups or phenol-formaldehyde resin compound and at least one polydiene.

EFFECT: increased adhesion with rubber and improved dynamic fatigue characteristics of rubber article.

58 cl, 22 tbl, 20 ex

FIELD: manufacture of reinforcing components introduced into rubber-based articles: drive belts, hoses and automobile tires.

SUBSTANCE: proposed method includes submergence of complex carbon fibers into impregnating bath filled with solution of resorcinol-formaldehyde resin and rubber latex followed by drying and twisting the fibers which are spread beforehand for obtaining increased developed surface of each fiber.

EFFECT: complete and smooth impregnation of reinforcing components; enhanced strength parameters of articles.

20 cl, 9 ex

FIELD: manufacture of composite materials based on thermoplastic matrix and used in mechanical engineering for producing of friction parts and units.

SUBSTANCE: method involves treating carbon graphite filament with 1-2%-solution of fluorine-containing oligomer with molar weight of 2000-5000, or "Epilam" for 5-10 min, followed by thermal processing at temperature of 373±5 K for 0.5-1.0 hour or in corona discharge field at voltage of 10-40 kV for 1-5 min.

EFFECT: increased strength and tribotechnical characteristics of composite materials based on thermoplastic matrix and carbon fillers.

1 tbl, 4 ex

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