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Copolymer of furan glycidyl ether or ester and carbon dioxide, and preparation thereof

A technology of glycidyl ether and glycidyl ester, which is applied in the field of copolymers of furan glycidyl ether or ester and carbon dioxide, can solve the problems of unseen polymer materials and achieve favorable effects for utilization

Active Publication Date: 2011-06-08
迁安市宏奥低碳科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there are no patents and literature reports about using furan glycidyl ethers or esters and carbon dioxide as raw materials to synthesize polymer materials

Method used

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  • Copolymer of furan glycidyl ether or ester and carbon dioxide, and preparation thereof
  • Copolymer of furan glycidyl ether or ester and carbon dioxide, and preparation thereof
  • Copolymer of furan glycidyl ether or ester and carbon dioxide, and preparation thereof

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Experimental program
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Effect test

preparation Embodiment 1

[0034] at a purity of 99.99% N 2 Add 0.000977mol Y(CCl 3 COO) 3 , 40ml 1,3-dioxapentane and 0.00977mol glycerol, to be Y (CCl 3 COO) 3 After all dissolved, slowly add 0.01954mol ZnEt dropwise to the preparation bottle 2 , ZnEt 2 It is advisable to control the reaction temperature at 35-45°C for the dropping speed. ZnEt 2 After the dropwise addition, after no gas is released, place the preparation bottle in a constant temperature bath for aging. The aging conditions are: the temperature of the constant temperature bath is 60°C; the frequency of mechanical oscillation is 150 times / min; the amplitude is 40mm; A total of 2 hours was carried out to obtain a white suspension liquid which was a rare earth three-way catalyst.

preparation Embodiment 2

[0036] The synthesis of furyl methyl glycidyl ether, in the there-necked flask equipped with electric stirrer, thermometer and constant pressure dropping funnel, add 7.6mol epichlorohydrin, 800mL sodium hydroxide solution (50%w / w), and 0.076mol tetra-tert-butylammonium bisulfate, and then 3.8mol of purified furanmethanol was dropped into the above-mentioned three-necked flask at a rate of 6mL / min under a constant pressure dropping funnel under strong stirring at 400rpm, and the temperature of the control system did not exceed 20°C , After reacting for 4 hours, the reaction solution was washed with distilled water until neutral, and the obtained organic phase was dried for 24 hours with 60 g of anhydrous magnesium sulfate, and the dried organic phase was filtered to remove anhydrous magnesium sulfate. The obtained organic phase was distilled off under reduced pressure (2.0KPa) to remove unreacted epichlorohydrin to obtain furyl methyl glycidyl ether crude product. The crude pro...

preparation Embodiment 3

[0038] Synthesis of Glycidyl Tetrahydrofurancarboxylate

[0039] 1) Synthesis of sodium tetrahydrofuran formate, 1.0 mol of sodium hydroxide and 40 ml of distilled water were added to a three-necked flask, then 1.1 mol of tetrahydrofuran formic acid and 80 mL of ethanol (99.5% in purity) were mixed with 6 mL of tetrahydrofuran formic acid through a constant pressure dropping funnel under vigorous stirring at 450 rpm. Drop into the above-mentioned three-necked flask at a rate of 1 / min, control the system temperature at 25°C, and react for 4 hours, distill off ethanol and water, wash with acetone 3 times, each time with 100mL, and vacuum dry at 70°C to constant weight. Sodium tetrahydrofuran formate was obtained.

[0040] 2) Synthesis of glycidyl tetrahydrofuran formate Add 1.0 mol sodium tetrahydrofuran formate, 5.0 mol epichlorohydrin, and 0.015 mol tetra-tert-butyl ammonium bisulfate to a three-necked flask equipped with a spherical condenser, heat with an oil bath, and contr...

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Abstract

The present invention provides a copolymer of furan-type glycidol ether or furan-type glycidyl ester and carbon dioxide, and a preparation method thereof. The copolymer is prepared by polymerizing the furan-type glycidol ether or furan-type glycidyl ester with the carbon dioxide under the action of a rare-earth three-way catalyst, wherein the furan-type glycidol ether is furan methyl glycidol ether, 5-methylfuran methyl glycidol ether or tetrahydrofuran methyl glycidol ether, and the furan-type glycidyl ester is furan formic-acid glycidyl ester, 5-methylfuran formic-acid glycidyl ester or tetrahydrofuran formic-acid glycidyl ester. The highest polymerization yield of the copolymer is 1.854*10<3> grams of polymer per mol of Zn; the number average molecular weight of the copolymer is 16.6*10<4> g / mol; the glass transition temperature of the copolymer is 8.7 DEG C below zero; and the initial thermal decomposition temperature of the copolymer is 272 DEG C.

Description

technical field [0001] The invention belongs to a copolymer of furan glycidyl ether or ester and carbon dioxide and its preparation method Background technique [0002] With the decrease of petroleum resources, reducing the dependence of polymer materials on petroleum resources has become an important research topic for polymer scientists in various countries. In the early 1990s, French scientist Gandini A and others synthesized high polymer polyfuryl ether (Polym. commun., 31, 210-212, 1990; Polymer, 37 (21), 4815-4821, 1996; Polym.J., 29(6), 479-486, 1997), and then comprehensively expounded the importance of furan compounds in polymer synthesis under the title of "Furan in Polymer Chemistry", (Prog. Polym.Sci., 22, 1203-1379, 1997), in 2004, introduced the progress of substituted furan chemistry and related polymerization (Topics in catalysis, 27(1-4), 11-29, 2004). At the end of the 1960s, Professor Inoue Shohei successfully synthesized carbon dioxide and epoxide copol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/02C08G64/34
Inventor 乔立军候继强魏军王献红赵晓江王佛松
Owner 迁安市宏奥低碳科技有限公司