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A kind of synthetic method of self-plasticized modified polycaprolactone

A technology of polycaprolactone and a synthesis method, which is applied in the synthesis field of modified polycaprolactone, can solve the problems of low strength, limited application and the like, and achieve the effect of improving plasticization rigidity

Inactive Publication Date: 2019-02-15
TIANJIN WEIRUI SUPERMOLECULE MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But its strength is not high, which limits its application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Mix 27g of polycaprolactone (mole number: 0.05; OH mole number: 0.15) with trihydroxy functional group molecular weight 540 and 29.1g toluene-2,4-diisocyanate (mole number: 0.15; NCO mole number: 0.300) , After stirring the reaction at 80-100°C, lower it to 60°C, add 6.5g of isooctyl alcohol (0.05 moles), stir and react at 60°C for 240 minutes, raise the temperature to 100°C, until there is basically no isooctyl alcohol vapor, and the fluidity is very good , basically no bubbles, the solution is clear and transparent, pump air until the solution has no bubbles, stop heating, let stand, and you are ready. Observed overnight, it was found that the solution was uniform and stable, flowing slowly at room temperature, and had good fluidity when heated to 80°C.

Embodiment 2

[0017] Mix 73.03g of polycaprolactone (mole number: 0.1352; OH mole number: 0.4057) with trihydroxy functional group molecular weight of 540 and 68.16g hexamethylene diisocyanate (mole number: 0.4057; NCO mole number: 0.8114), After stirring and reacting at 80-100°C for 3 hours, lower it to 25°C, add 17.58g of isooctyl alcohol (mole number: 0.1352), and stir at room temperature for 0.5h. The solution is colorless and transparent, relatively viscous, and turns white after stirring. .

[0018] At this time, raise the temperature to 110°C and stir for 1.5h to react, continue to add 39.69g of hexamethylene diisocyanate (moles: 0.2363, NCO moles: 0.4725), and stir at 100°C for 30mins until the solution is clear, free of alcohol vapor, and free of bubbles After that, let it stand still, and you will get it. Observed at 100°C, the fluidity of the solution is good, the bubbles disappear, and the solution changes from white to clear

Embodiment 3

[0020] Mix 13.5g of polycaprolactone (mol number: 0.025; OH mole number: 0.075) with trihydroxy functional group molecular weight of 540 and 12.6g hexamethylene diisocyanate (mol number: 0.075; NCO mole number: 0.15), After stirring and reacting at 100°C for 3 hours, lower it to 25°C, add 3.25g of isooctyl alcohol (mole number: 0.025), and stir at room temperature for 0.5h. The solution is colorless and transparent, relatively viscous, and turns white with many bubbles after stirring.

[0021] At this point, raise the temperature to 100°C and stir for 1.5h to react, then continue to add 5.18g of hexamethylene diisocyanate (moles: 0.03083, NCO moles: 0.06167), and stir at 100°C for 20min until the solution is clear, free of alcohol vapor and bubbles After that, let it stand still, and you will get it. Observed at 100°C, the fluidity of the solution was good, the bubbles disappeared, and the solution changed from white to clear.

[0022] Effect experiment example

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PUM

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Abstract

The invention provides a synthesis method of self-plasticized modified polycaprolactone. The method includes the following steps of mixing polycaprolactone with diisocyanate, stirring the mixture for reaction at a temperature of 80-100 DEG C, adding small-molecule alcohol with plasticization after lowering the temperature to 20-60 DEG C, conducting stirring for reaction at a temperature of 60-110 DEG C till the solution is clear and free of alcohol stem and bubbles, and standing. The ratio of the OH mole number of polycaprolactone to the NCO mole number of diisocyanate and the OH mole number of small-molecule alcohol is 3:(6-9):1. Polycaprolactone is used as a matrix, small-molecule alcohol with plasticization is used as plasticizer, diisocyanate is used as a cross-linking agent, grafting is conducted between the plasticizer and polycaprolactone, and therefore the plasticization rigidity of polycaprolactone is effectively improved; the material having the flexible performance and plasticization rigidity is formed.

Description

technical field [0001] The invention relates to a method for synthesizing self-plasticized modified polycaprolactone with both flexibility and plasticizing rigidity. Background technique [0002] Polycaprolactone Polycaprolactone (referred to as PCL) is formed by ring-opening polymerization of ε-caprolactone under the condition of a metal organic compound (such as tetraphenyltin) as a catalyst and dihydroxyl or trihydroxyl as an initiator. It belongs to the polymerization type For polyester, its molecular weight and degree of disproportionation vary with the type and amount of starting materials. PCL is an aliphatic linear polyester with a Tg of -60°C, very soft and extremely stretchable. But its strength is not high, which limits its application. Contents of the invention [0003] The problem to be solved by the present invention is to provide a self-plasticizing modification that uses diisocyanate as a crosslinking agent to graft flexible materials with small molecule ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/76C08G18/73C08G18/66C08G18/42
CPCC08G18/2805C08G18/4277C08G18/66C08G18/73C08G18/7614
Inventor 刘学成
Owner TIANJIN WEIRUI SUPERMOLECULE MATERIAL SCI & TECH