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Suspending solid phase polymerization method for preparing polymer

A solid-phase polymerization and polymer technology, which is applied in the field of suspension solid-phase polymerization for producing polymers, can solve the problems of difficult continuous production, easy agglomeration, affecting polymer properties, etc., and achieves good polymerization effect and prevents agglomeration. Effect

Inactive Publication Date: 2009-02-18
TORAY FIBER RES INST(CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is: (1) there is autoacceleration; (2) dispersant must be used, and after the polymerization is completed, it is difficult to remove from the polymer product, which will affect the performance of the polymer product (such as appearance, aging performance, etc.); ( 3) The particles of the polymerized product will contain a small amount of monomer, which is not easy to completely remove and affect the performance of the polymer; (4) It is difficult to produce by continuous method.
The disadvantage of solid phase polymerization is that solid phase particles, especially those with smaller particle sizes, tend to agglomerate during crystallization or polymerization, resulting in difficulty in stirring and flowing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Starting material: Nylon 6 prepolymer powder (containing sodium hypophosphite 0.03wt%), powder particle size D≈200um, molecular weight (determined by end group analysis, the same below) Mn=7k, melting enthalpy ΔHm=58J / g, melting point Tm=204°C, glass transition temperature Tg=45°C

[0040] Liquid inert medium: phenyl silicone oil

[0041] Inject 250ml of phenyl silicone oil into a 500ml three-neck flask with a magnet. One port of the three-neck flask was connected to nitrogen gas, the other port was connected to a vacuum system, and the other port was inserted into a thermocouple thermometer. After the three-neck flask was placed in an oil bath, stirring was started, the vacuum was turned on, and nitrogen was replaced three times. Under a nitrogen atmosphere, slowly add 25 g of nylon 6 prepolymer powder into a three-necked flask. After opening the vacuum to lower the pressure to 200 Pa, the temperature was raised to 180° C. and kept at a polymerization temperature T...

Embodiment 2

[0043] Starting material: Nylon 6 prepolymer powder (containing sodium hypophosphite 0.03wt%), powder particle size D≈500um, molecular weight (determined by end group analysis, the same below) Mn=7k, melting enthalpy ΔHm=58J / g, melting point Tm=204°C, glass transition temperature Tg=45°C

[0044] Liquid inert medium: phenyl silicone oil

[0045] Inject 250ml of phenyl silicone oil into a 500ml three-neck flask with a magnet. One port of the three-neck flask was connected to nitrogen gas, the other port was connected to a vacuum system, and the other port was inserted into a thermocouple thermometer. After the three-neck flask was placed in an oil bath, stirring was started, the vacuum was turned on, and nitrogen was replaced three times. Under a nitrogen atmosphere, slowly add 25 g of nylon 6 prepolymer powder into a three-necked flask. After opening the vacuum to lower the pressure to 200 Pa, the temperature was raised to 180° C. and kept at a polymerization temperature T...

Embodiment 3

[0047] Starting material: Nylon 6 prepolymer powder (containing sodium hypophosphite 0.03wt%), powder particle size D≈200um, molecular weight (determined by end group analysis, the same below) Mn=8k, melting enthalpy ΔHm=60J / g, melting point Tm=206°C, glass transition temperature Tg=45°C

[0048] Liquid inert medium: phenyl silicone oil

[0049] Inject 250ml of phenyl silicone oil into a 500ml three-neck flask with a magnet. One port of the three-neck flask was connected to nitrogen gas, the other port was connected to a vacuum system, and the other port was inserted into a thermocouple thermometer. After the three-neck flask was placed in an oil bath, stirring was started, the vacuum was turned on, and nitrogen was replaced three times. Under a nitrogen atmosphere, slowly add 25 g of nylon 6 prepolymer powder into a three-necked flask. After opening the vacuum to reduce the pressure to 200 Pa, the temperature was raised to 190° C. and kept at a polymerization temperature ...

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Abstract

The invention discloses a suspension solid-phase polymerization method for producing polymers, comprising the steps of suspending monomer or prepolymer powder or particle in liquid inert medium or gaseous inert medium to solid-phase polymerize. The polymerization temperature is between the glass transition temperature of monomer or prepolymer and the melting point. The invention solves the problems that the common solid-phase polymerization is easy to cause polymerization heat, the crystalization heat is hard to spread and particle or powder is easy to agglomerate. The suspension solid-phase polymerization method of the invention is suitable for (but not limited to) condensation polymerization and is also suitable for (but not limited to) preparing and manufacturing aromatic polyester, aliphatic polyester, polycarbonate, polyamide, polyimide, polysulfone, polyether and the like.

Description

technical field [0001] The present invention relates to a method for polymerizing polymers. Background technique [0002] suspension polymerization [0003] Suspension polymerization is a polymerization reaction in which the monomer is dispersed into countless small liquid droplets suspended in water by strong stirring and under the action of a dispersant, and is initiated by an oil-soluble initiator. [0004] A suspension polymerization system generally includes four basic components: monomer, initiator, water, and suspending agent. Wherein the monomer is insoluble or slightly soluble in water, and the initiator is soluble in the monomer. Suspending agent is a kind of substance that can disperse oil-soluble monomers in water to form a stable suspension, generally water-soluble polymer substances (such as polyvinyl alcohol, sodium polyacrylate, S-MAA copolymer, gelatin, cellulose, Starch, etc.), or water-insoluble inorganic substances (such as carbonates, sulfates, talc, ...

Claims

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Application Information

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IPC IPC(8): C08G63/78C08G64/20C08G69/00C08G73/10C08G75/20
Inventor 何勇朱可新郭晓王枫夏天成曹晓秀
Owner TORAY FIBER RES INST(CHINA) CO LTD
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