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Preparation method of polybutylene succinate

A technology of polybutylene succinate and butanediol, which is applied in the field of synthesis of biodegradable aliphatic polyester polymer materials, can solve the problems of complicated operation steps, increased production energy consumption, high reaction temperature, etc. Small amount, improved catalytic efficiency, and high catalytic activity

Active Publication Date: 2021-01-29
YINGKOU KANGHUI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN 101671435 B provides a complex catalyst with hydroxycarboxylic acid and phosphoric acid ester as complexing agent, the main components are titanium alkoxide, silicon alkoxide and glycol, and it is used for the synthesis of PBS, although the chroma Better PBS product, but its reaction temperature is higher when using this catalyst, which increases the production energy consumption
Patent CN 105061744 B provides a catalyst compounded by adding titanate after the reaction of butanediol, organophosphorus compound and hindered phenolic antioxidant. PBS with good color above 36MPa, but heat stabilizer needs to be added in the polycondensation stage, and the operation steps are cumbersome

Method used

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  • Preparation method of polybutylene succinate
  • Preparation method of polybutylene succinate
  • Preparation method of polybutylene succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] A high-efficiency composite catalyst is prepared by the following steps:

[0056] (1) Add amino acid ester (methyl serine), titanate (diethylene glycol titanate), silicate (methyl orthosilicate) and metal acetate (aluminum acetate) to 1,4-butyl The reaction is carried out in diol and monohydric alcohol (ethanol); the reaction temperature is 50°C, and the reaction time is 8h; the mass ratio of amino acid ester to titanate is 0.4:1; the mass ratio of silicate to titanate is 0.06:1 The mass ratio of metal acetate to titanate is 0.001:1; the mass ratio of 1,4-butanediol to titanate is 1.2:1; the mass ratio of monohydric alcohol to metal acetate is 35:1 ;

[0057] (2) adopt the mode of underpressure distillation to remove the small molecule that reaction generates, wherein the absolute pressure of underpressure distillation is 1kPa;

[0058] (3) adding a phosphoric acid compound (triethyl phosphate) to the system after removing small molecules to react again to obtain the ...

Embodiment 2

[0061] A high-efficiency composite catalyst is prepared by the following steps:

[0062] (1) Add amino acid ester (threonine methyl ester), titanate (diethylene glycol titanate), silicate (orthosilicate methyl ester) and metal acetate (cobalt acetate) to 1,4 -React in butanediol and monohydric alcohol (ethanol); the reaction temperature is 60°C, the reaction time is 9h; the mass ratio of amino acid ester to titanate is 0.3:1; the mass ratio of silicate to titanate is 0.08 :1; the mass ratio of metal acetate to titanate is 0.0013:1; the mass ratio of 1,4-butanediol to titanate is 1.2:1; the mass ratio of monohydric alcohol to metal acetate is 50 :1;

[0063] (2) adopt the mode of underpressure distillation to remove the small molecule that reaction generates, wherein the absolute pressure of underpressure distillation is 1kPa;

[0064] (3) adding phosphoric acid compounds (triethyl phosphonoacetate) to the system after removing small molecules to react again to obtain the hig...

Embodiment 3

[0067] A high-efficiency composite catalyst is prepared by the following steps:

[0068] (1) Add amino acid ester (methyl glycine), titanate (diethylene glycol titanate), silicate (methyl orthosilicate) and metal acetate (zinc acetate) to 1,4-butyl The reaction is carried out in diol and monohydric alcohol (n-propanol); the reaction temperature is 60°C, and the reaction time is 8h; the mass ratio of amino acid ester to titanate is 0.2:1; the mass ratio of silicate to titanate is 0.05 :1; the mass ratio of metal acetate to titanate is 0.0015:1; the mass ratio of 1,4-butanediol to titanate is 1.5:1; the mass ratio of monoalcohol to metal acetate is 50 :1;

[0069](2) adopt the mode of underpressure distillation to remove the small molecule that reaction generates, wherein the absolute pressure of underpressure distillation is 1.2kPa;

[0070] (3) adding phosphoric acid compounds (triethyl phosphonoacetate) to the system after removing small molecules to react again to obtain t...

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Abstract

The invention relates to a preparation method of polybutylene succinate, which comprises the following steps: by using succinic acid and 1, 4-butylene glycol as raw materials, sequentially carrying out an esterification reaction, a pre-polycondensation reaction and a final polycondensation reaction under the catalytic action of an efficient composite catalyst to obtain polybutylene succinate; theintrinsic viscosity of the prepared polybutylene succinate is greater than or equal to 1.8 dL.g<-1>, the L value is greater than or equal to 85, and the acid value is less than or equal to 10mol / t; the synthesis method of the efficient composite catalyst comprises the following steps: (1) adding a substance A, titanate, silicate and metal acetate into a mixed solution of 1, 4-butanediol and monohydric alcohol for reaction; wherein the substance A is amino acid or amino acid ester, and the monohydric alcohol is methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol or tert-butanol; (2) removing small molecules generated by the reaction; and (3) adding a phosphoric acid compound into the system from which the small molecules are removed, and reacting to obtain the high-efficiencycomposite catalyst.

Description

technical field [0001] The invention belongs to the technical field of synthesis of biodegradable aliphatic polyester polymer materials, and relates to a preparation method of polybutylene succinate, in particular to a method widely used in daily life for plastic absorption, blow molding, medical treatment, etc. A preparation method of high molecular weight polybutylene succinate (PBS) for degradable plastic products. Background technique [0002] On the road of polymer development, the mass production and consumption of polymer materials synthesized from petroleum and other fossil resources has brought great convenience to human life, but at the same time, it has caused the increasing scarcity of fossil resources and the continuous occurrence of "white pollution". Intensified, etc., these severe practical problems have attracted people's attention. As the society pays more and more attention to sustainable development and the promulgation of the "Plastic Restriction Order"...

Claims

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Application Information

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IPC IPC(8): C08G63/16C08G63/78C08G63/85
CPCC08G63/16C08G63/78C08G63/85
Inventor 刘建魏志勇涂著李平张伟尚祖明
Owner YINGKOU KANGHUI PETROCHEM