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Method for preparing modified PBS copolyester by using camphor alcohol

A copolyester and modification technology, which is applied in the field of preparing modified PBS copolyester with camphor alcohol, can solve the problems of low elongation at break, low glass transition temperature, slow degradation speed, etc., and achieve good thermal stability , easy to operate, and reduce the effect of dependence

Pending Publication Date: 2021-12-17
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, PBS still has some disadvantages, such as glass transition temperature (T g ) low, low elongation at break, slow degradation, etc., which will greatly limit its application in some fields

Method used

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  • Method for preparing modified PBS copolyester by using camphor alcohol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: the preparation of TCDM monomer

[0023] After camphoric acid (10 g) and 156 mL of anhydrous tetrahydrofuran were mixed and dissolved, lithium aluminum tetrahydrogen (5.85 g) was slowly added to the solution under ice-cooling, stirred at room temperature for 4 hours, and then heated to reflux at 70° C. for 0.5 h. Afterwards, water (125 mL) and hydrochloric acid solution (250 mL, 2M) were added successively, extracted with dichloromethane, washed with saturated sodium bicarbonate, and dried over anhydrous magnesium sulfate. Suction filtration and removal of the solvent under reduced pressure gave the crude product. The obtained product was recrystallized with a mixed solvent of dichloromethane and n-hexane to obtain 6 g of pure product with a yield of 72.1%.

Embodiment 2

[0024] Embodiment 2: prepare PTS polyester with TCDM

[0025] Add 4g (23.22mmol) TCDM and 3.08g (21.11mmol) dimethyl succinate to a 100mL airtight there-necked flask to obtain a mixed solution, the molar number of TCDM is 1.1 times that of dimethyl succinate, add catalyst titanic acid Tetrabutyl ester 0.63 mg, slowly inject nitrogen and continue to stir, heat to 130°C, react at this temperature for 4 hours, remove the nitrogen protection, change the vacuum to 0.03-0.06mbar, and continue polycondensation at 240-250°C reaction. After the reaction mixture was cooled to room temperature, 10 mL of chloroform was added to dissolve it, and then methanol was added for precipitation, and the precipitated solid was suction-filtered and fully dried to obtain a copolyester.

Embodiment 3

[0026] Embodiment 3: prepare random PBS copolyester by TCDM, butanediol, dimethyl succinate

[0027] Add 1g (5.80mmol) TCDM, 4.71g (52.24mmol) 1,4-butanediol and 8.48g (58.05mmol) dimethyl succinate into a 100mL airtight three-necked flask to obtain a mixed solution, add catalyst tetrabutyl titanate Esters 0.63 mg, nitrogen was slowly introduced and continued to stir, heated to 130°C, reacted at this temperature for 4 hours, removed the nitrogen protection, changed to vacuum to 0.03-0.06mbar, and continued the polycondensation reaction at 240-250°C. After the reaction mixture was cooled to room temperature, 10 mL of chloroform was added to dissolve it, and then methanol was added for precipitation, and the precipitated solid was suction-filtered and fully dried to obtain a copolyester.

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Abstract

The invention relates to a method for preparing modified PBS copolyester by using (1S, 3R)-(1)-cis-1, 2, 2-trimethylcyclopentane-1, 3-dimethanol (TCDM). PTS polyester, random PBS copolyester and block PBS copolyester are prepared under the conditions of high temperature and high vacuum by using camphoric acid as a raw material and tetrabutyl titanate as a catalyst. The preparation method comprises the following steps: (1) preparing (1S, 3R)-(1)-cis-1, 2, 2-trimethylcyclopentane-1, 3-dimethanol (TCDM) from camphoric acid; 2) preparing PTS polyester from the TCDM; 3) preparing a random PBS copolyester from the TCDM; 4) preparing the block PBS copolyester from PBS and PTS. The method disclosed by the invention has the advantages that the rigid alicyclic diol is extracted from natural camphor and has high reaction activity, rigidity and better thermal stability. Raw materials are wide in source and low in price; the polyester synthesis process is simple, green and environment-friendly, and is beneficial to industrial production; the prepared modified PBS copolyester material is good in thermal stability, structural and functional diversification is easy to realize, and the performance can be comparable with that of polyester based on a petroleum raw material. The polyester material is degradable, does not cause white pollution, and meets the environmental protection requirement.

Description

technical field [0001] The invention relates to the technical field of renewable resource utilization and green synthesis, specifically a (1S,3R)-(1)-cis-1,2,2-trimethylcyclocyanide derived from (D)-camphor A method for preparing modified polybutylene succinate (PBS) copolyester from pentane-1,3-dimethanol (TCDM). Background technique [0002] Polybutylene succinate (PBS), is a bio-based polymer. PBS is considered as a candidate material to replace polyethylene or polypropylene in many fields because of its similar melting point to low-density polyethylene, good mechanical properties, and thermal stability. However, PBS still has some disadvantages, such as glass transition temperature (T g ) low, low elongation at break, slow degradation rate, etc., which will greatly limit its application in certain fields. [0003] The object of the present invention proposes a solution to the above-mentioned problem, uses a kind of novel bio-based monomer (1S, 3R)-(1)-cis-1,2,2-trimet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/199
CPCC08G63/199C08G2230/00
Inventor 庞成才王思予江雪双
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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