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A kind of biodegradable alternating aliphatic polyester amide and its preparation method

A polyester amide, aliphatic technology, applied in the field of polymer materials, can solve problems such as high structure, achieve broad application prospects, good biodegradability, and fewer by-products.

Active Publication Date: 2021-10-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the biodegradable alternating aliphatic polyester amide cannot have both higher molecular weight and more regular structure in the prior art, and to provide a biodegradable alternating aliphatic polyester amide and its Preparation

Method used

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  • A kind of biodegradable alternating aliphatic polyester amide and its preparation method
  • A kind of biodegradable alternating aliphatic polyester amide and its preparation method
  • A kind of biodegradable alternating aliphatic polyester amide and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0057] A preparation method of biodegradable alternating aliphatic polyester amide, the process is as follows:

[0058] (1) Add 186.7g (3mol) of ethanolamine and 200ml methanol into a 2L three-necked flask, and under mechanical stirring, pass N 2 , and stabilize the system temperature at 0°C, then slowly add 303.67g (1.5mol) dibutyl oxalate through the normal pressure funnel for about 2 hours, after the dropwise addition is completed, continue the reaction for 0.5 hours, cool to below 0°C and suction filter, and use Wash with 150ml*3 methanol and dry in a vacuum oven at 50°C for 24 hours to obtain 210g of N,N-di(2-hydroxyethyl)oxamide, such as figure 1 Shown, its Tm (melting point) is 171 ℃;

[0059] (2) Weigh 176.17g (1mol) of N,N-di(2-hydroxyethyl)oxamide, 146.14g (1mol) of adipic acid, 0.0332g of tin protochloride and 0.1612g of ammonium dihydrogen phosphate and mix them evenly. Nitrogen replacement three times, in N 2 In the atmosphere, react at 200°C for 3 hours;

[0...

Embodiment 2

[0070] A preparation method of biodegradable alternating aliphatic polyester amide, the process is as follows:

[0071] (1) Preparation of straight chain oxamide diol: 225.3g (3mol) of 3-amino-1-propanol and 250ml methyl alcohol are added in the 2L three-necked flask, under mechanical stirring, pass into N 2 , and stabilize the system temperature at 20°C, then slowly add 219.2g (1.5mol) diethyl oxalate through the normal pressure funnel for about 2 hours, continue the reaction for 1.5 hours after the dropwise addition, cool to below 5°C and filter with suction, and use 150ml *3 Washed with methanol, dried in a vacuum oven at 50°C for 24 hours to obtain 229.8g of N,N-di(3-hydroxypropyl)oxamide, such as figure 1 As shown, its Tm is 166°C;

[0072] (2) Weigh 204.2g (1mol) of N,N-di(3-hydroxypropyl)oxamide, 146.14g (1mol) of adipic acid, 0.1752g of stannous octoate and 0.1752g of diammonium hydrogen phosphate, and mix them evenly under nitrogen gas permutation three times, at N ...

Embodiment 3

[0076] A preparation method of biodegradable alternating aliphatic polyester amide, the process is as follows:

[0077] (1) Preparation of straight-chain oxamide diol: 267.42g (3mol) of 4-amino-1-butanol and 250ml methanol are added in a 2L three-necked flask, under mechanical stirring, feed N2, and the temperature of the system is stabilized at 20°C, then slowly add 261.29g (1.5mol) dipropyl oxalate through the normal pressure funnel for about 2 hours, continue the reaction for 1.5 hours after the dropwise addition, cool to below 5°C and filter with suction, and wash with 150ml*3 methanol, at 50 Under vacuum oven drying at ℃ for 24 hours to obtain 283.62g N,N-two (4-hydroxybutyl) oxalamide, such as figure 1 As shown, its Tm is 172°C;

[0078] (2) Weigh 255.52g (1mol) of N,N-di(4-hydroxybutyl)oxamide, 118.1g (1mol) of succinic acid, 0.3736g of octyl stannous chloride and 0.7472g of calcium hydrogen phosphate and mix evenly, Nitrogen replacement three times, in N 2 In the at...

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Abstract

The invention relates to a biodegradable alternating aliphatic polyester amide and a preparation method thereof. The preparation method is as follows: under the action of a catalyst and a phosphorus-containing cocatalyst, linear oxamide diol and a linear aliphatic diacid are prepared The polycondensation reaction produces a biodegradable alternating aliphatic polyester amide, wherein the phosphorus-containing cocatalyst is an ammonium salt containing hydrogen phosphate, a calcium salt containing hydrogen phosphate, a sodium salt containing hydrogen phosphate or a magnesium salt containing hydrogen phosphate; The main chain of the finally obtained biodegradable alternating aliphatic polyester amide is formed by alternating bonding of straight-chain oxamide diol units and straight-chain aliphatic diacid units, and the biodegradable alternating aliphatic polyester amide The weight average molecular weight is 50,000 to 1,000,000 g / mol. The preparation method of the present invention is simple to operate, pollution-free, and has few by-products. The finally obtained biodegradable alternating aliphatic polyester amide has good biodegradability, and the alternating structure is regular, the molecular weight is high, and the thermal and mechanical properties are excellent. good.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a biodegradable alternating aliphatic polyester amide and a preparation method thereof, in particular to a biodegradable alternating aliphatic polyester amide with high mechanical strength, good toughness and biodegradability. its preparation method. Background technique [0002] With the public's increasing concern about environmental issues, more and more researchers have focused their attention on the development of new biodegradable polymers. Polybutylene succinate (PBS), polyhydroxybutyrate-hydroxyvalerate (PHBV) and polylactic acid (PLA) are currently the most typical biodegradable polymers and have been industrialized. They are used in daily plastic products, Some applications have been found in packaging materials and medical products. However, aliphatic polyesters generally have problems such as strong hydrophobicity, poor heat resistance, low mechanical proper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/44
CPCC08G69/44C08G2230/00
Inventor 刘涛何勇马博谋周亮王学利俞建勇
Owner DONGHUA UNIV
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