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Preparation method of biodegradable polyester

A biodegradable polyester and oxide technology, applied in the field of biodegradable polyester preparation, can solve the problems of difficult esterification and inactivation of titanium-based catalysts, and achieve the effect of inhibiting side reactions and inhibiting formation

Active Publication Date: 2013-03-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, in the diesterization polymerization process, in the presence of aromatic dibasic acids, the side reaction of 1,4-butanediol (BDO) to THF is very severe, and THF can easily lead to the deactivation of titanium-based catalysts. , so that the esterification reaction is difficult to carry out effectively

Method used

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  • Preparation method of biodegradable polyester
  • Preparation method of biodegradable polyester

Examples

Experimental program
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Effect test

preparation example Construction

[0015] The preparation method of described biodegradable polyester provided by the present invention comprises the following steps:

[0016] (1) Under the conditions of the first esterification reaction, component a and component b are reacted in the first reactor in the presence of the first catalyst and the second catalyst to obtain the first reaction mixture, said component The molar ratio of component a to the added amount of component b is 1:0.8-3;

[0017] (2) Under the second esterification reaction conditions, component b and component c are reacted in the second reactor in the presence of the first catalyst and the second catalyst to obtain a second reaction mixture, the group The molar ratio of component c to the added amount of component b is 1:0.8-3;

[0018] (3) Under polycondensation reaction conditions, the first reaction mixture and the second reaction mixture are reacted in the presence of a third catalyst;

[0019] The component a is an aromatic dibasic aci...

Embodiment 1

[0046] This example is used to illustrate the preparation method of the biodegradable polyester provided by the present invention.

[0047] Add 0.60 mol of terephthalic acid, 1.11 mol of 1,4-butanediol, 0.25 mmol of tetrabutyl titanate (purchased from Beijing Chemical Reagent Co.), 0.14 mmol of Butyltin oxide (purchased from Beijing No. 3 Chemical Plant) and 0.14 mmol of triphenylhydroxytin (purchased from Beijing Chemical Reagent Company) were stirred and heated to reflux under a nitrogen atmosphere, and the temperature was adjusted to 230 ° C. The reaction was stopped when the water was completely evaporated to obtain the first reaction mixture.

[0048] To another three-necked flask with a volume of 500ml, add 0.60mol of 1,4-butanedioic acid, 0.90mol of 1,4-butanediol, 0.25mmol of tetrabutyl titanate (purchased from Beijing Chemical Reagent Company), 0.14mmol of dibutyltin oxide (purchased from Beijing No. 3 Chemical Factory) and 0.14mmol of triphenylhydroxytin (purchased ...

preparation example 1

[0051] Add 0.60 mol of terephthalic acid, 1.11 mol of 1,4-butanediol, 0.25 mmol of tetrabutyl titanate (purchased from Beijing Chemical Reagent Company), 0.14 mmol of dibutyl Tin oxide (purchased from Beijing No. 3 Chemical Plant) and 0.14 mmol of triphenylhydroxytin (purchased from Beijing Chemical Reagent Company), under a nitrogen atmosphere, stirred and heated to reflux, and the temperature was adjusted to 230 ° C. The water to be reacted was When it is completely evaporated, add 0.48mmol of lanthanum stearate to the reactor, adjust the absolute pressure in the reactor to below 200Pa, adjust the temperature to 240°C, and polycondense at this temperature and pressure for 7 hours to obtain light yellow polymer. The glass transition temperature of the polyester measured according to a differential scanning calorimeter (DSC) measurement method was 42.6°C.

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Abstract

A preparation method of a biodegradable polyester comprises steps of: (1) carrying out a reaction on an ingredient a and an ingredient b under existence of a first catalyst and a second catalyst; (2) carrying out a reaction on the ingredient b and an ingredient c under existence of the first catalyst and the second catalyst; (3) carrying out a reaction on the products obtained from the step (1) and (2) with existence of a third catalyst. The ingredient a is aromatic diacid and / or acid anhydrides of aromatic diacid; the ingredient b is acyclic dihydric alcohol; the ingredient c is at least one selected from aliphatic dibasic acid, acid anhydrides of aliphatic dibasic acid, alicyclic diacid and acid anhydrides of alicyclic diacid; the first catalyst is at least a compound selected from M oxide, M(OR1)n and M(-OOCR2)n or a mixture of the three; the second catalyst is at least an organo tin compound; the third catalyst is at least a compound with a chemical formula of RE(R3)3. Polyester prepared by the method has good biodegradation performance, high molecular weight and more concentrated molecular weight distribution.

Description

technical field [0001] The invention relates to a preparation method of biodegradable polyester. Background technique [0002] At present, thermoplastic aromatic polyesters, which are widely used in industry and daily life, have excellent thermal stability and mechanical properties, are easy to process and low in price. Polyethylene terephthalate (PET), and polybutylene terephthalate (PBT), for example, have been widely used in the manufacture of fibers, films and containers. However, these aromatic polyesters are difficult to degrade after being used and discarded, and no obvious direct degradation of aromatic polyesters such as PET and PBT by microorganisms has been observed so far. In order to combine the excellent properties of aromatic polyesters, since the 1980s, those skilled in the art have devoted themselves to the research of synthesizing aliphatic-aromatic copolyesters, that is, introducing aromatic segments into aliphatic polyesters, which not only ensures the c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/181C08G63/183C08G63/84
Inventor 祝桂香张伟韩翎许宁
Owner CHINA PETROLEUM & CHEM CORP