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Method for catalyzed synthesis of hemicellulose grafted polylactic acid through organic alkali in ionic liquid

A hemicellulose and ionic liquid technology, applied in the field of biomass organic synthesis, can solve the problems of low grafting efficiency, reduced reaction efficiency, energy waste, etc., and achieve the effects of high product substitution, low reaction energy consumption, and improved performance

Inactive Publication Date: 2016-05-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the grafting efficiency is low, the high temperature reaction conditions cause energy waste and the transesterification reaction is prone to occur during the grafting process, which reduces the reaction efficiency, and the metal catalyst is not easy to completely remove, which affects the application of the product in biology, medicine and electronic products.

Method used

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  • Method for catalyzed synthesis of hemicellulose grafted polylactic acid through organic alkali in ionic liquid

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Embodiment 1

[0024] The method for synthesizing hemicellulose-grafted polylactic acid catalyzed by an organic base in a kind of ionic liquid of the present embodiment, the specific synthetic route is as follows:

[0025] (1) Under nitrogen protection, add hemicellulose (xylan mass percentage ≥ 55%) into the ionic liquid 1-allyl-3-methylimidazole chloride, dissolve at 80°C for 30 minutes to obtain hemicellulose prime solution; the mass volume ratio of hemicellulose to ionic liquid is 1:30 (g / mL); the ionic liquid is vacuum-dried at 70°C and 0.1MPa for 72h before use;

[0026] (2) Under nitrogen protection, L-lactide monomer and organic base catalyst 1,8-diazabicycloundec-7-ene are added to the hemicellulose solution in step (1), so that L -Lactide monomer undergoes ring-opening graft copolymerization reaction with hemicellulose under the action of an organic base catalyst; the reaction temperature is controlled at 50°C, and the reaction time is 12h; L-lactide monomer and hemicellulose anhyd...

Embodiment 2

[0030] The method for synthesizing hemicellulose-grafted polylactic acid catalyzed by an organic base in a kind of ionic liquid of the present embodiment, the specific synthetic route is as follows:

[0031] (1) Under nitrogen protection, add hemicellulose (xylan mass percentage ≥ 55%) into ionic liquid 1-butyl-3-methylimidazole chloride, dissolve at 80°C for 30 minutes to obtain hemicellulose Solution; the mass volume ratio of hemicellulose to ionic liquid is 1:60 (g / mL); the ionic liquid is dried at 110°C under normal pressure for 12h before use;

[0032] (2) Under nitrogen protection, L-lactide monomer and organic base catalyst 4-dimethylaminopyridine are added in the hemicellulose solution of step (1), make L-lactide monomer react in the organic base catalyst Ring-opening graft copolymerization reaction occurs with hemicellulose under the action of hemicellulose; the reaction temperature is controlled at 80°C, and the reaction time is 24h; the molar ratio of L-lactide mono...

Embodiment 3

[0036] The method for synthesizing hemicellulose-grafted polylactic acid catalyzed by an organic base in a kind of ionic liquid of the present embodiment, the specific synthetic route is as follows:

[0037] (1) Under nitrogen protection, add hemicellulose (xylan mass percentage ≥ 55%) into the ionic liquid 1-hexyl-3-methylimidazole chloride, dissolve at 80°C for 30 minutes to obtain a hemicellulose solution The mass volume ratio of hemicellulose to ionic liquid is 1:10 (g / mL); the ionic liquid is freeze-dried at -40°C for 36h before use;

[0038] (2) Under nitrogen protection, L-lactide monomer and organic base catalyst 1,5,7-triazabicyclo[4.4.0]dec-5-ene are added to the hemicellulose in step (1) In the solution, the ring-opening graft copolymerization reaction of L-lactide monomer and hemicellulose occurs under the action of an organic base catalyst; the reaction temperature is controlled at 130°C, and the reaction time is 6h; the L-lactide monomer and The molar ratio of h...

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Abstract

The invention belongs to the technical field of biomass organic synthesis and discloses a method for catalyzed synthesis of hemicellulose grafted polylactic acid through organic alkali in ionic liquid. The synthesis method includes the steps that hemicellulose is added into the ionic liquid, a hemicellulose solution is obtained after dissolution, then L-lactide monomers and an organic alkali catalyst are added, and reaction is performed for 3-48 h at the temperature of 20-150 DEG C; after the reaction ends, a quenching agent is added for a quenching reaction, after dialysis, reaction liquid is frozen and dried, obtained solid is washed and dried, and the hemicellulose grafted polylactic acid is obtained. According to the method, the hemicellulose serves as raw materials, the ionic liquid serves as reaction media, the organic alkali serves as the catalyst, the advantages of environmental friendliness, high efficiency, easy operation, low reaction energy consumption and high product substitution degree are achieved, and the obtained product can be applied to the fields of biology, food, agriculture and the like.

Description

technical field [0001] The invention belongs to the technical field of biomass organic synthesis, and in particular relates to a method for synthesizing hemicellulose-grafted polylactic acid catalyzed by an organic base in an ionic liquid. Background technique [0002] With the increasing shortage of non-renewable resources such as oil and the aggravation of environmental problems, it has become an urgent problem to find green and renewable energy to replace traditional energy. Lignocellulosic biomass has the advantages of wide sources, large reserves, renewable, short regeneration cycle, and biodegradability, and has gradually attracted people's attention. It plays a pivotal role in the fields of agriculture, biology, medicine, and chemical industry. As one of the three major components of lignocellulosic biomass, hemicellulose has been neglected due to its disadvantages such as heterogeneous structure, low molecular weight, low degree of polymerization, and strong hydrophi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08G63/81C08B37/14
CPCC08G63/08C08B37/14C08G63/81
Inventor 刘传富张雪琴孙润仓
Owner SOUTH CHINA UNIV OF TECH
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