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Process for synthesizing aliphatic polycarbonate

A polycarbonate and synthesis method technology, applied in the field of chemical synthesis, can solve problems such as low catalytic efficiency and difficulty in realizing carbon dioxide copolymerization, achieve high catalytic activity, and expand the effect of application fields

Inactive Publication Date: 2009-05-27
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although Chen Shang has made good progress in the application of double metal cyanide catalysts in the copolymerization of carbon dioxide, they can only be applied to the copolymerization of carbon dioxide and propylene oxide, carbon dioxide and cyclohexene oxide. The catalytic efficiency is still low, only 200

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  • Process for synthesizing aliphatic polycarbonate
  • Process for synthesizing aliphatic polycarbonate
  • Process for synthesizing aliphatic polycarbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Dissolve 0.01 mol of potassium hexacyanocobaltate in 50 mL of water, and dissolve 0.3 mol of zinc chloride in a mixture of 150 mL of water and 50 mL of tert-butanol. Under vigorous stirring, slowly drop the potassium hexacyanocobaltate solution into the zinc chloride solution at 20°C, and continue to stir vigorously after the precipitate is formed to fully complex the ligand tert-butanol with the precipitate. After centrifugation to separate the precipitate, the resulting precipitate is re-slurried with a mixture of tert-butanol and water in a volume ratio of 1:3, and the centrifugation and slurry-washing are repeated several times to gradually increase the volume ratio of tert-butanol / water to 3:1. Finally, potassium ions can not be detected in the centrifugal liquid with potassium reagent. The precipitate was dried in a vacuum oven at 20°C for 100 hours to obtain a Zn / Co double metal cyanide catalyst, the structural formula of which is (Zn) 2.82[Co(CN) 7.38 ]Cl 0.49 L 1.3...

Embodiment 2

[0030] Dissolve 0.01 mol of potassium hexacyanoferrate in 50 mL of water, and dissolve 0.5 mol of zinc oxide and zinc chloride in a mixture of 150 mL of water and 150 mL of tert-butanol. Under vigorous stirring, slowly drip the potassium hexacyanoferrate solution into the mixed solution of zinc oxide and zinc chloride at 30°C, and continue to vigorously stir after the precipitate is formed to fully complex the ligand tert-butanol with the precipitate. Afterwards, the precipitate was separated by filtration, and the resulting precipitate was re-slurried with a mixture of tert-butanol and water in a volume ratio of 1:3. Repeated centrifugation and slurried washing several times, and successively increased the ratio of tert-butanol / water in the washing liquid to 3:1 . Finally, potassium ions can not be detected in the centrifugal liquid with potassium reagent. The precipitate was dried in a vacuum oven at 50°C for 45 hours to obtain a Zn / Fe double metal cyanide catalyst, the structur...

Embodiment 3

[0033] Dissolve 0.01 mol potassium tetracyano nickelate in 50 mL of water, and dissolve a 1:1 mixture of 0.05 mol of zinc hydroxide and zinc chloride in a mixture of 50 mL of water and 150 mL of glyme. Under vigorous stirring, slowly drip the potassium tetracyano nickelate solution into the mixture solution of zinc hydroxide and zinc chloride at a molar ratio of 1:1 at 50°C. After the precipitate is formed, continue to vigorously stir to make the ligand glyme and The precipitate is fully complexed. Afterwards, the precipitate was separated by filtration, and the obtained precipitate was re-slurried with a mixture of 1:3 glyme and water, centrifuged and washed for several times, and the ratio of glyme / water in the washing solution was increased to 3: 1. Finally, potassium ions can not be detected in the centrifugal liquid with potassium reagent. The precipitate was dried in a vacuum oven at 40°C for 10 hours to obtain a Zn / Ni double metal cyanide catalyst. Its structural formula is...

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Abstract

The invention discloses a method for synthesizing aliphatic polycarbonate. The method comprises the following steps of putting double metal cyanide catalyst, carbon dioxide and epoxide into a high-pressure reactor, well mixing and heating the materials for catalytic reaction and obtaining a copolymer, wherein the apparent crystallinity of the double metal cyanide, which is obtained by use of X-ray powder diffraction characterization, is more than or equal to 70 percent. The high-crystallinity double metal cyanide catalyst used in the method has higher catalytic activity in the reaction of the carbon dioxide and propylene oxide, thereby overcoming the technical bias that the catalytic activity of crystalline-state double metal cyanide is generally considered to be lower than that of amorphous double metal cyanide in the field.

Description

Technical field [0001] The present invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing medium and high molecular weight aliphatic polycarbonate with carbon dioxide and epoxide using double metal cyanide as a catalyst. Background technique [0002] Double metal cyanide is a universal epoxide homopolymerization catalyst. Its synthesis is generally obtained by reacting metal salt and metal cyanide salt in an aqueous solution, plus organic ligands. Its synthesis technology has been described in JP4145123, US5470813 , EP700949, WO 97 / 40086 and CN1255074 and other patent documents. By changing the types of metal and organic ligands, the current double metal cyanide used in the homopolymerization of epoxides can achieve quite high catalytic activity. However, it is generally believed that only low crystalline or even amorphous double metal cyanide can achieve better catalytic effects, and the crystallinity is characterized by whethe...

Claims

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Application Information

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IPC IPC(8): C08G64/34C08G64/02
Inventor 张敏邹志强陈立班
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI