Process for preparing high-molecular aliphatic polyester

An aliphatic polyester, high molecular weight technology, applied in the field of preparation of high molecular weight aliphatic polyester, can solve the problems of difficult to obtain a variety of polyester varieties, difficult to use in medical and food fields, high toxicity of diisocyanates, etc. The effect of improving the degree of reaction and molecular weight, easy recycling, high molecular weight and yield

Inactive Publication Date: 2004-03-17
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the amount of dihydric alcohol is large and needs to be recovered; the reaction temperature is high and difficult to control; high vacuum is required and the equipment is expensive; and the raw material diisocyanate is highly toxic and difficult to use in the medical and food fields
The disadvantage is that ethylene oxide is highly toxic and difficult to control; there are few types of similar monomers, and there is little room for choice, and it is difficult to obtain a variety of polyester varieties; it is easy to form polyether chain links and reduce the melting point of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a 250ml four-necked flask, add 0.3mol succinic acid, 0.27-0.33mol butanediol, 0.005-0.5g stannous chloride catalyst, 100ml decahydronaphthalene, install a mechanical stirrer, a water separator, a thermometer, and Nitrogen is passed, heated with a silicone oil bath, reacted at 100-180°C for 0.1-12h, and then heated to 150°C-200°C for 1-14h. The total reaction time is 1-14h. Stirring and heating were stopped, and the decahydronaphthalene was poured out after the reaction system was cooled, and then vacuum-dried (0.094Mpa, 120°C, 8h) to obtain the product with a yield of 96.0%. IR: 1717cm -1 , HNMR: δ1.69, δ2.60, δ4.09, the area ratio of the three peaks is 1:1:1, proving that the obtained product is polybutylene succinate. The number average molecular weight measured by GPC is 78912, CHCl at 20°C 3 The medium intrinsic viscosity is 1.68dl / g.

Embodiment 2

[0023] The raw materials in Example 1 were changed to adipic acid and hexanediol, and other conditions were the same as in Example 1 to obtain the product with a yield of 96.8%. IR: 1727cm -1 ; HNMR: δ 1.33, δ 1.62, δ 2.28, δ 4.02, the area ratio of the four peaks is 1: 2: 1: 1, which proves that the obtained product is polyethylene adipate. 20℃CHCl 3 The medium intrinsic viscosity is 1.65dl / g.

Embodiment 3

[0025] The raw materials in Example 1 were changed to succinic acid and hexanediol, and other conditions were the same as in Example 1 to obtain the product with a yield of 95.8%. IR: 1724cm -1 ; HNMR: δ1.34, δ1.60, δ2.58, δ4.05, the area ratio of the four peaks is 1:1:1:1, which proves that the obtained product is polyhexamethylene succinate. 20℃CHCl 3 The intrinsic viscosity is 1.51dl / g.

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PUM

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Abstract

The present invention relates to the preparation process of high molecular weight aliphatic polyester. Aliphatic diatomic acid and aliphatic diatomic alcohol are made to react in decalin solvent with catalyst of stannous chloride, stannous zincate, n-butyl titanate, isopropyl titanate, etc at 100-200 deg.c for 1-14 hr to obtain the high molecular weight aliphatic polyester. The preparation process of the present invention is simple, low in cost, easy to control and high in yield, and the product has high molecular weight and high purity.

Description

[0001] Field [0002] The invention relates to a preparation method of high molecular weight aliphatic polyester. Background technique [0003] The aliphatic polyester can be used as agricultural mulch, fishing gear, plastic packaging bags, foam plastics, disposable tableware, women's hygiene products and disposable medical appliances, etc., which are difficult to recycle plastic products, and play an important role in solving the increasingly serious white pollution. effect. [0004] JP2002020474 invention discloses a preparation method of aliphatic polyester. The method is to add dibasic acid and dibasic alcohol into decahydronaphthalene solvent, use divalent organic stannoxane as a catalyst, react at 150 DEG C for 1 hour, and then react at 193 DEG C for 72 hours to obtain the product. The number average molecular weight of the obtained product was 73600. The disadvantage of this method is that the reaction time is long, the energy consumption is large, and it is difficul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/00
Inventor 谭惠民孙杰罗运军张大伦张维
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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