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Microsuspension Polymerization of Styrene-n-Phenylmaleimide-Acrylonitrile

A technology of maleimide and micro-suspension polymerization, applied in the field of water-phase micro-suspension polymerization, can solve the problems of complex process, difficult application and processing, affecting polymer properties, etc., and achieves high Vicat softening point and high glass transition temperature. , the effect of good application performance

Active Publication Date: 2017-01-04
Z RIVER GRP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Put in suspending agent, chain transfer agent, styrene, acrylonitrile, N-phenylmaleimide, and initiator at one time, heat up to polymerize, and then mature to obtain a terpolymer. The process is simple and easy to industrialize, and it is white granular Solid (average particle size 150-500μm), causing certain difficulties in application and processing, the glass transition temperature and Vicat softening point of the copolymer need to be improved
[0004] 2), the document "N-phenylmaleimide / styrene / acrylonitrile emulsion copolymer and PVC blending" proposes a method for emulsion copolymerization, which requires emulsification, polymerization, demulsification and other processes, and the process is complicated. Difficult to industrialize:
[0005] The monomer dissolved with the initiator is suspended in water under the action of dispersant and mechanical stirring to carry out free radical polymerization. The method is suspension polymerization, and there will be dispersant residue in the product, which will affect the performance of its polymer; water is used as Solvent, under the action of an emulsifier and with the help of mechanical stirring, the monomer is dispersed into an emulsion in water, and the polymerization initiated by the initiator is called emulsion polymerization, but the process is complicated and difficult to industrialize; microsuspension polymerization adopts special The composite emulsification system requires an emulsifier-refractory auxiliary agent microemulsion. The composite emulsification system has a strong ability to protect the polymer monomer particles, and the polymerization is initiated by an oil-soluble initiator. The particle size is between emulsion polymerization and suspension polymerization. Microsuspension polymerization not only has the advantages of simple suspension polymerization process and easy industrialization, but also has the advantages of fine particle size and uniform polymer chain segment of emulsion polymerization, which can significantly improve the performance of polymers. One of the main means of aggregation arising from physical properties

Method used

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  • Microsuspension Polymerization of Styrene-n-Phenylmaleimide-Acrylonitrile
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  • Microsuspension Polymerization of Styrene-n-Phenylmaleimide-Acrylonitrile

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1, a kind of aqueous phase microsuspension polymerization method that contains 18%PMI terpolymer, carries out following steps successively:

[0032] 1) Aggregation

[0033] Add 228g of styrene, 100g of acrylonitrile, 72g of N-phenylmaleimide, 800g of water, 10g of sodium dodecylbenzenesulfonate, 1g of dodecyl alcohol, and iso-neodecanoate peroxide into a 2000ml three-necked flask. Propylphenyl 0.5g, 2-naphthol 0.4g, sodium bicarbonate 1g, stir at 30°C for 30 minutes, heat up to 60-65°C for 6h;

[0034] 2) Centrifuge and dry

[0035] After the polymerization reaction time is up, add 0.05g bisphenol A to end the polymerization reaction, filter, and the resulting filter cake is air-dried at 100° C. for 1 hour to obtain a white powdery solid (polystyrene-N-phenylmaleimide- Acrylonitrile terpolymer) 390g, yield 97.5%.

[0036] 3) Test results

[0037] Glass transition temperature: 135.7~138.7℃; Vicat softening point: 120.3~124.2℃; average particle size: 75μm. ...

Embodiment 2

[0038] Embodiment 2, a kind of aqueous phase microsuspension polymerization method containing 25%PMI terpolymer, carry out following steps successively:

[0039] 1) Aggregation

[0040] In a 2000ml three-necked flask, add 208g of styrene, 92g of acrylonitrile, 100g of N-phenylmaleimide, 800g of water, 10g of sodium dodecylbenzenesulfonate, 1g of dodecyl alcohol, and iso-neodecanoate peroxide. Propylphenyl 0.5g, 2-naphthol 0.4g, sodium bicarbonate 1g, stir at 30°C for 30 minutes, heat up to 60-65°C for 6h;

[0041] 2) Centrifuge and dry

[0042] After the polymerization reaction time is up, add 0.05g bisphenol A to end the polymerization reaction, filter, and the resulting filter cake is air-dried at 100° C. for 1 hour to obtain a white powdery solid (polystyrene-N-phenylmaleimide- Acrylonitrile terpolymer) 394g, yield 98.5%.

[0043] 3) Test results

[0044] Glass transition temperature: 145.3~150.4℃; Vicat softening point: 130.3~138.0℃; average particle size: 81μm.

Embodiment 3

[0045] Embodiment 3, a kind of aqueous phase microsuspension polymerization method containing 34% PMI terpolymer, carries out following steps successively:

[0046] 1) Aggregation:

[0047] Add 168g of styrene, 96g of acrylonitrile, 136g of N-phenylmaleimide, 800g of water, 10g of sodium dodecylbenzenesulfonate, 1g of dodecyl alcohol, and iso-neodecanoate peroxide into a 2000ml three-necked flask. Propylphenyl 0.5g, 2-naphthol 0.4g, sodium bicarbonate 1g, stir at 30°C for 30 minutes, heat up to 60-65°C for 6h;

[0048]2) Centrifuge and dry:

[0049] After the polymerization reaction time is up, add 0.05g bisphenol A to end the polymerization reaction, filter, and the resulting filter cake is air-dried at 100° C. for 1 hour to obtain a white powdery solid (polystyrene-N-phenylmaleimide- Acrylonitrile terpolymer) 396g, yield 99%.

[0050] 3) Test results

[0051] Glass transition temperature: 150.2~154.7℃; Vicat softening point: 155.1~160.8℃; average particle size: 85μm.

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Abstract

The invention discloses a water-phase microsuspension polymerization method of polystyrene-N-phenylmaleimide-acrylonitrile terpolymer, which comprises the following steps: 1) polymerization: putting styrene , acrylonitrile and N-phenylmaleimide, and put in deionized water, compound emulsifier, initiator, anti-sticking agent and pH regulator, stir, and heat up to 40-85°C for polymerization The polymerization reaction time is 2 to 7 hours; 2) centrifugation and drying: after the polymerization reaction time is up, add a terminator accounting for 0.1 to 1‰ of the total weight of the monomer to end the polymerization reaction, filter, and obtain the obtained filter cake after drying. Styrene‑N‑phenylmaleimide‑acrylonitrile terpolymer. The method of the invention has the advantage of high monomer conversion rate.

Description

technical field [0001] The present invention relates to a kind of polymerization method of styrene-N-phenylmaleimide-acrylonitrile terpolymer, namely the water of styrene-N-phenylmaleimide-acrylonitrile terpolymer phase microsuspension polymerization method. Background technique [0002] N-phenylmaleimide (referred to as PMI) is a rigid heat-resistant monomer, and its copolymer is widely used in the heat-resistant modification of ABS, PVC, SAN, PMMA and other resins. Among them, styrene-N- Phenylmaleimide-acrylonitrile terpolymer is an excellent ABS heat-resistant modifier. Existing preparation method is specifically as follows: [0003] 1), Patent CN200710069041.6 reports the formation of styrene-N-phenylmaleimide-acrylonitrile terpolymer by one-step suspension polymerization. Put in suspending agent, chain transfer agent, styrene, acrylonitrile, N-phenylmaleimide, and initiator at one time, heat up to polymerize, and then mature to obtain a terpolymer. The process is si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/08C08F220/44C08F222/40C08F2/18C08F2/42
Inventor 张超叶小明张华张琪
Owner Z RIVER GRP LTD