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Preparation method of aliphatic polycarbonate diol

A polycarbonate two, aliphatic technology, applied in the field of polycarbonate preparation, can solve the problems of separation difficulties, carbonate decarbonylation, low catalyst activity, etc., and achieve the effect of simple reaction operation and regular product structure

Inactive Publication Date: 2011-07-13
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of low catalyst activity, difficult separation and severe decarbonylation of carbonates in the above-mentioned prior art, and provide a method for preparing polycarbonate diols

Method used

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  • Preparation method of aliphatic polycarbonate diol
  • Preparation method of aliphatic polycarbonate diol
  • Preparation method of aliphatic polycarbonate diol

Examples

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Effect test

Embodiment 1

[0018] In a 250mL glass flask, add 34.30g (0.39 mole) of ethylene carbonate, 35.40g (0.30 mole) of 1,6-hexanediol and 0.67g of zinc acetate, with 26g o-xylene as entrainer, in Reaction at 140°C for 8 hours, azeotropic separation of ethylene glycol, and then vacuum distillation at 1.33KPa at this temperature until no effluent was obtained to obtain 42.20 g of white waxy solid polycarbonate diol. The average molecular weight and the content of the decarboxylated ether segment were analyzed by nuclear magnetic resonance (the same below), and the analysis results are shown in Table 1.

Embodiment 2

[0020] In a 150mL glass flask, add 13.20g (0.15 mole) of ethylene carbonate, 35.40g (0.30 mole) of 1,6-hexanediol and 0.50g of zinc acetate, with 26g p-xylene as entrainer, in React at 140°C for 4 hours, react at 1607°C for 4 hours, azeotropically separate ethylene glycol, then distill under reduced pressure at 1.99KPa at this temperature until there is no effluent, and obtain white waxy solid polycarbonate Dihydric alcohol 36.30g, analysis result is shown in Table 1.

Embodiment 3

[0022] In a 150mL glass flask, add 66.00g (0.75 mole) of ethylene carbonate, 17.70g (0.15 mole) of 1,6-hexanediol and 0.20g of zinc acetate, with 26g m-xylene as an entrainer, in Reaction at 147°C for 8 hours, azeotropic separation of ethylene glycol, and then vacuum distillation at 1.60KPa at this temperature until no effluent was obtained to obtain 37.00 g of white waxy solid. The analysis results are shown in Table 1.

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Abstract

The invention relates to a preparation method of aliphatic polycarbonate diol. The preparation method comprises the following steps of: sequentially putting diol, ethylene carbonate, a lewis acid catalyst and an entrainer into a reactor, wherein the proportion of the materials is that: the molar ratio of the ethylene carbonate to the diol is (0.5-5): 1, the using amount of the catalyst accounts for 0.1-5 percent of the total mass of the ethylene carbonate and the diol, and the using amount of the entrainer accounts for 10-54 percent of the total mass of the ethylene carbonate and the diol; reacting for 4-20h at a temperature of 120-180 DEG C under the ordinary pressure till no diol is separated out; after the reaction is ended, carrying out reduced pressure distillation at a temperature of 120-200 DEG C under the vacuum of 1.33-1.99KPa to remove unreacted raw materials and the entrainer till no fractions flow out to obtain the pure ethylene carbonate diol product. The aliphatic polycarbonate diol obtained by adopting the preparation method provided by the invention is simple and convenient for reaction operation and has a regular product structure; the carbonyl removal ratios are all less than or equal to 3.0 percent; and glycol as a byproduct cannot pollute the environment.

Description

technical field [0001] The invention belongs to the preparation of polycarbonate, in particular to a preparation method of aliphatic polycarbonate diol. Background technique [0002] Aliphatic polycarbonate diol (APC) is one of the special polyols. It is a compound with multiple carbonate groups in the molecule and terminated by hydroxyl groups. Due to the greater flexibility of its molecular chain, it can As a raw material for the synthesis of a new generation of polycarbonate polyurethane (PCU) soft segment and polyester. Polycarbonate polyurethane is a new type of polyurethane material. It not only has good mechanical properties of traditional polyurethane elastomers, but also has excellent hydrolytic stability, heat resistance, oxidation resistance and wear resistance. At present, polycarbonate diol has been widely used in the preparation of various polyurethane materials with good quality and excellent performance. With the continuous improvement of medical technology...

Claims

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Application Information

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IPC IPC(8): C08G64/38C08G64/30C08G18/44
Inventor 王家喜李金丽李云庆周宏勇王晓梅
Owner HEBEI UNIV OF TECH
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