The method of obtaining antistatic polyurethane

 

(57) Abstract:

Usage: in the chemical industry, in particular to obtain an antistatic polyurethane. The inventive method to produce these polymers is in the interaction of isocyanate prepolymer based on toluene diisocyanate and simple or complex polyester with aromatic diamines and/or butanediol or polyoxyethyleneglycol in the environment of N, N-diethylhydroxylamine in the presence of chloride monovalent copper. table 1.

The invention relates to the chemistry of polymers, namely, anti-static polyurethane, which can be used for the manufacture of anti-static products and coatings, in particular for lining shafts of the paper machines.

A method of obtaining antistatic polyurethane by reacting the chloride of divalent cobalt solvent (acetone, tetrahydrofuran, butyl acetate) with 2,4-diisocyanate in a molar ratio of reagents, respectively 1:(5-15) for 1.5-6 hours the reaction mixture is injected into simple or complex the polyester, and then the solvent is distilled off and the reaction mass is heated for 30 min at 120aboutWith under vacuum, the project is a method for antistatic polyurethane by reacting isocyanate component and connections, containing active hydrogen atoms, in the presence of bivalent copper chloride in a solvent, where the isocyanate component using 2,4-toluylenediisocyanate, as compounds containing active hydrogen atoms is a simple or complex polyester and the solvent of bivalent copper chloride - acetone or tetrahydrofuran. The method is realized by the interaction of bivalent copper chloride in a solvent with 2,4-diisocyanate in a molar ratio of reagents, respectively 1:(6-15) for 4-10 h, the resulting reaction mass is injected into simple or complex polyester. The number of source reagents chloride divalent copper, 2,4-toluylene diisocyanate and simple or complex polyester - for the synthesis of anti-static polyurethane respectively 1,74-3,48 wt.h., 20,9-28,0 wt.h., 100 wt.h. Then the solvent is distilled off and the reaction mass is heated for 30 min at 120aboutWith under vacuum, the resulting product is poured into the form and receive castable polyurethane products (2).

The disadvantages of this method are the low shore hardness (56 srvc.ed.) and high rates of residual deformation (8%), and the duration of the process and large deposits antistatic polyurethane roll covers machines in the paper industry.

The aim of the invention is to increase the hardness and decrease the residual deformation antistatic polyurethane, as well as reducing the duration of their production process and reducing the amount of solvent used.

This objective is achieved in that in a method of producing an antistatic polyurethane by reacting isocyanate component and compounds containing active hydrogen atoms, in the presence of bivalent copper chloride in the solvent as the isocyanate component using the isocyanate prepolymer based on toluene diisocyanate and simple or complex polyester with mol.m. (1-2)103as compounds containing active hydrogen atoms of aromatic diamines and/or butanediol or polyoxyethyleneglycol mol.m. 106-1558, and the solvent is N,N-diethylhydroxylamine, when the mass ratio of bivalent copper chloride to N, N-diethylhydroxylamine equal to (0.5 to 1.5):1.0 and to the isocyanate prepolymer to 0.16 to 3.0% by weight of the prepolymer.

The invention is carried out as follows.

P R I m e R 1. 0.15 g of ferrous chloride copper dissolved in 0.15 g of N, N-diethylhydroxylamine, i.e., when the mass ratio of chloride dohale the(2,0 mol) of 2,4-toluylene diisocyanate and sampled at 74.25 g (1.0 mol) of polyether - polyoxyethyleneglycol (mol.m. 1000) type the bivalent copper chloride (in an amount of 0.15 wt.% by weight of prepolymer) in N,N-diethylhydroxylamine, and lead the interaction in 80aboutC for 5 min under vacuum, then add 16,19 g of methylene-bis-(0-Chloroaniline). The reaction mass is stirred at 80aboutC for 5 min under vacuum and then poured into molds. Form with the polymer mass is placed in a heat chamber at 115-120aboutC and incubated for 24 h

P R I m e R s 2-3. The method is carried out analogously to example 1, the difference is the mass ratio of chloride of divalent copper to the isocyanate prepolymer in percent by weight of the prepolymer (see table).

P R I m e R 4. The method is carried out analogously to example 2, the difference is the mass ratio of bivalent copper chloride to N,N-diethylhydroxylamine (see table).

P R I m e R 5. 1.0 g of ferrous chloride copper dissolved in 0,67 g of N, N-diethylhydroxylamine, i.e., when the mass ratio of bivalent copper chloride and N,N-diethylhydroxylamine of 1.5:1.0 in. In 100 g of isocyanate prepolymer obtained by the interaction 14,59 g (2.0 g mole) of 2,4-toluylene diisocyanate and 85,41 g (1.0 mol) of a compound of polyester - polyethyleneglycoladipinate (mol.m. 2037) add the interaction at 80aboutC for 5 min under vacuum, then add to 1.77 g of 1,4-butanediol and 10,07 g of methylene-bis-(0-Chloroaniline). The reaction mass is stirred at 80aboutC for 5 min under vacuum and then poured into molds. Form with the polymer mass is placed in a heat chamber at 155-120aboutC and incubated for 24 h

P R I m e R s 6-7. The method is carried out analogously to example 5. The difference is the mass ratio of chloride of divalent copper to the isocyanate prepolymer in percent by weight of the prepolymer (see table).

P R I m e R 8. The method is carried out analogously to example 5, the difference is the mass ratio of bivalent copper chloride to N,N-diethylhydroxylamine (see table).

P R I m e R 9. 3.0 g of ferrous chloride copper dissolved in 2.0 g of N, N-diethylhydroxylamine, i.e., when the mass ratio of bivalent copper chloride to N,N-diethylhydroxylamine of 1.5:1.0 in. In 100 g of isocyanate prepolymer obtained by the interaction 25,75 g (2,0 mol) of 2,4-toluylene diisocyanate and sampled at 74.25 g (1.0 mol) of polyether - polyoxyethyleneglycol (mol.m. 1000) add the bivalent copper chloride (in an amount of 3.0 wt.% by weight of prepolymer) in N,N-diethylhydroxylamine and keep interaction at 80aboutC for 5 min under vacuumoperated at 80aboutC for 5 min under vacuum and then poured into molds. Form with the polymer mass is placed in a heat chamber at 115-120aboutC and incubated for 24 h

P R I m e R s 10-11. The method is carried out analogously to example 9, the difference is the mass ratio of chloride of divalent copper to the isocyanate prepolymer in percent by weight of the prepolymer (see table).

P R I m e R 12. 1.0 g of ferrous chloride copper dissolved in 0,67 g of N, N-diethylhydroxylamine, i.e., when the mass ratio of bivalent copper chloride to N,N-diethylhydroxylamine of 1.5:1.0 in. In 100 g of isocyanate prepolymer obtained by the interaction 14,51 g (2,0 mol) of 2,4-toluylene diisocyanate and 85,41 g (1 mol) of a compound of polyester - polyethyleneglycoladipinate (mol.m. 2037), add the bivalent copper chloride (in an amount of 1.0 wt.%) by weight of prepolymer) in N,N-diethylhydroxylamine and keep interaction at 80aboutC for 5 min under vacuum, then add 3,96 g of 1,4-butanediol and of 1.33 g of diethylene glycol. The reaction mass is stirred at 80aboutC for 5 min under vacuum and then poured into molds. Form with the polymer mass is placed in a heat chamber at 115-120aboutC and incubated for 24 h

P R I m e p 13. 3.0 g of ferrous chloride copper to radaxian of 1.5:1.0 in. In 100 g of isocyanate prepolymer obtained by the interaction 25,75 g (2,0 mol) of 2,4-toluylene diisocyanate and sampled at 74.25 g (1.0 mol) of polyether - polyoxyethyleneglycol (mol.m. 1000) add the bivalent copper chloride (in an amount of 3.0% by weight of prepolymer) in N,N-diethylhydroxylamine and keep interaction at 80aboutC for 5 min under vacuum, then add to 1.60 g of m-phenylenediamine and 13,82 g of methylene-bis-(0-Chloroaniline). The reaction mass is stirred at 80aboutC for 5 min under vacuum and then poured into molds. Form with the polymer mass is placed in a heat chamber at 115-120aboutC and incubated for 24 h

P R I m e R 14. Obtaining antistatic polyurethane according to the method prototype. 2,69 g (0,02 mol) of ferrous chloride copper dissolved in 100 ml of acetone and subjected to interaction with 27,44 g (0,30 mol) of 2,4-toluylene diisocyanate (molar ratio of reagents 1-15) within 6 hours

In 100 g of polyether - polyoxyethyleneglycol - enter the resulting reaction mixture, acetone is distilled off and the reaction mass is heated for 30 min at 120aboutWith under vacuum and then poured into molds. Form with the polymer mass is placed in a heat chamber at 90aboutC and incubated for 24 h


263-75 shore a Durometer Hardness;

270-75 - residual deformation;

270-75 - tear Resistance and volume resistivity and specific surface electric resistance according to the method Dobrovolsky C. N., Kralovec A. N. The determination of the specific resistance and the permanent Hall on samples, dual samples van der Bau // Physics and technics of semiconductors. 1979. So 13. N 2. S. 386-389.

The results of electrical and physico-mechanical test antistatic polyurethane obtained by the present method and the method prototype, presented in the table.

According to the data given in the table, it is seen that the hardness of samples obtained by the present method, the above average by 20.E., and the residual strain is 2-3 times lower compared to the samples obtained by the method prototype, the duration of the process is reduced about 15 times, and also reduces the amount of used solvent on average 300 times.

At the same time, indicators of tensile strength at break of samples obtained by the present method do not differ materially from that index in samples obtained by the method prototype.

The METHOD of OBTAINING Antistaticity, in the presence of bivalent copper chloride in a solvent, characterized in that, to increase the hardness and reduce the residual deformation antistatic polyurethane, as well as reducing the duration of their production process and reduce the amount of solvent used as the isocyanate component using the isocyanate prepolymer based on toluene diisocyanate and simple or complex polyester (mol.m. 1000 - 2000, as compounds containing active hydrogen atoms, aromatic diamines and/or butanediol or polyoxyethyleneglycol mol.m. 106 - 1558, and the solvent is N, N-diethylhydroxylamine when the mass ratio of bivalent copper chloride and N,N-diethylhydroxylamine (0.5 to 1.5) : 1, and the number of bivalent copper chloride 0.15 to 3.0% by weight isocyanate prepolymer.

 

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2 cl, 1 tbl

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13 cl, 6 ex, 4 tbl

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27 cl, 16 ex, 8 tbl, 3 dwg

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1 cl, 6 tbl

FIELD: chemistry.

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EFFECT: possibility of simple obtaining of transparent varnish coatings with high resistance to crack formation under atmospheric impact and perfect resistance to scratching, which do not cause any ecological problems.

15 cl, 2 tbl, 4 ex

FIELD: chemistry.

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EFFECT: possibility to obtain transparent varnish coating with high resistance to formation of cracks under atmospheric impact and perfect resistance to scratching.

18 cl, 4 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to thermally solidificated covering substances based on aprotic solvents. Claimed is covering substance, which contains at least one compound (A), which contains hydroxyl groups, at least one compound (B) with free and/or blocked isocyanate groups, and at least one catalyst (D) for cross-linking silane groups, with one (i) or several components of covering substance containing hydrolysed silane groups and (ii) covering substance can be finally solidificated for covering, which has statistically distributed regions of lattice Si-O-Si. Obtained from covering substance solidificated coating has index of further cross-linking (PCI) lower than 2, with index of the further linking (PCI) being determined as coefficient from memory module E'(200) of finally solidificated coating, measured at 200°C, to minimum of memory module E'(min) of finally solidificated covering, measured at temperature higher than temperature of transition into glass-like state of Tg, and memory modules E'(200) and E'(min),as well as temperature of transition into glass-like state Tg are measured on free films with thickness of layer 40 mcm+/-10 mcm by means of dynamic mechanical thermal analysis (=DMTA) at rate of heating 2 K per minute and frequency 1 Hz and DMTA measurement on free films with thickness of layer 40 mcm+/-10 mcm, which are solidificated for 20 minutes at object temperature 140°C and after solidifying are kept for 8 days at 25°C, before carrying out DMTA measurements. Polyisocyanate (B) at least partially has one or several similar or different structural units of formula -X-Si-R"XG3-X, where G = identical or different hydrolysed groups, in particular alcoxy group, X=organic residue with from 1 to 20 carbon atoms, R" =alkyl, cycloalkyl, aryl or aralkyl, and carbon chain can be broken by non-adjacent oxygen groups, sulphur or NRa, with Ra=alkyl, cycloalkyl, aryl or aralkyl, x=0 to 2. Catalyst (D) is phosphorus-containing, and covering substance contains catalyst (D) from 0.1 to 10 wt % in terms of non-volatile components of covering substance. Also claimed are multi-step method of applying coating with application of claimed covering substance, as well as application of claimed method and versions of claimed coating application.

EFFECT: possibility to obtain transparent varnish coating with high resistance to atmospheric impact.

18 cl, 4 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing coating material. Disclosed is a method of producing coating material in form of powdered lacquer or a fluid resin, characterised by that one or more alcohols or polyols react with one or more silanes selected from a group consisting of (isocyanatomethyl)methyl-dimethoxysilane, 3-isocyanatopropyl-trimethoxysilane and 3-isocyanatopropyl-triethoxysilane, to form a covalent bond between the alcohol or polyol and the silane such that the reaction product is a high-molecular weight silane which is cured directly using a catalyst, wherein all alcohol or polyol organic functional groups participate in the reaction with the silane organic functional group. Coating material and use thereof are also disclosed.

EFFECT: disclosed method enables to obtain coating material which can be used to make scratch-resistant coatings.

12 cl, 4 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a coating agent containing (a) at least one binding substance (A) with reactive hydroxyl groups, (b) at least one cross-linking agent (B) having free and/or blocked isocyanate groups which, during cross-linking, can react with the reactive groups of the binding substance (A), and at least one catalyst (C) for the cross-linking silane groups, said catalyst being a phosphoric acid compound, specifically phosphoric acid or a phosphoric acid compound blocked with a bicyclic amine having the value pKb ≥ 3 and boiling point > 100°C. One or more components (A) and/or (B) and/or at least another component of the coating agent contain hydrolysable silane groups.

EFFECT: obtaining scratch-resistant and weather-resistant coatings.

17 cl, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to compositions of adhesive, suitable for binding polymer with metal and compounds used in them. Claimed are compounds of the structures given below , in which n has values 1-2; a equals 1-3 and b equals 0-2; but if a=3, b=0; if a=2, b=1; so that, at least, one alkoxy group is present; R1 is selected from H and C1-C2 alkyl, and where, when a>1, at least, one of R1 is not hydrogen; R2 is selected from C1-C2 alkyl; X and Y can represent O; and R3 represents residue, containing nitrobenzene, quinone dioxime or quinone oxime. Also claimed are: oligomer of said composition, compositions for binding element with natural or synthetic caoutchouc, method of binding said substrates and obtained product.

EFFECT: possibility if obtaining caoutchouc/metal compound, long-lasting at relatively high mechanical tensions and atmospheric impact.

13 cl

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