Preparation method of poly (carbonate ester-ether) trihydric alcohol

A technology of trihydric alcohols and carbonates, applied in the field of polymers, can solve problems such as difficult insertion of carbon dioxide or epoxy monomers, low content of carbonate units, long reaction induction period, etc.

Active Publication Date: 2014-06-25
JUYUAN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Therefore, low-molecular-weight poly(carbonate-ether) polyols prepared by DMC-catalyzed copolymerization of carbon dioxide and epoxides have problems such as low content of carbonate units, high content of by-product cyclic carbonates, and high polymerization temperature. The adduct of glycerol and epoxide is directly used as a chain transfer agent to participate in the copolymerization of carbon dioxide and epoxide to prepare poly(carbonate-ether) triol. Due to the strong nucleophilicity of the terminal hydroxyl group, it is complexed with the active center of the catalyst. Strong and difficult to be replaced, making it difficult for carbon dioxide or epoxy monomer to insert into the active center of the catalyst, resulting in a longer reaction induction period

Method used

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  • Preparation method of poly (carbonate ester-ether) trihydric alcohol
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  • Preparation method of poly (carbonate ester-ether) trihydric alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Preparation of Rare Earth Doped Y-DMC

[0054] 0.78g (0.004mol) YCl 3 and 11.42 g (0.084 mol) ZnCl 2 Dissolve in a mixed solution formed by 60ml deionized water and 30ml tert-butanol, heat the formed solution to 50°C and keep the temperature constant for 20min, then add 1.32g (0.004 mol) analytically pure K 3 [Co(CN) 6 ] and 20ml of deionized water, add dropwise for 45 minutes, keep the reaction constant at 50°C, stir for 1 hour to obtain a suspension; centrifuge the obtained suspension for 10 minutes with a centrifuge (5000rpm), and pour out the separated clear liquid , the sediment was successively treated with 60ml of 50°C TBA and H 2 The mixed solution of O was pulped and washed 5 times, and finally washed once with TBA pulp, TBA and H 2 TBA and H in the mixed solution of O 2 The volume ratio of O was 30 / 30, 40 / 20, 50 / 10, 60 / 0 respectively, the stirring speed during the washing process was 5000 rpm, the centrifugation time was 10 min, and then the obtained sed...

Embodiment 2

[0056] Preparation of Rare Earth Doped Nd-DMC

[0057] 0.1g (0.004mol) Nd(NO 3 ) 3and 11.42 g (0.084 mol) ZnCl 2 Dissolve in a mixed solution formed by 60ml deionized water and 30ml tert-butanol, heat the formed solution to 50°C and keep the temperature constant for 20min, then add 1.32g (0.004 mol) analytically pure K 3 [Co(CN) 6 ] and 20ml of deionized water, add dropwise for 45 minutes, keep the reaction constant at 50°C, stir for 1 hour to obtain a suspension; centrifuge the obtained suspension for 10 minutes with a centrifuge (5000rpm), and pour out the separated clear liquid , the sediment was successively treated with 60ml of 50°C TBA and H 2 The mixed solution of O was pulped and washed 5 times, and finally washed once with TBA pulp, TBA and H 2 TBA and H in the mixed solution of O 2 The volume ratio of O was 30 / 30, 40 / 20, 50 / 10, 60 / 0 respectively, the stirring speed during the washing process was 5000 rpm, the centrifugation time was 10 min, and then the obtain...

Embodiment 3

[0059] Preparation of Rare Earth Doped La-DMC

[0060] 0.98g (0.004mol) La(Cl 3 CCOO) 3 and 11.42 g (0.084 mol) ZnCl 2 Dissolve in a mixed solution formed by 60ml deionized water and 30ml tert-butanol, heat the formed solution to 50°C and keep the temperature constant for 20min, then add 1.32g (0.004 mol) analytically pure K 3 [Co(CN) 6 ] and 20ml of deionized water, add dropwise for 45 minutes, keep the reaction constant at 50°C, stir for 1 hour to obtain a suspension; centrifuge the obtained suspension for 10 minutes with a centrifuge (5000rpm), and pour out the separated clear liquid , the sediment was successively treated with 60ml of 50°C TBA and H 2 The mixed solution of O was pulped and washed 5 times, and finally washed once with TBA pulp, TBA and H 2 TBA and H in the mixed solution of O 2 The volume ratio of O was 30 / 30, 40 / 20, 50 / 10, 60 / 0, respectively, the stirring speed during washing was 300 rpm, the centrifugation time was 10 min, and then the obtained sed...

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Abstract

The invention discloses a preparation method of poly (carbonate ester-ether) trihydric alcohol. According to the preparation method of the poly (carbonic ester-ether) trihydric alcohol, carbon dioxide, an epoxy compound and tribasic acid have a polymerization reaction under the action of a catalyst to obtain the poly (carbonic ester-ether) trihydric alcohol; the catalyst is rare earth doped Zn3[Co(CN)6]2 based bimetallic cyanide; the tribasic acid is one or more than one of oxalosuccinate, tricarballylic acid, 1,3,5- trimesic acid, 1,2,4-benzenetricarboxylic acid and phosphoric acid; and the time of polymerization reaction is 3-9 hours. The preparation method of the poly (carbonic ester-ether) trihydric alcohol has short reaction induction period and short reaction time and has high carbonic ester unit content and low byproduct cyclic carbonic ester content.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a preparation method of poly(carbonate-ether) trihydric alcohol. Background technique [0002] Carbon dioxide is a major greenhouse gas and can be utilized as carbon and oxygen resources at the same time. How to efficiently utilize carbon dioxide resources has become a hot research topic today. The researchers found that the copolymerization of carbon dioxide and epoxy compounds to prepare polycarbonate is an effective way to utilize carbon dioxide. Among them, low-molecular-weight polymer triols can be used as raw materials for the production of polyurethane for the production of foaming materials, elastomers, sealants, coatings and adhesives. Different types of triols can synthesize different types of polyurethanes, and endow polyurethanes with different properties to meet various needs. Polymer triols mainly include polyether triols, polyester triols and poly(carbonate-eth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34C08G64/18
Inventor 刘顺杰秦玉升王献红王佛松
Owner JUYUAN CHEM IND CO LTD
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