Preparation method of poly(carbonic ester-ether)polyol

一种多元醇、碳酸酯的技术，应用在聚合物领域，能够解决浪费生产原料、反应时间延长、达不到生产的要求等问题，达到减少时间、诱导期短、反应时间短的效果

Active Publication Date: 2015-11-18
HUAFON GROUP +1
View PDF10 Cites 19 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, with double metal cyanide (DMC) as catalyzer, the method for preparing poly(carbonate-ether) polyol with carbon dioxide and epoxide as raw material has obtained extensive reports: Kuyper (US4826887, US4826953), Hinz (US6173599B1 ) etc. have reported the use of low molecular weight polypropylene glycol as the initiator, based on Zn 3 [Co(CN) 6 ] 2 The double metal cyanide compound is a catalyst, and carbon dioxide and propylene oxide are the method for preparing poly(carbonate-ether) polyols as raw materials; Reactivity, the polymerization reaction is carried out at 110 ° C and higher temperatures, which inevitably leads to a very low content of carbonate units ( 20%), and the generation of by-product not only wastes production raw material, also can increase separation cost; content, the reaction time will be greatly extended, and the production requirements cannot be met.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of poly(carbonic ester-ether)polyol
  • Preparation method of poly(carbonic ester-ether)polyol
  • Preparation method of poly(carbonic ester-ether)polyol

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0024] The invention provides a kind of preparation method of poly(carbonate-ether) polyol, comprising:

[0025] reacting carboxylic acid and epoxide to obtain an intermediate product; the acidity constant of the carboxylic acid is 0.2-4;

[0026] in Zn 3 [Co(CN) 6 ] 2 Under the action of the rare earth doped double metal cyanide, the intermediate product and carbon dioxide are polymerized to obtain poly(carbonate-ether) polyol;

[0027] The Zn 3 [Co(CN) 6 ] 2 The rare earth doped double metal cyanide is composed of rare earth salt compound, zinc salt compound, K 3 [Co(CN) 6 ] and tert-butanol prepared.

[0028] The invention reacts carboxylic acid and epoxide to obtain an intermediate product; the acidity constant of the carboxylic acid is 0.2-4. In an embodiment of the present invention, the reaction temperature of the carboxylic acid and the epoxide is 40°C to 150°C; in other embodiments, the reaction temperature of the carboxylic acid and the epoxide is 60°C to 12...

Embodiment 1

[0039] 0.78g of YCl 3 and 11.42g of ZnCl 2 Dissolve in a mixed solution formed by 60 mL of deionized water and 30 mL of tert-butanol, heat the mixed solution to 50 °C and keep the temperature for 20 min, and add 1.32 g of Analytical grade K 3 [Co(CN) 6 ] and 20mL of deionized water, the reaction time is 45min, and the reaction is carried out at 50°C. After the dropwise addition, continue to stir at 50°C for 1h to obtain a suspension;

[0040] Centrifuge the suspension at a speed of 5000 rpm for 10 min with a centrifuge, pour out the separated clear liquid, and wash the sediment with 60 mL of a mixed solution of tert-butanol and water at 50 ° C for 5 times, and finally Wash once with tert-butanolized pulp, the volume ratios of tert-butanol and water in the mixed solution of tert-butanol and water are 30 / 30, 36 / 24, 42 / 18, 48 / 12, 54 / 6, respectively. The stirring speed is 300rpm, and the washing time of each pulping is 10min. The suspension after each pulping is centrifuged wi...

Embodiment 2

[0042] Place the weighing bottle at 80°C and fill it with CO 2 gas for 6 times, and the weighing bottle was cooled to room temperature, and the above-mentioned weighing bottle was used to weigh trifluoroacetic acid, and the autoclave was evacuated at 80°C to 2 The gas was treated 6 times and then cooled to room temperature, 8g of trifluoroacetic acid was added into the above-mentioned autoclave, 100mL of propylene oxide was added into the autoclave, stirred at a speed of 500rpm, and the autoclave was placed in a constant temperature of 70°C. Carry out reaction in warm bath, the time of reaction is 5min, obtains intermediate product;

[0043] The Zn that 60mg embodiment 1 prepares 3 [Co(CN) 6 ] 2 The rare earth-doped double metal cyanide compound is added in the above-mentioned autoclave, and carbon dioxide is passed into the above-mentioned autoclave to make the above-mentioned intermediate product and carbon dioxide carry out polymerization reaction, and the reaction press...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
polydispersity indexaaaaaaaaaa
polydispersity indexaaaaaaaaaa
polydispersity indexaaaaaaaaaa
Login to view more

Abstract

The present invention provides a preparation method of poly(carbonic ester-ether)polyol. The method comprises the steps of: reacting carboxylic acid with acidity constant of 0.2-4with epoxide to obtain an intermediate product; reacting the intermediate product with carbon dioxide for a polymerization reaction under the effect of Zn3[Co(CN)6]2 rare earth-doped double metal cyanide to obtain poly(carbonic ester-ether)polyol. The preparation method of poly(carbonic ester-ether)polyol provided by the present invention employs carboxylic acid with appropriate acidity constant as an initiator; carboxylic acid is used to activate the epoxide; and the activated in-situ generated polyethers with different molecular weight are used as a chain transfer agent for participating polymerization reaction of carbon dioxide and an epoxide under the effect of Zn3[Co(CN)6]2 rare earth-doped double metal cyanide. The preparation method of the poly(carbonic ester-ether)polyol the has short reaction time, and content of a byproduct propylene carbonate is low.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a preparation method of poly(carbonate-ether) polyols. Background technique [0002] Carbon dioxide is a greenhouse gas and can be used as carbon and oxygen resources at the same time. How to efficiently use carbon dioxide resources has become a hot research topic today. At present, take double metal cyanide (DMC) as catalyzer, take carbon dioxide and epoxide as the method for raw material preparation poly(carbonate-ether) polyol has obtained extensive report: Kuyper (US4826887, US4826953), Hinz (US6173599B1 ) etc. have reported the use of low molecular weight polypropylene glycol as the initiator, based on Zn 3 [Co(CN) 6 ] 2 The double metal cyanide compound is a catalyzer, is the method for raw material preparation poly(carbonate-ether) polyol with carbon dioxide and propylene oxide; Reactivity, the polymerization reaction is carried out at 110 ° C and higher temperatures,...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34
CPCC08G64/32B01J27/26C08G64/34B01J23/80C08K3/28C08L69/00
Inventor 刘顺杰秦玉升王献红乔立军王佛松
Owner HUAFON GROUP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap