The method of obtaining heat-resistant polymers


(57) Abstract:

The invention relates to the chemistry of polymers, in particular a process for the production of thermostable polymers of polybenzamidazole used as coatings, molding compositions, adhesives for laminates, adhesives with high physical-chemical and mechanical properties. The essence of the invention: production method of heat-resistant polymers by the reaction of migration copolymerization of bismaleimide and amino derivatives in the melt, as the use of amino compound of the formula given in the description, where R' = -CH2-, -O-, -SO2- simple connection. The technical result is an increase in thermal stability of the polymer, the improvement of physical-mechanical characteristics and cheaper materials based on it. table 1.

The invention relates to a method for producing a thermostable polymers of polybenzamidazole suitable for use as coatings, molding compositions, adhesives for laminates, adhesives with high physical-chemical and mechanical characteristics.

The known method of synthesis of polybenzimidazole (Batirov I. Synthesis and study of polyimides based on 1,7-diphenyl-2,6-di(AMINOPHENYL)biometricheskikh tetracosanoic acids with diamines, containing pre-formed benzimidazole fragments. Polynicotinate obtained in the first stage in the solution of dimethylacetamide at room temperature for 10-12 h, have a large molecular weightAve= from 0.2 to 2.0 DL/g . The cyclization of polyamidation carry out thermal and chemical methods. According to the dynamic thermogravimetric analysis, polybenzimidazole have high heat resistance. However, obtaining products on the basis of these polymers by the methods of direct and injection molding, and their use as impregnating compositions is difficult because generated by thermal cyclization of volatile products, leading to the formation of defects, which significantly degrades the quality of the product.

The closest in technical essence and the achieved effect is a method of obtaining heat-resistant polymers (Ed. St. USSR N 879985, class C 08 G 73/18, 1981) adopted for the prototype based on bismaleimide and bisbenzimidazole with different substituents in the 2-position, but the resulting polymers have insufficient thermal stability and mechanical strength.

The aim of the invention is to improve the heat resistance of the polymer to improve the Li method for producing a heat-resistant polymers by the reaction of bismaleimide and amino, containing benzotryazolyl group, as the last use of the compounds of formula

< / BR>
where R'= -O-, -CH2-, -SO2- simple connection.

The reaction is carried out according to the following scheme:

< / BR>
where R = -CH2-; R'= -O-, -CH2-, -SO2- simple connection.

Synthesis of polymers was carried out in the melt at 190 - 210oC at different molar ratio of bis-benzotriazole (GBT) to bismaleimide (MEPI).

Application of the above method allows you to easily adjust the molecular weight of the resulting polymer by changing the ratio of initial reagents and the number of multiple bonds in the polymer. The prepolymers formed by the excess of bismaleimide, well soluble in organic solvents and soften at 98-110oC. Polymerization by multiple bonds in the process of thermal processing leads to the formation of crosslinked structures with high thermal stability and good physical and mechanical properties.

The resulting thermosets can be used to obtain products through direct and injection molding, and as binders for laminates and coatings.

Example 1. In the polycondensation tube, equipped with trubek) bisbenzimidazole. Then by passing the inert gas is removed from the air, the test tube is placed in a pre-heated up to 190oC metal bath and incubated for 5 minutes, the polymer Yield 94%. The softening temperature of the polymer is equal to 98-112oC.

In the infrared region of the spectrum observed absorption characteristic imenik cycles at 1700-1725 and 1780 cm-1, out-of-plane deformation vibrations of CH aromatic nuclei at 820 cm-1and the absorption at 3070 cm-1typical of H-C=C-H maleimide fragment.

Elemental analysis (calculated/found): H - 3,95/3,67; C - 69,18/68,85; N - 11,65/11,20 for composition C97H66N14O16.

According to the dynamic thermogravimetric analysis (5 deg/min, in air), the polymer loses 10% of its initial weight at 350-360oC.

Example 2. In the polycondensation tube contains tubes for input and output of inert gas, put the mixture 1,7918 g (0,005 mol) of diphenylethylenediamine and 0,62565 g (0,0025 mol) bisbenzimidazole. Then by passing the inert gas is removed from the air, the test tube is placed in a preheated 200oC metal bath and incubated for 10 minutes Yield floor is a mini-analysis (5 deg/min, on the air), the polymer loses 10% of its initial weight at 330-350oC.

Physico-mechanical properties termootdelenii polymers of General formula

< / BR>
presented in the table.

Using the proposed method to obtain polymers in comparison with the known advantages are the following:

1. The use of cheaper derivatives.

2. The production of composite materials with improved thermal and mechanical characteristics.

The method of obtaining heat-resistant polymers by the reaction of migration copolymerization of bis-maleimide and amino derivatives in the melt, characterized in that as the use of amino compounds of the formula

< / BR>
where R1= -CH2-, -O-, -SO2- simple connection.


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FIELD: polymer production.

SUBSTANCE: ,2-dihydro-2,2,4-trimethylquinoline polymer, useful as stabilizer against thermooxidative, atmospheric, and ozone-caused aging of rubbers, is obtained by condensation of aniline with 2.5-5.5 molar equivalents of acetone in an anhydrous medium in presence of hydrogen chloride catalyst under following conditions: pressure, temperature 85-105оС, content of chloride ion 1.5-2.3%, reaction time 5-12 h. After distilling away excess acetone, condensation product is polymerized for 4-12 h in presence of hydrogen chloride at 80-95оС and content of chloride ion in reaction mixture 7.5-11%. Polymer is recovered by neutralizing reaction mixture, extraction with nonpolar solvent, and separation polymer and monomer fraction from solvent.

EFFECT: lowered temperature conditions of process.

1 tbl, 24 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing 1,2-dihydro-2,2,4-trimethylquinoline used as an inhibitor of rubber aging agent. Polymer is prepared by condensation reaction of aniline with acetone in the presence of hydrogen chloride. The condensation product is polymerized in the presence of hydrochloric acid, neutralized with alkali followed by extraction of the end product from organic layer in the presence of toluene in the mole ratio of alkali to hydrogen chloride in reaction mass = (0.5-0.8):1 to form an aqueous and organic layers. Then the end product is isolated from an organic layer by distilling off the solvent. Method provides preparing 1,2-dihydro-2,2,4-trimethylquinoline polymer with the content of isopropylbianiline 0.04 wt.-%, not above.

EFFECT: improved method for preparing.

1 tbl, 12 ex

FIELD: medicine.

SUBSTANCE: invention describes an agent used in disinfection of skin integument and comprising polyguanidine compound as a disinfecting component and a solvent. As a disinfecting component polyguanidine compound is used, namely, poly-(4,9-dioxadodecane guanidine) phosphate or poly-(4,9-dioxadodecane guanidine) chloride, or polyhexamethylene guanidine citrate, or polyhexamethylene guanidine gluconate, or polyhexamethylene guanidine benzoate, or polyhexamethylene guanidine sebacate, or polyhexamethylene guanidine chloride, or a synergetic mixture of a polyguanidine compound with polyethylene pyrrolidinium chloride with molecular mass 50000-100000 Da taken in the ratio = 1:(1-10). As a solvent water or ethyl alcohol, or mixture of ethyl alcohol and water are used, and agent proposes additionally propylene glycol, polyethylene glycol and nutritive acid salt chosen from the group comprising citric acid sodium or potassium salt, or lactic acid sodium or potassium salt in the following ratio of components, wt.-%: above indicated polyguanidine compound or its synergetic mixture with polyethylene pyrrolidinium chloride with molecular mass 50000-100000 Da in the ratio = 1:(1-10), 0.5-3.0; polyethylene glycol, 0.1-1.0; propylene glycol, 1.0-10.0; nutrient organic acid salt, 0.1-1.5, and solvent, the balance. Invention can be used in surgery, obstetrics, cardiology for hygienic treatment of hands of surgeons and medicinal staff. Invention provides enhancing level and spectrum of the disinfecting agent, reducing its toxicity and negative effect on skin integuments.

EFFECT: improved, enhanced and valuable medicinal properties of agent.

1 tbl, 9 ex

FIELD: molecular biology.

SUBSTANCE: disclosed is molecular transfecting complex (MTC) comprising of plasmide DNA carrying necessary genetic information, polyethyleneimine, modifies with acylhydrazine groups and being capable to form ion complexes with plasmide DNA, ligand molecules for receptor-mediated MTC addressing to certain cell types and providing prolonged MTC circulation in blood. Ligand molecule contains one or more aldehyde groups, whereby such molecules may be attached after DNA-acylhydrazidopolyethyleneimine complex formation. Invention is useful in medicine for gene therapy.

EFFECT: complexes with prolonged storage life.

5 cl, 8 dwg, 10 ex

FIELD: chemistry.

SUBSTANCE: method includes polycondensation of α,ω-diamine with guanidine salt. Hydrophobic α,ω-diamine mixed with hexamethylene diamine or mixed with 4,9-dioxadodecadiamine H2N-(CH2)3-0-(CH2)4-0-(CH2)3-NH2 is used in the following ratio, % w/w: hydrophobic α,ω-diamine - 16-60, hexamethylene diamine or 4,9-dioxadodecadiamine - 84-40, and as a hydrophobic α,ω-diamine 1,10-decamethylene diamine H2N-(CH2)10-NH2 or 1,12-dodecamethylene diamine (H2N-(CH2)12-NH2 or N,N-bis-(3-aminopropyl) dodecylamine are used, biocide polyguanidine is obtained by the indicated method. It is characterized by hydrophilic and hydrophobic properties and is represented by the following formula: where n = 30-50, , R1 and R2 = H, CH3, C2H5, C4H9, C8H17, CH2C6H5.

EFFECT: invention allows to obtain water soluble products.

3 cl, 2 tbl, 25 ex

FIELD: inorganic chemistry.

SUBSTANCE: invention covers water soluble sizing compounds providing oil resistance/grease- and waterproofness applied for cellulose materials processing, containing repeated elements including polyamine with at least 3 nitrogen atoms in every repeated monomer element where amides are partially or completely substituted with a. cellulose interacting group resulted from reaction of polyamine and at least one reactive chemical compound selected from number including epihalohydrin, epiorganosulfonates and oxirane implying that interaction with cellulose arises after polyamine reaction or due to further reactivation; b. hydrophilic and hydrophobic fluorine-containing chemical group substituted with alkyl chain containing hydrophilic group; besides cellulose interacting group cross-links polyamine groups, and substance molecular weight Mw is from 10000 to 35000000 daltons determined by gel-penetrating chromatography relative to, polymethylmethacrylate standard. In addition invention covers chemical substance containing polymer composition with product of interaction between fluorocarbon-substituted polyamine of IV structure or epihalohydrin or epiorganosulfonate; method of sized paper production providing oil resistance/grease- and waterproofness (versions); paper production (versions); aqueous dispersion (versions). This substance effectively works providing oil resistant/grease- and waterproof sizing at high temperatures.

EFFECT: sizing compound production providing oil resistance/grease- and waterproofness of cellulose materials.

36 cl, 20 tbl, 125 ex

FIELD: chemistry.

SUBSTANCE: invention relates to new organic polymers, in particular, to unsaturated polyoxims which can be used for producing polyamines, polyamides, chelating agents and other chemical products and can form a basis for preparation of medical products, antioxidants, pigments, hermetics and catalysts. The invention proposes an unsaturated polyoxims of the general formula: [-CH2)a-(R)C(R1)-]m-[-(CH2)b-CH(R2)-C(=NOH)-CH(R3)-(CH2)c-]n-[-(CH2)b-CH(R2)-C(=O)-CH(R3)-(CH2)c-]p-[-CH2-C(R2)=C(R3)-CH2-]q, where m=0-547, n=2-19, p = 0-17, q = 1-680; R, R1, R2, R3 are hydrogen, halogen, alkyl, phenyl or cyanic group, while a, b and c are integers from 0 to 3. The invention comprises also the method of producing the aforesaid unsaturated polyoxims consisting in interaction of unsaturated polymer with nitrogen protoxide at 50 to 350°C and nitrogen protoxide of 0.01 to 100 atm in organic solvent with subsequent processing by hydroxylamine at 10 to 90°C and atmospheric pressure in organic solvent or in heterophase system "organic solvent-water".

EFFECT: production of new unsaturated polyoxims with controlled three types of groups, ie oxym, carbonyl and dual bond C=C, expanding their applications.

12 cl, 13 ex

FIELD: chemistry.

SUBSTANCE: invention refers to polymer ligand with athranilamide main-chain units and to metal polymer complex wherein polymer ligand forms luminescent complexes with rare earth ions. Polymer ligand is described with the general formula -(A-B)m-: where A is a fragment of methylene-bis-anthranilic acid, B is a fragment of dicarboxylic acid chosen from dicarboxylic acid series, R= -(CH2)6-, -(CH2)7-, -(CH2)8-, m refers to values MM within 80 kDa to 200 kDa. Metal polymer complex based on polymer ligand is described with the general formula -(A-B)m-Me: , where A is a fragment of methylene-bis-anthranilic acid, B is a fragment of dicarboxylic acid chosen from dicarboxylic acid series,

, m refers to values MM within 80 kDa to 200 kDa, Me is rare-earth metal from the group including Tb3+ and Eu3+, in ratio metal ion: metal polymer complex, wt % 0.3-3.9.

EFFECT: invention allows for high-strength metal polymer complex of improved thermal stability and luminescence intensity.

2 cl, 2 tbl, 12 ex, 6 dwg

FIELD: chemistry.

SUBSTANCE: present invention relates to new organic polymers of a range of unsaturated polyoximes, which can be used for obtaining polyamines, polyamides, chelating agents, for making medicinal agents, antioxidants, pigments and sealing compounds. Description is given of unsaturated polyoxime with general formula: [-(CHR1)x-CR2=CH-(CHR3)y-]a-[-(CHR1)x-CHR2-C(=O)-(CHR3)y-]b-[-(CHR1)x-CHR2-C(=NOH)-(CHR3)y-]c-[-R4-]d, where: x, y - ranges from 1 to 12; a - from 1 to 2000; b - 0 - 2000; c - from 2 to 2000;d - from 1 to 2000; R1, R2, R3 - hydrogen, alkyl or halogen; R4 - [-CH(C6H5)-CH2-] or [-CH(CN)-CH2-]. Unsaturated polyoxime is obtained from reacting unsaturated polyketone with hydroxylamine at 5-100°C and atmospheric pressure in an organic solvent or a heterophase organic solvent - water system.

EFFECT: unsaturated polyoximes, in contrast to known saturated polyoximes, widen the scope of modifying polymer and potential areas of their use.

8 cl, 10 ex

FIELD: chemistry.

SUBSTANCE: method of producing copolymers of polyguanidine salts involves treating polyguanidine chloride with a metal compound in an alcoholic solvent, separating the formed metal chloride precipitate through filtration, mixing the filtrate and acid with formation of a copolymer of polyguanidine salts, and subsequent drying the desired product. The polyguanidine chlorides used have general formula , where R is alkylene with straight and branched structure with C4-C12, oxaalkykene[-CH2-]P O[-CH2-]q, dioxaalkylene [-CH2-]P O[-CH2-]q O[-CH2-]r, trioxaalkylene [-CH2-]pO[-CH2-]q O[-CH2-]r O[-CH2-]s, tetraoxaspiroalkylene , n ranges from 2 to 1000; p, q, r, s assume values from 2 to 12, the metal compound used is potassium hydroxide, the alcoholic solvent used is a mixture of ethanol and rectificate with isopropanol in ratio (100-30):(0-70), where the said alcoholic solution of potassium hydroxide is mixed with dry crushed polyguanidine chloride, mixture of organic or mineral (except hydrofluoric) mono- or polybasic acid or mixture acid with filtrate is done after vacuum distillation of alcohol from the filtrate at pressure ranging from 0.1 to 0.2 atm and temperature from 50 to 60°C. Copolymers of polyguanidine salts of general formula: , where R is alkylene with straight or branched structure with C4-C12, oxaalkylene [-CH2-]P O[-CH2-]q, dioxaalkylene [-CH2-]p O[-CH2-]q O[-CH2-]r, trioxaalkylene [-CH2-]P O[-CH2-]q O[-CH2-]r O[-CH2-]s, tetraoxaspiroalkylene, where (n-x): x=19:1-1:19; n=2-100; p, q, r, s assume values from 2 to 12, A is an anion of organic or mineral (except hydrofluoric) mono- and polybasic acid or a mixture of acids.

EFFECT: improvement of method.

3 cl, 4 ex, 4 tbl

Antifriction coat // 2345110

FIELD: chemistry.

SUBSTANCE: antifriction coat can be used in gear pumps for reducing friction and wear resulted from corrosion or mechanical effects in tribojoints under effects of chemically active reagents, high temperature and loads on engaged parts to ensure required stable gaps between the said parts. The antifriction coat consists of three layers, i.e. inner, intermediate and upper layers. Note here that the inner layer represents a composition comprising 90 wt % of a polyimide varnish and 10 wt % of chromophosphatealuminic bond, the intermediate layer being made from 100 wt % of a pure polyimide varnish. Finally, the top layer represents a composition containing 90 wt % of polyimide varnish, 8 wt % of colloid graphite and 2 wt % of lecithin. Thickness of the aforesaid inner layer is within the limits of from 8 up to 10 mcm, thickness of the intermediate layer is within the limits of from 16 up to 20 mcm, thickness of the top layer is within the limits of from 24 up to 30 mcm, while the required thickness of the coat is provided by grinding the top layer.

EFFECT: longer life of friction assembly units and parts operated in chemically active environments.

2 tbl

FIELD: chemistry.

SUBSTANCE: composition for fixing wrapping articles contains A) 1-60 wt % of at lest one resin of α,β-unsaturated polyether based on at least one unsaturated mono-, di- or tricarboxylic acid and/or substance containing molecules with mono-, di- or tricarboxylic acid groups, at least one polyol, B) 0.1-80 wt % of at least one inorganic and/or an organic-inorganic hybrid component, having functional groups for reaction with components A) and C), where said hybrid components are polymers or colloidal solutions based on silicon, titanium or zirconium and oxygen atoms, which contain hydroxyl and/or alkoxy groups and/or hydroxyalkyloxy groups and/or organic fragments, which have epoxy and/or isocyanate and/or unsaturated groups, C) 2-80 wt % of at least one monomer and/or oligomeric unsaturated component, which is styrene, vinyl toluene, hexanediol dimethacrylate, butanediol dimethacrylate and/or (meth)acrylates of products of a polyaddition reaction of ethylene oxide with trimethylolpropane capable of reaction with components A and B, and D) 0-15 wt % conventional additives, where wt % is calculated relative the total weight of the composition.

EFFECT: excellent heat conductivity properties and high level of electrical insulation along with excellent adhesion and thermal stability.

6 cl, 1 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to use of nanomaterials in wire enamel for improving thermal properties of enamel. The nanomodified wire enamels are usually used in making insulated winding wire. The polymer base of wire enamel is selected from a group comprising polyamideimide, polyester, polyesterimide, polyurethane and mixtures thereof. The nanomaterial is selected from a group comprising nano-oxides, metal nano-oxides, metal oxides or hydroxides of aluminium, tin, born, germanium, gallium, lead, transition metals, lanthanides, actinides and mixtures thereof. The nanomaterial is also selected from a group comprising nano-oxides, metal nano-oxides, metal oxides and hydroxides of aluminium, silicon, titanium, zinc, yttrium, vanadium, zirconium, nickel and mixtures thereof. After applying enamel on the wire and curing thereof, the wire exhibits improved thermal and mechanical properties.

EFFECT: improved thermal properties of enamel.

8 cl, 6 tbl

FIELD: chemistry.

SUBSTANCE: invention is aimed at aqueous binding solutions for primer coat of antistick coatings based on polyamideimide, polyether imide, also including water, amine and one or more solvents selected from acetoacetamides, guanidines, or mixtures of acetoacetamides and guanidines.

EFFECT: technical result is obtaining stable aqueous binding compositions with suitable toxicity profile and a good adhesion to substrate and good wear resistance.

6 cl, 3 tbl, 21 ex

FIELD: chemistry.

SUBSTANCE: method comprises (a) depositing without depositing the intermediate pigmentiferous primer-surfacer imparting colour to the base coat composition and (b) depositing a curable unpigmented coat composition on the mentioned base coat layer, wherein the base coat layer is formed by depositing a curable aqueous composition comprising (i) a continuous phase comprising water and (ii) a dispersed phase comprising: (A) polymer particles comprising carboxyl functional group comprising ethylenically unsaturated monomers containing ethylenically multi-unsaturated monomer. Mentioned ethylenically multi-unsaturated monomer is present in an amount of 2-30 wt % based on the total weight of the ethylenically unsaturated monomers and (B) polycarbodiimide.

EFFECT: ensuring base coat composition which is cured during the dehydration stage resulting in a high degree of cure prior to depositing coating varnish, which allows to cure the coating varnish at a lower temperature.

1 dwg, 2 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: antiscuff coating is made from the composition, containing the following components (in weight percent): the organic binder of 30%-60%, the solid lubricant of 30%-60%, the corrosion inhibitor of 6%-15%, the levelling agent of 0.01%-0.1%, the wetting agent 0.01%-0.1% and in addition the mixture of solvents. The organic binder is the liquid polyamide-imide resin with the solids content of 38-42%. The solid lubricant is any substance from the molybdenum disulphide and tungsten disulphide or the combination of molybdenum disulphide or tungsten disulfide with polytetrafluoroethylene. Preferably, the solid lubrication and the corrosion inhibitor are the surface-modified with the silane bonding agent. The antiscuff coating is obtained by spraying the coating on the surface of the threaded joint of pump-compressor and casing tubes, treated with phosphate; thus avoiding the environmental contamination with the heavy metal powder, contained in the threaded grease.

EFFECT: production of coatings that have good antiscuff and anticorrosive properties.

7 cl, 8 dwg, 16 ex