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Preparation method of branched polystyrene-maleic anhydride and application thereof

A technology of maleic anhydride and polystyrene, applied in chemical instruments and methods, chemical/physical processes, transportation and packaging, etc., can solve the problems of poor dispersion stability, large dispersion index, and high reaction temperature of the dispersion, and achieve The effect of controllable polymer structure and properties, good product application performance and excellent product performance

Inactive Publication Date: 2013-07-17
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method is loaded down with trivial details, and technique is comparatively complicated, and reaction temperature is higher
[0005] Tian Anli et al. ("Macromolecular Materials Science and Engineering", 2005, 21 (6): 102-109) synthesized a random copolymer of styrene maleic anhydride by solution radical polymerization, and used it for ultrafine Pigment water-based dispersion system, the prepared pigment dispersion has good dispersion performance, but the polydispersity index of polymer molecular weight is relatively large, the preparation conditions have a great influence on the performance of the polymer, and the dispersion stability of the dispersion is not good
Zhang Lianbing and others ("Printing and Dyeing", 2010, 11:1-4,13) adopted reversible addition. Styrene-maleic anhydride copolymer PRSMA was synthesized by fractured chain transfer (RAFT) polymerization. PRSMA hydrolyzate was used as a dispersant, and the pigment was dispersed by ultrasonic pulverization. The obtained dispersion had a small and uniform particle size and stable dispersion. High stability, but the raw materials are difficult to obtain, and may impart color and odor to the polymer, hindering its application

Method used

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  • Preparation method of branched polystyrene-maleic anhydride and application thereof
  • Preparation method of branched polystyrene-maleic anhydride and application thereof
  • Preparation method of branched polystyrene-maleic anhydride and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 1.04g (10mmol) styrene, 1.176g (12mmol) maleic anhydride, 0.1g (0.67mmol) p-vinylbenzylmercaptan to a 100ml four-neck round bottom flask equipped with a thermometer, reflux condenser and stirrer , 0.232g AIBN, and then add 44g of toluene as a polymerization solvent, place the flask in a constant temperature oil bath, heat and stir to 30°C and pass N 2 After 15 minutes, close the system, raise the temperature to 65°C, and stir for 10 hours at a constant temperature. After the reaction, the product is suction-filtered and rinsed with hot toluene (about 40°C) for several times, then dissolved in acetone, and a small amount of insoluble impurities are filtered off. Dissolving, precipitating, and purifying three times were repeated and dried in a vacuum oven to obtain 2.138 g of branched polystyrene maleic anhydride product with a monomer conversion rate of 92.3%.

Embodiment 2

[0029] Add 1.04g (10mmol) styrene, 1.176g (12mmol) maleic anhydride, 0.2g (1.34mmo) p-vinylbenzylmercaptan to a 100ml four-neck round bottom flask equipped with a thermometer, a reflux condenser and a stirrer , 0.29g AIBN, and then add 46g of toluene as the polymerization solvent, place the flask in a constant temperature oil bath, heat and stir to 35°C and pass N 2 After 20 minutes, close the system, raise the temperature to 70°C, and stir at constant temperature for 15 hours. After the reaction, the product is suction filtered and washed with hot toluene (about 40°C) for several times, then dissolved in acetone, and a small amount of insoluble impurities are filtered off. Precipitate and separate with toluene. After repeated dissolution, precipitation, and purification three times, vacuum oven drying obtained 2.160 g of branched polystyrene maleic anhydride product, and the monomer conversion rate was 89.4%.

Embodiment 3

[0031] Add 1.04g (10mmol) styrene, 1.176g (12mmol) maleic anhydride, 0.3g (2mmol) p-vinylbenzylmercaptan, 0.327g AIBN, and then add 35g of toluene as polymerization solvent, place the flask in a constant temperature oil bath, heat and stir to 40°C and turn on N 2 After 25 minutes, close the system, raise the temperature to 75°C, and stir for 20 hours at a constant temperature. After the reaction, the product is suction filtered and washed with hot toluene (about 40°C) for several times, then dissolved in acetone, and a small amount of insoluble impurities are filtered off. Precipitate and separate with toluene. After repeated dissolution, precipitation, and purification three times, vacuum oven drying obtained 2.204 g of branched polystyrene maleic anhydride product, and the monomer conversion rate was 87.6%.

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Abstract

The invention relates to a preparation method of branched polystyrene-maleic anhydride, comprising the steps of: (1) under normal pressure, dissolving p-vinylbenzyl mercaptan, styrene, maleic anhydride, and an initiator for free radical polymerization in a polymerization solvent; (2) under stirring, heating the solution obtained in step (1) to a temperature of 30-40DEG C and introducing nitrogen to the solution, sealing the reaction container, keeping stirring, raising the temperature of the solution to 65-80DEG C and preserving the heat for a reaction of 10-24h; (3) after the reaction, conducting pumping filtration to the solution obtained in step (2), leaching the solid from filtration with a hot precipitating agent, then dissolving the solid in an organic solvent, filtering out insoluble impurities therein, conducting precipitation and pumping filtration to the obtained solution in a precipitating agent, subjecting the solid obtained from filtration to dissolution, precipitation and pumping filtration, and carrying out vacuum drying to the generated solid. According to the invention, the polymerization conditions are mild, the polymers have controllable structural performance, and the polymerization product has excellent performance, simple and convenient preparation operations, as well as good application.

Description

technical field [0001] The invention relates to the field of functional polymer materials, in particular to the field of styrene-maleic anhydride (SMA) copolymers. Background technique [0002] Compared with traditional linear polymers, branched polymers have low viscosity, high density and a large number of terminal functional groups due to their highly branched structure, no entanglement between molecules, and a large number of reactive end groups. performance. [0003] Styrene (St)-maleic anhydride (MA) copolymer has excellent heat resistance, rigidity, dimensional stability and excellent emulsification, film forming, thickening and other characteristics, and is widely used in latex coatings, water treatment agents, Adhesive modifiers, textile auxiliaries, printing inks and other fields have always been research hotspots for scholars. However, there are few reports on branched styrene maleic anhydride, and it is very challenging to develop the preparation technology of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/08C08F212/08C08F2/38B01F17/52C09B67/20C09K23/52
Inventor 刘晓亚熊小梅刘敬成付少海江金强贾秀丽王宝清
Owner JIANGNAN UNIV
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