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Preparation method of poly(carbonic ester-ether) glycol and preparation method of catalyst thereof

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

Active Publication Date: 2012-05-02
南通华盛高聚物科技股份有限公司
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  • Claims
  • Application Information

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Problems solved by technology

[0006] Hyde KW uses a substantially amorphous Zn-based 3 [Co(CN) 6 ] 2 The DMC prepared poly(carbonate-ether) polyol, the polymer content in the system after reaction is no more than 20wt%, the cyclic carbonate content is between 9wt%~52wt%, and the carbonate unit content in the polymer is 1 % to 35%, the number average molecular weight is about 3000g / mol, the monomer conversion rate is very low in this method, and the activity is also very low

Method used

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  • Preparation method of poly(carbonic ester-ether) glycol and preparation method of catalyst thereof
  • Preparation method of poly(carbonic ester-ether) glycol and preparation method of catalyst thereof
  • Preparation method of poly(carbonic ester-ether) glycol and preparation method of catalyst thereof

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[0040] The invention discloses a preparation method of poly(carbonate-ether) glycol, comprising the following steps:

[0041] Zn-based doped with rare earth 3 [Co(CN) 6 ] 2 The double metal cyanide (abbreviated as Ln-DMC) is used as a catalyst, and carbon dioxide and epoxy compounds are polymerized in the presence of a chain transfer agent to obtain poly(carbonate-ether) glycols. 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 preparation.

[0042] In the present invention, the epoxy compound is preferably one or more of ethylene oxide, propylene oxide, butylene oxide, cyclohexane oxide and epichlorohydrin. The chain transfer agent is preferably ethylene glycol, propylene glycol, butanediol, pentanediol, cyclopentanediol, hexanediol, cyclohexanediol, heptanediol, ethylene glycol, diethylene glycol , triethylene glycol, tetraethylene glycol, monopropylene...

Embodiment 1

[0055] The preparation of the Y-DMC1 of embodiment 1 rare earth doping

[0056] 0.39g (0.002mol) 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 constant for 20min, then add 1.32g ( 0.004mol) 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 w...

Embodiment 2

[0057] The preparation of the Y-DMC2 of embodiment 2 rare earth doping

[0058] 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 2The volume ratio of O is 30 / 30, 36 / 24, 42 / 18, 48 / 12, 54 / 6 respectively, the stirring speed of slurry washing is ...

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Abstract

The invention discloses a preparation method of rare earth-doped double metal cyanide catalyst and a method for preparing low molecular weight poly (carbonic ester-ether) glycol by using the catalyst to catalyze the copolymerization of carbon dioxide and epoxy compounds. The preparation method of poly (carbonic ester-ether) glycol comprises the following steps: using rare earth-doped double metalcyanide based on Zn3[Co(CN)6]2 as a catalyst, and letting carbon dioxide and epoxy compounds be subject to polymerization in the presence of chain transferring agent to obtain the poly(carbonic ester-ether) glycol. According to the invention, compared with the prior art, the rare earth-doped double metal cyanide based on Zn3[Co(CN)6]2 used herein efficiently catalyzes the copolymerization of carbon dioxide and epoxy compounds under the effect of chain transferring agent; and compared with double metal cyanide without doping, the rare earth-doped double metal cyanide based on Zn3[Co(CN)6]2 used herein has higher catalytic activity and better product selectivity.

Description

technical field [0001] The invention relates to the technical field of polymers, more specifically, to a preparation method of poly(carbonate-ether) glycol and a preparation method of a catalyst thereof. Background technique [0002] Carbon dioxide is a cheap, easy-to-obtain, non-toxic chemical raw material with abundant reserves. 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. Since the advent of carbon dioxide and epoxy compound copolymers, the catalytic system for catalyzing the copolymerization of carbon dioxide and epoxy compounds to prepare polycarbonates with high molecular weight and high carbonate unit content has made great progress and has been industrialized. Double metal cyanide catalyst (abbreviated as DMC) is a heterogeneous catalyst that is not sensitive to air...

Claims

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Application Information

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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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