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Polythioether ketone imide terpolymer and preparation method thereof

A technology of polysulfide ketone imide terpolymer and phthalimide is applied in the field of preparation of the polysulfide ketone imide polymer, and can solve difficult equimolar ratio, narrow processing window, sodium sulfide Easy to oxidize and other problems

Active Publication Date: 2011-04-27
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005]Although polysulfideimide has advantages such as those mentioned above, compared with traditional polymers, its higher cost and narrower processing window limit its wide application
In order to reduce costs, the following preparation method is disclosed, see Patent No. ZL02104269.1 Chinese invention patent "Preparation method of dichlorophthalimide and dichlorobenzophenone or dichlorodiphenyl sulfone copolymer" (authorized announcement No.: CN1171930C), this patent uses disubstituted phthalimide and dichlorodiphenyl sulfone or dichlorobenzophenone to copolymerize with sodium sulfide as coupling agent, but because sodium sulfide is easy to oxidize, it is difficult to realize the polycondensation reaction during polymerization Equimolar ratio, so the viscosity of the resulting copolymer is lower

Method used

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  • Polythioether ketone imide terpolymer and preparation method thereof
  • Polythioether ketone imide terpolymer and preparation method thereof
  • Polythioether ketone imide terpolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] In a 250ml three-necked flask, add 5.29g (0.01mol) 4,4'-bis(4-chloroimide) diphenyl ether, 2.51g (0.01mol) 4'4-dichlorobenzophenone, 0.67g ( 0.021mol) of sulfur, 5.67g (0.063) of paraformaldehyde, 1.68g of sodium hydroxide, 0.50g of calcium chloride, add 100ml of N-methylpyrrolidone (solid content: 8%) after deoxygenation with nitrogen three times, and heat to 150°C After reacting for 5 hours, after cooling to room temperature, 0.11 g of chlorobenzene was added, and then heated to 180° C. for 3 hours of reaction, and the reaction solution was cooled to room temperature for aftertreatment.

[0059] Slowly pour the reaction solution into methanol and stir for 2 hours, filter and boil with water for 1 hour, filter, wrap the filter cake with filter paper, extract it with a mixed solution of ethanol and acetone in Soxhlet extraction for 24 hours, and then extract The obtained polymer was baked in a vacuum oven at 200° C. for 48 hours.

[0060] The intrinsic viscosity of the...

Embodiment 2

[0062] Add 54.85g (0.100mol) 3,4'-bis(4-nitroimide) diphenylmethane and 48.04g (0.100mol) 3,3'-bis(3-fluoroimide) into a 1000ml three-necked flask Amine) biphenyl mixture, 27.22g (0.100mol) 4,4'-dinitrobenzophenone, 9.14g (0.285mol) sulfur, 21.56g (0.57mol) sodium borohydride, 41.46g potassium carbonate, 5.23g Sodium iodide, add 4000ml dimethyl sulfoxide and 1000ml xylene (solid content: 13.7%) after deoxygenating with argon three times, heat to 180°C and react for 20 hours, cool to room temperature and add 3-nitrodi The benzophenone was then heated to 200° C. for 1 hour reaction, and the reaction solution was cooled to room temperature for aftertreatment.

[0063] Slowly pour the reaction solution into ethanol and stir for 2 hours, filter and boil with water for 2 hours, filter, wrap the filter cake with filter paper, extract it with a mixed solution of ethanol and acetone in Soxhlet extraction for 24 hours, and then extract The obtained polymer was baked in a vacuum oven at...

Embodiment 3

[0066] Add 22.22g (0.04mol) 2,2'-(4,4'-bis(3-chloroimide) diphenyl) isopropane and 14.17g (0.03mol) 3,3' in a 500ml three-necked flask - a mixture of bis(3-fluoroimide)benzophenone, 2.18g (0.01mol) 3,3'-difluorobenzophenone and 4.47g (0.01mol) bis(4-(4-chlorobenzene Keto) phenyl) ether mixture, 2.88g (0.09mol) sulfur, 5.04g (0.09) reduced iron powder, 9.07g sodium bicarbonate, 0.3g18-crown-6, add 300mlN after argon deoxygenation three times, N-dimethylformamide was heated to 180° C. for 20 hours, and then 20 ml of oxalic acid was added to quench the polymerization reaction.

[0067] The reaction solution was slowly poured into water and stirred for 2 hours, filtered, boiled in water for 2 hours, filtered, and the filter cake was baked in a vacuum oven at 200°C for 48 hours.

[0068] The intrinsic viscosity of the obtained polymer in m-cresol at 30°C was 0.68 dL / g, and the glass transition temperature (Tg) was 220°C. The heat distortion temperature is 190°C, and the 5% therma...

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Abstract

The invention discloses polythioether ketone imide terpolymer and a preparation method thereof. The polythioether ketone imide terpolymer is characterized by being prepared by the following steps of: adding sulfur, disubstituted phthalimide, disubstituted ketone, a reducing agent and a reaction assistant into a reactor into which a solvent is filled; heating to react for a certain period of time;pouring reaction solution into a precipitator; and stirring, purifying and drying. Compared with the prior art, the invention has the advantages that: the disubstituted phthalimide and the disubstituted ketone are used as raw materials and the sulfur is used as a coupling agent for preparation; and an obtained product is hypocrystalline and has high dissolubility, mechanical performance and heat resistance, low melting viscosity, wider processing window and high processing performance.

Description

technical field [0001] The invention relates to a thioether ketimide polymer, which belongs to the technical field of polymer industry, and also relates to a preparation method of the polythioether ketimide polymer. Background technique [0002] Polythioetherimide is introduced into the rigid polyimide main chain due to the introduction of flexible units of thioether bonds. In addition to good thermomechanical properties, this type of polymer also has good solubility, low melt viscosity and With the characteristics of melt processing, it is a very promising thermoplastic heat-resistant polymer material. Synthesis of polythioetherimide by traditional methods has attracted the attention of some research groups, and there are related literature reports, such as: US patents US3989712, US4054584, US4092297, US4499285 and US4625037. [0003] China's literature in this regard such as: CN1038676C, CN1724528A, mainly reported that chlorine (or nitro) substituted phthalic anhydride w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/024C08G75/0263
Inventor 方省众胡本林严庆丁孟贤
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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