Biomass based polyester preparation method

A technology of biomass-based polyester and polyester, which is applied in the fields of polymer materials and chemical engineering, can solve the problems of water pollution, white pollution, non-renewability, etc., and achieve the effect of avoiding the polymerization process and high quality

Active Publication Date: 2015-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the one hand, because of their good resistance to environmental factors and biological factors, they are durable for a long time; on the other hand, becau

Method used

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  • Biomass based polyester preparation method
  • Biomass based polyester preparation method
  • Biomass based polyester preparation method

Examples

Experimental program
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Embodiment 1

[0017] Example 1: Add 10mmol of 2,5-dimethylolfuran, 15mmol of succinic acid, and 0.1mmol of dibutyltin oxide into a 50mL round bottom flask. Under the protection of nitrogen, it was heated to 180°C; it was reacted at this temperature for 8h. Unreacted monomers and other impurities were then distilled off under reduced pressure. The temperature was raised to 230°C, the vacuum was adjusted to 5mmHg, and the reaction was continued for 3h. Cool to room temperature, add 10ml of chloroform to dissolve, then drop the chloroform solution of polyester into 60ml of methanol for precipitation, centrifuge, decant and remove the supernatant, the obtained polysuccinic acid 2,5-dihydroxy Methyl furyl ester is a milky white solid, dried under vacuum at 50°C for 12h. Calculated according to the feeding amount of the monomer 2,5-dimethylolfuran, the molar yield of the polymer is 90%. NMR spectrogram measurement results and attribution analysis are: 1 H NMR (CDCl 3 -d 1 ,ppm):2.68(4H,-OC-...

Embodiment 2

[0020] Embodiment 2: with 10mmol2,5-dimethylolfuran, 10mmol oxalic acid, 0.01mmolZn(OAc) 2 Added to a 50mL round bottom flask. Under the protection of nitrogen, it was heated to 100°C; it was reacted at this temperature for 2h. Unreacted monomers and other impurities were then distilled off under reduced pressure. Raise the temperature to 250°C, adjust the vacuum to 1.5mmHg, and continue the reaction for 0.5h. Cool to room temperature, add 10ml of dichloroethane to dissolve, then drop the polyester dichloroethane solution into 90ml of methanol for precipitation, centrifuge, decant and remove the supernatant, the obtained polyoxalic acid 2,5-Dihydroxymethylfuryl ester is a milky white solid, dried under vacuum at 50°C for 12h. Calculated according to the feeding amount of monomer 2,5-dimethylolfuran, the molar yield of the polymer is 96%. NMR spectrogram measurement results and attribution analysis are: 1 H NMR (CDCl 3 -d 1,ppm):5.17(4H,-C-CH 2 -O-), 6.34 (2H, furan-H)....

Embodiment 3

[0023] Example 3: 10mmol2,5-dimethylolfuran, 9mmolmalonic acid, 0.001mmolSb 2 (OCH 2 CH 2 O) 3 Added to a 50mL round bottom flask. Under the protection of nitrogen, it was heated to 135°C; the reaction was carried out at this temperature for 0.5h. Unreacted monomers and other impurities were then distilled off under reduced pressure. The temperature was raised to 270°C, the vacuum degree was adjusted to 10mmHg, and the reaction was continued for 10h. Cool to room temperature, add 10ml of chloroform to dissolve, then drop the chloroform solution of polyester into 80ml of methanol for precipitation, centrifuge, decant and remove the supernatant to obtain polymalonic acid 2,5-dimethylol The furyl ester was a milky white solid, which was dried under vacuum at 50°C for 12h. Calculated according to the feeding amount of the monomer 2,5-dimethylolfuran, the molar yield of the polymer is 98%. NMR spectrogram measurement results and attribution analysis are: 1 H NMR (CDCl 3 -d...

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Abstract

A biomass based polyester preparation method is as follows: biomass based monomer 2, 5-dihydroxy methyl furan and a dibasic acid are used as raw materials for esterification prepolymerization for reaction for 0.5-10h in the presence of a catalyst at 90-300 DEG C under the protection of nitrogen; ester exchange condensation is performed at 150-350 DEG C under the condition of 1-10mmHg vacuum, and the reaction is performed for 0.1-15h; a dissolution-precipitation method is used for purification and removing of impurities and unreacted monomers and oligomers to obtain the biomass based polyester product. The biomass based polyester product prepared by the preparation method is high in yield, easy in product separation, and environmental friendly, and has good application prospects.

Description

technical field [0001] The invention relates to the fields of polymer materials and chemical engineering, in particular to a method for preparing biomass-based polyester through esterification and transesterification condensation reaction of 2,5-dimethylolfuran and dibasic acid under catalysis. Background technique [0002] The excessive dependence of polymer materials such as plastics, chemical fibers, and polyesters on fossil resources such as petroleum, and the impact on the environment caused by their difficulty in degrading during use, make it urgent to find new, renewable and clean resources. Biomass is not only a carrier for efficient storage of solar energy, but also a renewable organic carbon resource. Using catalytic technology to efficiently convert organic carbon in renewable biomass into chemicals and polymer materials is one of the important ways to alleviate and supplement the shortage of petroleum resources, and has important scientific significance and appli...

Claims

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Application Information

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IPC IPC(8): C08G63/672C08G63/78
Inventor 马继平徐杰杨艳良贾秀全王敏石松高进
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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