PASSI terpolymer and preparation method thereof

A sulfonimide terpolymer and terpolymer technology, applied in the field of preparation of the polysulfide sulfoneimide polymer, can solve the problems of narrow processing window, little industrial significance, high cost, etc.

Active Publication Date: 2010-05-12
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 and molecular weight of the obtained copolymer are low, and the industrialization is of little significance

Method used

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  • PASSI terpolymer and preparation method thereof
  • PASSI terpolymer and preparation method thereof
  • PASSI terpolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Add 5.29g (0.01mol) 4,4'-bis(4-chloroimide) diphenyl ether, 2.87g (0.01mol) 4'4-dichlorodiphenyl sulfone in a 250ml three-necked flask , 0.67g (0.021mol) sulfur, 5.67g (0.063) paraformaldehyde, 1.68g sodium hydroxide, 0.25g calcium chloride, add 100mlN-methylpyrrolidone (solid content: 8%) after logical nitrogen deoxygenation three times, After heating to 150° C. for 5 hours, cooling to room temperature, adding 0.11 g of chlorobenzene, heating to 180° C. for 3 hours, and cooling the reaction solution to room temperature for aftertreatment.

[0050] 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 in a Soxhlet extractor with a mixed solution of ethanol and acetone for 24 hours, and then The obtained polymer was baked in a vacuum oven at 200° C. for 48 hours.

[0051] The intrinsic viscosity of the obtained polymer in m-cresol at 30°C is 0.65dL / g...

Embodiment 2

[0052] Example 2: Add 54.85g (0.100mol) 3,4'-bis(4-nitroimide) diphenylmethane and 48.04g (0.100mol) 3,3'-bis(3- Fluoroimide) biphenyl mixture, 30.83g (0.100mol) 4,4'-dinitrodiphenyl sulfone, 9.14g (0.285mol) sulfur, 21.56g (0.57mol) sodium borohydride, 41.46g carbonic acid Potassium, 5.23g sodium iodide, 4000ml dimethyl sulfoxide and 1000ml xylene (solid content: 14%) were added after argon deoxygenation three times, heated to 180°C and reacted for 20 hours, cooled to room temperature and added 3 -The nitrobenzophenone was heated to 200° C. for 1 hour to react, and the reaction solution was cooled to room temperature for aftertreatment.

[0053] 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 200° C. for 48 hou...

Embodiment 3

[0055] Example 3: Add 22.22g (0.04mol) 2,2'-(4,4'-bis(3-chloroimide) diphenyl)isopropane and 16.33g (0.03mol) in a 500ml there-necked flask 3,3'-bis(3-fluoroimide) diphenylsulfone mixture, 2.56g (0.01mol) 3,3'-difluorodiphenylsulfone and 5.19g (0.01mol) bis(4-(4 -Mixture of chlorophenylsulfone group) phenyl) ether, 2.88g (0.09mol) sulfur, 5.04g (0.09) reduced iron powder, 9.07g sodium bicarbonate, 0.3g18-crown-6, pass argon to deoxygenate three times Then add 300ml of N,N-dimethylformamide, heat to 180°C and react for 20 hours, then add 20ml of oxalic acid to quench the polymerization reaction.

[0056] 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.

[0057] The intrinsic viscosity of the obtained polymer in m-cresol at 30°C was 0.41 dL / g, and the glass transition temperature (Tg) was 249°C. The heat distortion temperature is 216...

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Abstract

The invention discloses a PASSI terpolymer and a preparation method thereof. The invention is characterized in that sulphur, disubstituted phthalimide, disubstituted sulphone, reducing agent and reaction aid in a reactor filled with solvent, heating for reaction for certain time, pouring reaction liquid into precipitating agent, stirring and filtering, desalting and filter cake and residual solvent to obtain the PASSI terpolymer. Compared with the prior art, the invention has the advantages that the obtained product has good thermal stability (e.g. fluidity, mechanical property and heat resistance), lower fusion viscosity, wider processing window and excellent processing performance; meanwhile, the introduction of sulphur and sulphone containing structure can further reduce preparation cost of polyimide polymer.

Description

technical field [0001] The invention relates to a polysulfide sulfone imide polymer, which belongs to the technical field of polymer industry, and also relates to a preparation method of the polysulfide sulfone imide 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 respect such as: CN1038676C, CN1724528A, mainly reported that chlorine (or nitro) substituted phthalic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/30
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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