Segmented polyester copolymer and preparation method thereof

A polyester block and copolymer technology, applied in the field of polymers, can solve the problems of low polyester molecular weight, poor chain extension efficiency, and imperfect preparation methods of polyester block copolymers, etc.

Active Publication Date: 2014-11-19
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many and mature synthesis methods of olefin block copolymers, but polyester block copolymers and their preparation methods are not perfect, and the method most reported in the literature is the transesterification method (Chinese patent 200810118233.6, Chinese patent 201110416884.5) , that is, two kinds of high molecular weight polyesters are used to undergo transesterification reaction under catalyst and high temperature, such as a biodegradable aliphatic polyester / aromatic polyester multi-block copolymer disclosed in Chinese patent 200910092100.0 and its preparation method and Application, it first synthesizes aliphatic polyester prepolymer A, then synthesizes aliphatic or aromatic polyester B, and synthesizes a multi-block copolymer under the action of a chain extender, which has the advantage of being compared with crystalline aliphatic polyester The introduction of rigid amorphous polyester chain segments can obtain good mechanical properties, but its disadvantage is that the chain extension efficiency is poor, and the prepared polyester has a low molecular weight

Method used

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  • Segmented polyester copolymer and preparation method thereof
  • Segmented polyester copolymer and preparation method thereof
  • Segmented polyester copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take a dry and clean 25ml thick-walled pressure-resistant reaction tube under argon atmosphere, add 5mmol exo-norbornene dianhydride, 0.1mmol bis-(triphenylphosphoryl)ammonium chloride, 5mmol epoxycyclohexane, 1ml Dissolve in toluene (the amount of solvent can dissolve quaternary ammonium salt compounds, epoxy compounds, acid anhydrides, etc.), react at 110°C for 1 hour; then add 5 mmol of internal norbornene diacid anhydride, 5 mmol of epoxy ring A mixed solution of hexane and 1ml of toluene (the amount of toluene can dissolve quaternary ammonium compounds, epoxy compounds, acid anhydrides, etc.), after reacting at 110°C for 4 hours, pour the reaction system into methanol with a volume of 50ml to settle , filtered, washed, and the resulting product was vacuum-dried at 45°C for 24h to obtain R 1 , R 3 For 2,3 substituted norbornene; R 2 , R 4 It is a polyester block copolymer with 1,2 substituted cyclohexane.

[0034] Among them, the m value is 15, and the n value i...

Embodiment 2

[0037] All the other operations are the same as in Example 1, and the difference is that in the step a) the acid anhydride is 5mmol external norbornene dioic anhydride, and the epoxy compound is 5mmol epoxycyclohexane; in the step b), the acid anhydride is 5mmol succinic anhydride, the epoxy compound It is 5mmol epoxycyclohexane. get R 1 It is the exo-norbornene substituted at the 2 and 3 positions, R 3 is hydrogen; R 2 , R 4 It is a polyester block copolymer of 1,2-substituted cyclohexane. The yield is 84%, the average molecular weight measured by GPC is 7050, the m value is 13, the n value is 18, and the molecular weight distribution is 1.6.

Embodiment 3

[0039] All the other operations are the same as in Example 1, and the difference is that in the step a) the acid anhydride is 5mmol external norbornene dioic anhydride, and the epoxy compound is 5mmol epoxycyclohexane; in the step b), the acid anhydride is 5mmol 3-oxabicyclo [3.1.0] The hexane-2,4-dione and the epoxy compound are 5 mmol of cyclohexane oxide. get R 1 It is the exo-norbornene substituted at the 2 and 3 positions, R 3 For 1,2-substituted cyclopropane; R 2 , R 4 It is a polyester block copolymer of 1,2-substituted cyclohexane. The yield is 85%, the average molecular weight measured by GPC is 5775, the m value is 11, the n value is 14, and the molecular weight distribution is 1.5.

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Abstract

The invention discloses a segmented polyester copolymer and a preparation method thereof. A structural formula of the copolymer is shown as a formula (I). An organic catalyst is directly adopted, so that the steps are simple and convenient in a polymer purification process, and heavy metal ions in a conventional method cannot be remained in a polymer. The esterification reaction of acid anhydride and an epoxy compound can be selectively catalyzed to obtain the polyester copolymer with geometrical isomerism chain segments, and generation of byproducts caused by catalysis of the open-loop auto-polymerization reaction of an epoxy group is avoided by the nuclear magnetic analysis of products.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to the stereoselective ring-opening of meso-acid anhydrides and epoxy compounds under organic catalysis to generate desymmetry and stereospecific (trans-, cis-) enantiomeric products. Polyester copolymers with geometrically isomeric segments were prepared by the method of sequential addition. Background technique [0002] Aliphatic polyesters are favored because they are biodegradable. However, it is difficult to obtain high molecular weight aliphatic polyester by conventional methods, and its thermal stability and mechanical properties are poor, which limits the application of aliphatic polyester. Therefore, in order to expand the application range of aliphatic polyesters, it is necessary to increase the molecular weight of aliphatic polyesters and modify aliphatic polyesters. [0003] A common way to improve the properties of polyester is to copolymerize it with other monomers ...

Claims

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Application Information

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IPC IPC(8): C08G63/58C08G63/682C08G63/87
Inventor 刘宾元韩冰张莉段中余
Owner HEBEI UNIV OF TECH
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