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Method for preparing aliphatic copolymerized carbonic ester polyols by stannous chloride complex catalysis

A technology of aliphatic polyol and copolycarbonate, which is applied in the field of polyurethane materials, can solve the problems of low catalytic efficiency, inconvenient use, poor performance of polycarbonate polyol, etc., and achieve the effect of less catalyst addition and easy use

Active Publication Date: 2019-07-26
HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All of the above catalysts have the disadvantage of low catalytic efficiency
In addition, when polycarbonate polyols are prepared by transesterification and polycondensation, a single polyol is usually used as a raw material, which is prone to deficiencies such as poor performance of polycarbonate polyols. It exists in the form of crystalline solid, which is inconvenient to use in the industrial production of polyurethane, and requires additional heating to melt or dissolve in a solvent
Furthermore, when crystalline polycarbonate polyol is used as the raw material of the soft segment, the appearance of the obtained polyurethane is often opaque, which leads to limitations in application and cannot be applied to the preparation of transparent appearance articles

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] 156g (1.32mol) of 1,6-hexanediol, 137.5g (1.32mol) of 1,5-pentanediol and 120mg (0.392mmol) of SnCl 2 (dab) 2 Add to a reactor equipped with a heating and stirring system, a temperature measuring system, a fractionation system and a constant pressure funnel. Pass argon to exhaust the air in the reaction system, stir under argon atmosphere and raise the temperature to 140°C under normal pressure, add 312g (3.46mol) of dimethyl carbonate dropwise, the dropwise addition is completed within 30 minutes, then stir and heat to reflux for 6 hours . Next, the temperature of the distillation head is controlled at 60-64°C, the mixture of by-product methanol and dimethyl carbonate is distilled, and the heating temperature is gradually increased from 140°C to 220°C. Lower the pressure at 220°C to 5kPa, and the reaction time is 3 to 4 hours. After cooling, a colorless transparent viscous liquid copolycarbonate polyol is obtained, and the yield reaches 96%. Its hydroxyl value is 50...

example 2

[0023] 140g (1.18mol) of 1,6-hexanediol, 123.8g (1.18mol) of 1,5-pentanediol, 23.8g (0.264mol) of 1,4-butanediol and 120mg (0.392mmol) of SnCl 2 (dab) 2 Add to a reactor equipped with a heating and stirring system, a temperature measuring system, a fractionation system and a constant pressure funnel. Pass argon to exhaust the air in the reaction system, stir under argon atmosphere and raise the temperature to 140°C under normal pressure, add 312g (3.46mol) of dimethyl carbonate dropwise, the dropwise addition is completed within 30 minutes, then stir and heat to reflux for 6 hours . Next, the temperature of the distillation head is controlled at 60-64°C, the mixture of by-product methanol and dimethyl carbonate is distilled, and the heating temperature is gradually increased from 140°C to 220°C. Lower the pressure at 220°C to 5kPa, and the reaction time is 3 to 4 hours. After cooling, a colorless transparent viscous liquid copolycarbonate polyol is obtained, and the yield r...

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PUM

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Abstract

The invention belongs to the field of polyurethane materials, and discloses a method for preparing aliphatic copolymerized carbonic ester polyols by stannous chloride complex catalysis. The method includes the steps: adding catalysts, mixed aliphatic polyols and dimethyl carbonate into a drying reactor with inert gas atmosphere according to proportion; performing reflux reaction at the temperatureof 130-140 DEG C under normal pressure; slowly heating the materials to reach the temperature of 140-220 DEG C; cooling the materials to directly obtain the colorless transparent viscous liquid copolymerized carbonic ester polyols. According to the preparation method, novel double active centers (metallic tin (II) and exposed nitrogen atoms) SnCl2(dab)2 are selected as the catalysts, the copolymerized carbonic ester polyols are synthesized, yield reaches up to 95% or more, and industrial production is facilitated.

Description

technical field [0001] The invention belongs to the field of polyurethane materials and relates to a preparation method of aliphatic copolycarbonate polyol. Background technique [0002] Polycarbonate polyol is a high-performance polyurethane raw material, which combines the excellent characteristics of both polyether type and polyester type polyurethane, such as high mechanical strength, excellent hydrolysis resistance and solvent resistance, heat fading resistance , Scratch resistance and weather resistance, etc. Therefore, its synthesis method and application research have received extensive attention. Among them, the transesterification polycondensation method has the following advantages: the source of raw materials is green and environmentally friendly, and the reaction conditions such as reaction temperature and reaction pressure are relatively mild. The transesterification polycondensation method has become the best synthesis method for polycarbonate polyols. The ch...

Claims

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Application Information

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IPC IPC(8): C08G64/30C08G64/02
CPCC08G64/0208C08G64/305
Inventor 张陆军李旭郝旭东周晓楠刘海涛秦瑜郭永春于玉建袁梦旗王晋王金良张淑芳
Owner HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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