Preparing method of poly (carbonic ester-ether) polyalcohol

A carbonate and polyol technology, applied in the polymer field, can solve the problems of low monomer conversion rate and activity

Active Publication Date: 2012-08-01
南通华盛高聚物科技股份有限公司
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Problems solved by technology

[0006] Hyde KW adopts polyhydric alcohol as chain transfer agent in the Chinese patent document whose publication number is CN 101511909A, to based on Zn 3 [Co(CN) 6 ] 2 The DMC prepared poly(carbonate-ether) polyol as a catalyst, the polymer content in the reacted system is no more than 20wt%, the cyclic carbonate content is between 9wt% and 52wt%, and the carbonate unit content in the polymer Between 1% and 35%, the monomer conversion and activity in this method are low

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[0027] The invention discloses a preparation method of poly(carbonate-ether) polyol, comprising the following steps: doping with rare earth based on Zn 3 [Co(CN) 6 ] 2 The double metal cyanide compound is used as a catalyst, and carboxylic acid is used as a chain transfer agent, and carbon dioxide and epoxy compounds are polymerized to obtain poly(carbonate-ether) polyols, and the rare earth-doped Zn-based 3 [Co(CN) 6 ] 2 The double metal cyanide is composed of rare earth salt compound, zinc salt compound, K 3 [Co(CN) 6 ] and tert-butanol (TBA) preparation.

[0028] According to the present invention, the epoxy compound is preferably one or more of ethylene oxide, propylene oxide, butylene oxide, cyclohexane oxide and epichlorohydrin. Described carboxylic acid is preferably one or more in aliphatic carboxylic acid, alicyclic carboxylic acid and aromatic carboxylic acid, wherein, described aliphatic carboxylic acid preferably comprises oxalic acid, malonic acid, succinic ...

Embodiment 1

[0042] The preparation of the Y-DMC of embodiment 1 rare earth doping

[0043] 0.78g (0.004mol) YCl 3 and 11.42g (0.084mol) ZnCl 2 Dissolve in the mixed solution formed by 60mL deionized water and 30mL tert-butanol, heat the formed solution to 50°C and keep the temperature for 20min, then add 1.32g (0.004 mol) analytically pure K 3 [Co(CN) 6 ] and 20mL of deionized water, the dropwise addition takes 45min, and the reaction is kept constant at 50°C. After the dropwise addition, continue to stir at 50°C for 1h to obtain a suspension; the resulting suspension is centrifuged with a centrifuge (5000rpm) for 10min , poured out the separated clear liquid, and the sediment was successively washed 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 is 30 / 30, 36 / 24, 42 / 18, 48 / 12, 54 / 6 respectively, the stirring speed of slurry washing is ...

Embodiment 2

[0044] Example 2 Preparation of Rare Earth Doped Nd-DMC

[0045] 1.0g (0.004mol) NdCl 3 and 11.42g (0.084mol) ZnCl 2 Dissolve in the mixed solution formed by 60mL deionized water and 30mL tert-butanol, heat the formed solution to 50°C and keep the temperature for 20min, then add 1.32g (0.004 mol) analytically pure K 3 [Co(CN) 6 ] and 20mL of deionized water, the dropwise addition took 45min, keeping the reaction temperature constant at 50°C, and continuing to stir at 50°C for 1h after the dropwise addition; the resulting suspension was centrifuged with a centrifuge (5000rpm) for 10min, poured out and separated The supernatant and the sediment were washed with 60mL 50℃ 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 is 30 / 30, 36 / 24, 42 / 18, 48 / 12, 54 / 6 respectively, the stirring speed of slurry washing is 300rpm, and the washing time of each sl...

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Abstract

The invention discloses a preparing method of poly (carbonic ester-ether) polyalcohol. Rare-earth doped bi-metal cyanides based on Zn3[Co(CN)6]2 serve as catalysts, carboxylic acids serve as chain transfer agents, and carbon dioxide and epoxy compounds are performed with a copolymerization reaction to obtain the poly (carbonic ester-ether) polyalcohol. Compared with the prior art, the carboxylic acids serve as chain transfer agents, and due to the fact that the carboxylic acids are strong in coordination capability, faster in chain transfer, capable of restraining continuous inserting of epoxy monomers and free of ether structure, unit content of carbonic ester is improved, and the prepared poly (carbonic ester-ether) polyalcohol has higher carbonic ester unit content. Experimental results indicate that molecular weight of the prepared poly (carbonic ester-ether) polyalcohol is 1500g/mol-5000g/mol, molecular weight distribution is 1.11-1.50, unit content of the carbonic ester is 40%-80%, catalytic activity is larger than 1.0kg/gLn-DMC, and cyclic carbonic ester content is less than 10wt%.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a method for preparing poly(carbonate-ether) polyols. Background technique [0002] Carbon dioxide is a cheap, easy-to-obtain, non-toxic chemical raw material with abundant reserves, so 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 poly(carbonate-ether) polyols can be used as raw materials for polyurethanes and have the advantages of both polycarbonate polyols and polyether polyols, so they have become an important development direction for carbon dioxide copolymers. [0003] Currently, the preparation of poly(carbonate-ether) polyols using double metal cyanide (DMC) as catalyst and carbon dioxide and epoxide as raw material has been widely repor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34
Inventor 高永刚王献红赵晓江王佛松
Owner 南通华盛高聚物科技股份有限公司
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