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,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0038] Example 1:

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

[0040] Liquid inert medium: phenyl silicone oil

[0041] Put 250ml of phenyl silicone oil into a 500ml three-necked flask with a magnet. The three-necked flask is connected to nitrogen at one end, vacuum system at the other, and thermocouple thermometer at the other. Put the three-necked flask in the oil bath and start stirring, turn on the vacuum, and replace the nitrogen three times. Under a nitrogen atmosphere, 25 g of nylon 6 prepolymer powder was slowly added to the three-necked flask. After opening the vacuum to lower the pressure to 200 Pa, the temperature was raised to 180°C and the polymerization temperature Ts was 180°C and the polymerization temperature pressure P wa...

Example Embodiment

[0042] Example 2:

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

[0044] Liquid inert medium: phenyl silicone oil

[0045] Put 250ml of phenyl silicone oil into a 500ml three-necked flask with a magnet. The three-necked flask is connected to nitrogen at one end, vacuum system at the other, and thermocouple thermometer at the other. Put the three-necked flask in the oil bath and start stirring, turn on the vacuum, and replace the nitrogen three times. Under a nitrogen atmosphere, 25 g of nylon 6 prepolymer powder was slowly added to the three-necked flask. After opening the vacuum to lower the pressure to 200 Pa, the temperature was raised to 180°C and the polymerization temperature Ts was 180°C and the polymerization temperature press...

Example Embodiment

[0046] Example 3:

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

[0048] Liquid inert medium: phenyl silicone oil

[0049] Put 250ml of phenyl silicone oil into a 500ml three-necked flask with a magnet. The three-necked flask is connected to nitrogen at one end, vacuum system at the other, and thermocouple thermometer at the other. Put the three-necked flask in the oil bath and start stirring, turn on the vacuum, and replace the nitrogen three times. Under a nitrogen atmosphere, 25 g of nylon 6 prepolymer powder was slowly added to the three-necked flask. After opening the vacuum to reduce the pressure to 200 Pa, the temperature was raised to 190°C and the polymerization temperature Ts was 190°C and the polymerization temperature pressure P w...

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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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