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Method for preparing aliphatic oligo carbonate polyol

A technology of aliphatic polyol and oligocarbonate, applied in the field of preparation of aliphatic oligocarbonate polyol, can solve the problems of product discoloration, low catalytic activity, yellowing, etc.

Inactive Publication Date: 2009-05-27
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, if Ti compounds are used as catalysts, undesired discoloration (yellowing) may occur when storing the resulting product
Organotin compounds are recently considered to be potential carcinogens in humans, and their catalytic activity is not very high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] x mol Mg(NO 3 ) 2 ·6H 2 O and y mol Al(NO 3 ) 3 9H 2 O was dissolved in 100ml distilled water to make solution A, and another 2(x+y)mol NaOH and 0.5ymol NaOH were taken 2 CO 3 Also dissolved in 100ml of distilled water to make solution B, where x+y=0.1mol, x:y=2:1. First add 100ml of distilled water to a four-neck flask equipped with a thermometer, mechanical stirring, and constant pressure funnel, raise its temperature to 333K under rapid stirring, and then add solutions A and B to the flask dropwise within 1 hour at this temperature During the dropping process, the pH value of the mixed solution was kept between 8 and 10. After the dropping was completed, the final pH value was adjusted to 10 by adding NaOH. Set it aside for 24 hours, and finally filtered it with suction and washed it with water until the pH value of the filtrate was 7, then dried it at 333K for 12 hours, and roasted it at 773K for 5 hours to obtain the catalyst.

[0020] In a reaction vessel ...

Embodiment 2

[0022] x mol Ni(NO 3 ) 2 ·6H 2 O and y mol Al(NO3)3·9H 2 O was dissolved in 100ml distilled water to make solution A, and another 2(x+y)mol NaOH and 0.5ymol NaOH were taken 2 CO 3 Also dissolved in 100ml of distilled water to make solution B, where x+y=0.1mol, x:y=3:1. First add 100ml of distilled water to a four-neck flask equipped with a thermometer, mechanical stirring, and constant pressure funnel, raise its temperature to 333K under rapid stirring, and then add solutions A and B to the flask dropwise within 1 hour at this temperature During the dropping process, the pH value of the mixed solution was kept between 8 and 10. After the dropping was completed, the final pH value was adjusted to 10 by adding NaOH. Set it aside for 24 hours, and finally filtered it with suction and washed it with water until the pH value of the filtrate was 7, then dried it at 333K for 12 hours, and roasted it at 773K for 5 hours to obtain the catalyst.

[0023] In a reaction vessel equip...

Embodiment 3

[0025] x mol Zn(NO 3 ) 2 ·6H 2 O and y mol Al(NO 3 ) 3 9H 2 O was dissolved in 100ml distilled water to make solution A, and another 2(x+y)mol NaOH and 0.5ymol NaOH were taken 2 CO 3 Also dissolved in 100ml of distilled water to make solution B, where x+y=0.1mol, x:y=4:1. First add 100ml of distilled water to a four-neck flask equipped with a thermometer, mechanical stirring, and constant pressure funnel, raise its temperature to 333K under rapid stirring, and then add solutions A and B to the flask dropwise within 1 hour at this temperature During the dropping process, the pH value of the mixed solution was kept between 8 and 10. After the dropping was completed, the final pH value was adjusted to 10 by adding NaOH. Set it aside for 24 hours, and finally filtered it with suction and washed it with water until the pH value of the filtrate was 7, then dried it at 333K for 12 hours, and roasted it at 773K for 5 hours to obtain the catalyst.

[0026]In a reaction vessel e...

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PUM

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Abstract

The invention discloses a making method of aliphatic oligocarbonate polyol under normal pressure, which is characterized by the following: setting the quantity of aliphatic polyol at 0.01ppm-10,000ppm corresponding to the quantity of catalyst; adding aliphatic polyol and catalyst in the reactor; heating to 80-200 deg.c; setting the molar rate of organic carbonate monomer and aliphatic polyol at 1:0.1- 10 to react 3-4h under 10-105Pa at 100-200 deg.c.

Description

technical field [0001] The invention relates to a method for preparing aliphatic oligocarbonate polyol through transesterification of organic carbonate and aliphatic polyol. Background technique [0002] Aliphatic oligocarbonate polyols have long been known as important intermediate products in the production of plastics, paints and adhesives. They can generally be obtained by aliphatic polyols with phosgene (DE-A 1 595 446), bis-chloroformates (DE-A 857 948), diaryl carbonates (DE-A 1 915 908), cyclic Reactive preparation of carbonates (DE-A 2 523 352), ethylene carbonate or dialkyl carbonates (DE-A 2 555 805). [0003] When diaryl carbonate (such as: diphenyl carbonate) is reacted with aliphatic polyhydric alcohol (such as: 1,6-hexanediol), by removing the by-product alcohol compound (such as: phenol ), a sufficient reaction conversion can be achieved (EP-A 0 533 275). But only about 13% of the diphenyl carbonate remains in the product, the rest is distilled off as phen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/02C08G64/30
Inventor 王心葵封悦霞亢茂青殷宁李其峰王军威
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI