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A kind of preparation method of butyl rubber/polylactic acid graft polymer

A technology of butyl rubber and graft copolymer, applied in the preparation of butyl rubber/polylactic acid graft polymer and the preparation of modified polylactic acid, can solve the problems of brittle fracture of polylactic acid and difficulty in forming polylactic acid film, etc. , to achieve good chain flexibility, improved toughness and processability, and good thermal stability.

Active Publication Date: 2021-05-14
ZHEJIANG CENWAY MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, rubber molecules and lactide are grafted and copolymerized to form butyl rubber / polylactic acid graft polymer, which effectively solves the existing technology that polylactic acid is prone to brittle fracture when stretched and difficult to form polylactic acid film. defect; and the butyl rubber / polylactic acid graft polymer prepared by the inventive method also has good thermal stability

Method used

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  • A kind of preparation method of butyl rubber/polylactic acid graft polymer
  • A kind of preparation method of butyl rubber/polylactic acid graft polymer
  • A kind of preparation method of butyl rubber/polylactic acid graft polymer

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Effect test

Embodiment 1

[0031] Such as figure 1 Shown, a kind of preparation method of butyl rubber / polylactic acid graft polymer comprises the following steps:

[0032] a. Take 10 g of butyl rubber with an unsaturation of 0.5% (0.89 mmol of isoprene unit, number average molecular weight of 239,000, molecular weight distribution of 2.02), completely dissolve in 800 ml of toluene, and keep the temperature at 30 o C, under stirring, add m-chloroperoxybenzoic acid toluene solution (8.9mmol, 100ml), the reaction time is 6 hours, the product is precipitated with a large amount of ethanol and dried in vacuum, and dried to obtain epoxidized butyl rubber; epoxy rate> 99 %. The epoxy butyl rubber yield is 95%.

[0033] b. Dissolve 5g epoxy butyl rubber (0.4 mmol epoxy group) completely in 150ml toluene, add 0.2ml 37% concentrated hydrochloric acid, react at room temperature for 6 hours, add a large amount of deionized water to wash, and vacuum dry to obtain hydroxyl Butyl rubber; the conversion rate of epo...

Embodiment 2

[0039] Such as figure 1 Shown, a kind of preparation method of butyl rubber / polylactic acid graft polymer comprises the following steps:

[0040] a. Take 10 g of butyl rubber with an unsaturation of 1% (1.78 mmol of isoprene units, number average molecular weight of 252,000, molecular weight distribution of 2.12), completely dissolve in 600 ml of toluene, and keep the temperature at 30 o C, under stirring, add m-chloroperoxybenzoic acid toluene solution (17.8mmol, 200ml), the reaction time is 3 hours, the product is precipitated with a large amount of ethanol and dried in vacuum, and dried to obtain epoxidized butyl rubber; epoxy rate> 99 %.

[0041] b. Dissolve 5g epoxy butyl rubber (0.85 mmol epoxy group) completely in 150ml toluene, add 0.4 ml 37% concentrated hydrochloric acid, react at room temperature for 6 hours, add a large amount of deionized water to wash, and vacuum dry to obtain hydroxyl Butyl rubber; the conversion rate of epoxy group to hydroxyl group is 80%.

...

Embodiment 3

[0044] Such as figure 1 Shown, a kind of preparation method of butyl rubber / polylactic acid graft polymer comprises the following steps:

[0045] a. Take 10 g of butyl rubber with an unsaturation degree of 1.5% (2.7 mmol of isoprene units, number average molecular weight of 239,000, molecular weight distribution of 2.21), completely dissolve in 1000 ml of toluene, and keep the temperature at 30 o C, under stirring, add m-chloroperoxybenzoic acid toluene solution (27 mmol, 200ml), the reaction time is 2 hours, the product is precipitated with a large amount of ethanol and dried in vacuo, and dried to obtain epoxidized butyl rubber; epoxy rate> 99 %.

[0046] b. Completely dissolve 5g epoxy butyl rubber (1.3mmol epoxy group) in 600ml toluene, add 0.6ml 37% concentrated hydrochloric acid, react at room temperature for 1 hour, add a large amount of deionized water to wash, and vacuum dry to obtain Hydroxylated butyl rubber; 99% conversion of epoxy groups to hydroxyl groups.

[...

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Abstract

The invention relates to a preparation method of a butyl rubber / polylactic acid graft polymer, belonging to the technical field of modified polylactic acid. The method comprises the following steps: a, preparing a butyl rubber solution; b, adding an epoxidizing agent to the butyl rubber solution to generate an epoxidized butyl rubber; c, preparing an epoxidized butyl rubber into an epoxidized butyl rubber base rubber solution, add acidic ring-opening reagent to generate hydroxylated butyl rubber; d, prepare hydroxylated butyl rubber into hydroxylated butyl rubber solution, add lactide and polymerization catalyst under the protection of inert atmosphere to generate butyl Graft copolymer of base rubber and polylactic acid. The macromolecular graft polymer of butyl rubber grafted polylactic acid prepared by the present invention has good thermal stability and chain flexibility in the main chain of butyl rubber, which improves the toughness and processability of polylactic acid. The grafted polymer is expected to be widely used in food preservation film, 3D printing materials and other fields.

Description

technical field [0001] The invention relates to a preparation method of modified polylactic acid, in particular to a preparation method of butyl rubber / polylactic acid graft polymer, and belongs to the technical field of modified polylactic acid. Background technique [0002] Polylactic acid is a new type of biodegradable biomaterial with high strength and good biocompatibility. It can be processed by blow molding, injection molding and other methods, and the processing is simple. However, the shortcomings of polylactic acid, such as brittleness, poor toughness, and low heat distortion temperature, limit the application of polylactic acid in many fields. [0003] The Chinese invention patent application with the application number CN 201910831884.8 discloses a method for preparing a linear comb-shaped fluorescent polylactic acid. The method first uses active anion reactions to prepare linear liquid polybutadiene, and then synthesizes linear polybutadiene through ring-opening...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/00
CPCC08G63/00C08G63/08
Inventor 贾翔宇任纪文张学琪翟路路付翁孙清李付姣文川叶媛园张阳
Owner ZHEJIANG CENWAY MATERIALS CO LTD
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