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Method of preparing transparent ultraviolet absorption membrane material from enzymatic hydrolysis lignin

A technology of enzymatically decomposing lignin and external absorption, which is applied in the field of membrane materials, can solve the problems of membrane loss of transparency and limit the scope of application, and achieve the effect of excellent hardness and high transparency

Inactive Publication Date: 2015-06-10
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

UV-absorbing film materials can be obtained by blending lignin with matrix resin, but this method will cause the film to lose its transparency, which greatly limits its scope of application

Method used

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  • Method of preparing transparent ultraviolet absorption membrane material from enzymatic hydrolysis lignin
  • Method of preparing transparent ultraviolet absorption membrane material from enzymatic hydrolysis lignin
  • Method of preparing transparent ultraviolet absorption membrane material from enzymatic hydrolysis lignin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) In a dry 250mL four-neck flask, add 6.0g LiCl and 98.0g DMAc (dimethylacetamide), and then add 3.0g of dry enzymatic lignin (Songyuan Bairui Biopolyol Co., Ltd.), Stir and dissolve at 70°C to a homogeneous solution; add catalyst triethylamine 1.2g and polymerization inhibitor hydroquinone 0.0450g to the above homogeneous system, and pass nitrogen protection at the same time; add acryloyl chloride 2.4g to the above solution, 50°C React for 3 hours; when the reaction is complete, pour the reaction solution into 1000 mL of distilled water, stir and centrifuge to collect the precipitate, wash with water several times until neutral, and dry at 50°C to constant weight to obtain a lignin-based macromer.

[0023] (2) Add 0.6g of lignin-based macromer, 4g of butyl methacrylate and 92mg of AIBN (azobisisobutylcyanide) into 30 mL of dioxane, and transfer the solvent to a 100mL eggplant-shaped reaction bottle During the process, nitrogen bubbles were used to remove oxygen for 1...

Embodiment 2

[0025] (1) In a dry 250mL four-neck flask, add 8.0g LiCl and 98.0g DMAc, then add 3.0g of dry enzymatic lignin (Songyuan Bairui Biopolyol Co., Ltd.), stir and dissolve at 70°C until homogeneous solution; add catalyst triethylamine 1.2g and polymerization inhibitor hydroquinone 0.0450g to the above homogeneous system, and pass through nitrogen protection at the same time; add acryloyl chloride 2.4g to the above solution, and react at 50°C for 3h; The reaction solution was poured into 1000 mL of distilled water, stirred and centrifuged to collect the precipitate, washed with water several times until neutral, and dried at 50°C to constant weight to obtain a lignin-based macromer.

[0026] (2) Add 0.6g of lignin-based macromer, 3g of butyl methacrylate and 72mg of AIBN (azobisisobutylcyanide) into 30mL of tetrahydrofuran, transfer the solvent to a 100mL eggplant-type reaction flask, blow with nitrogen Soak for deoxygenation for 10 minutes. Then heat up to 70°C and react for 10 h...

Embodiment 3

[0028] (1) In a dry 250mL four-neck flask, add 2.0g LiCl and 98.0g DMAc, then add 3.0g of dry enzymatic lignin, stir at 20°C for 5h to dissolve into a homogeneous solution; add catalyst to the above homogeneous system Triethylamine 1.2g and polymerization inhibitor hydroquinone 0.0450g, nitrogen protection at the same time; add acryloyl chloride 2.4g to the above solution, and react at 40°C for 5h; after the reaction, pour the reaction solution into 1000mL distilled water, stir and centrifuge The precipitate was collected, washed with water several times until neutral, and dried at 50°C to constant weight to obtain a lignin-based macromer.

[0029] (2) Add 0.6g of lignin-based macromer, 2.4g of butyl methacrylate and 60mg of AIBN (azobisisobutylcyanide) into 30mL of tetrahydrofuran, transfer the solvent to a 100mL eggplant type reaction flask, and nitrogen Deoxygenate by bubbling for 10 minutes. Then heat up to 70°C and react for 10 hours to obtain a polymer. The conversion r...

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Abstract

The invention relates to a method of preparing a transparent ultraviolet absorption membrane material from enzymatic hydrolysis lignin. The method comprises the following steps: subjecting lignin to graft modification so as to obtain a lignin-based macro-monomer; dissolving the lignin-based macro-monomer, an acrylic acid monomer and an initiator for free radical polymerization in an organic solvent, introducing nitrogen to remove oxygen and carrying out a reaction at a temperature of 50 to 100 DEG C for 6 to 24 h; and subjecting a polymer to precipitation in n-hexane with a temperature of 30 to 60 DEG C and carrying out filtering and drying so as to obtain the ultraviolet absorption membrane material. According to the invention, a lignin aromatic ring structure is genuinely introduced into a polymer structure, and the synthesized polymer lignin-based membrane material has the advantages of high transparency, excellent hardness, thermal stability and ultraviolet light absorption performance and can be widely applied in fields like functional uvioresistant paints.

Description

technical field [0001] The invention belongs to the technical field of membrane materials, and in particular relates to a method for preparing a transparent ultraviolet-absorbing membrane material by enzymatically decomposing lignin. Background technique [0002] With the continuous digestion of petroleum and coal resources and the increasing environmental problems, scientists around the world are researching and developing low-cost biomass-based polymerizable monomers to replace ethylene, styrene, vinyl acetate, acrylate and butadiene, etc. Petrochemical monomers to prepare bio-based polymer materials. Lignin is a natural polymer second only to cellulose on the earth, and it is cheap, degradable, and non-polluting. Therefore, all countries in the world attach great importance to the research and development of lignin-based materials. [0003] The main means of obtaining lignin is separation from by-products of chemical pulping and biomass refining by various methods. In o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F289/00C08F220/18C08F220/14C08L51/00
Inventor 储富祥刘晓欢王春鹏王基夫
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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