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A kind of preparation method of lignin graft copolymer

A technology of graft copolymer and lignin, which is applied in the field of preparing graft copolymers of lignin and styrene monomers, can solve the problem of limiting the applicability, stability and low electrocatalytic activity of lignin graft copolymers , limit the scope of application and other problems, to achieve high graft reaction yield, improve utilization, and reduce the amount of effects

Active Publication Date: 2017-04-05
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese invention patent CN 1148051A discloses a method for preparing graft copolymers of lignin and olefins or substituted olefin monomers by electrochemical methods. Lead oxide, but because gold and platinum electrodes are noble metals, the cost is high, and the stability and electrocatalytic activity of titanium electrodes or ceramic-based lead dioxide-plated electrodes are not high, which limits the scope of application of this method
Invention patent CN 1693342 discloses a method for preparing a graft copolymer with lignosulfonate modified by an esterifying agent and an acrylic monomer. The method obtained is a mixture of a lignin graft copolymer and an acrylate emulsion. Moreover, the ammonia water, emulsifier OP-10, sodium bisulfite, disodium hydrogen phosphate and other inorganic salts added during the grafting reaction, as well as the homopolymer without grafting reaction, etc. are mixed and cannot be separated, which limits The suitability of lignin graft copolymers as adhesives or resins
The invention patent CN 1071436A discloses a method for preparing a graft copolymer by using lignin and vinyl monomers under the action of a redox initiator composed of halide salts and peroxides, although the method prepares woody The yield of plain grafted copolymer is good, but the grafting efficiency is not high

Method used

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  • A kind of preparation method of lignin graft copolymer
  • A kind of preparation method of lignin graft copolymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A. Dissolve 0.2 g of lignin in 5 mL of dimethyl sulfoxide, add 1.0 mL of 0.1 mmol / mL ferrous chloride in methanol and stir to dissolve it, and remove it from the solution through repeated cycles of freezing-vacuumizing-nitrogen 0.5 mL of 30% hydrogen peroxide was added under the protection of nitrogen, and the reaction was stirred for 10 min, then 2.08 g of styrene was added, and at 30 o C stirred the reaction for 48 h. Add 80 mL of dilute hydrochloric acid to dilute, filter, wash with water until neutral, at 40 o C was dried in vacuo to constant weight to obtain a polymer.

[0027] B. After Soxhlet extraction of the above-mentioned polymer with benzene for 12 h, concentrate it at 40 o C dried in vacuum to constant weight to obtain a blend of graft copolymer and homopolymer.

[0028] C. Dissolve the blend of graft copolymer and homopolymer in dichloromethane to prepare a 1 g / mL solution, then add it to 9 times the volume of n-hexane for precipitation, use a mixed sol...

Embodiment 2

[0030] A. Dissolve 0.20 g of lignin in 5 mL of dimethyl sulfoxide, add 0.5 mL of 0.2 mmol / mL of ferrous chloride in methanol and stir to dissolve it, and remove it from the solution through repeated cycles of freezing-vacuumizing-nitrogen 0.5 mL of 30% hydrogen peroxide was added under the protection of nitrogen, and the reaction was stirred for 10 min, then 2.08 g of styrene was added, and at 30 o C stirred and reacted for 60 h. Add 80 mL of dilute hydrochloric acid to dilute, filter, wash with water until neutral, at 40 o C was dried in vacuo to constant weight to obtain a polymer.

[0031] B. The polymer obtained above was extracted by Soxhlet with toluene for 24 h, concentrated, and then extracted at 40 o C dried in vacuum to constant weight to obtain a blend of graft copolymer and homopolymer.

[0032] C. Dissolve the blend of graft copolymer and homopolymer in chloroform to prepare a 1 g / mL solution, then add it to 9 times the volume of n-pentane for precipitation, ...

Embodiment 3

[0034] A. Dissolve 0.20 g of lignin in 5 mL of dimethyl sulfoxide, add 0.5 mL of 0.2 mmol / mL of ferrous chloride in methanol and stir to dissolve it, and remove it from the solution through repeated cycles of freezing-vacuumizing-nitrogen 0.6 mL of 30% hydrogen peroxide was added under the protection of nitrogen, and the reaction was stirred for 10 min, then 2.08 g of styrene was added, and at 30 o C stirred the reaction for 48 h. Add 60 mL of dilute hydrochloric acid to dilute, filter, wash with water until neutral, at 40 o C was dried in vacuo to constant weight to obtain a polymer.

[0035] B. The polymer obtained above was extracted by Soxhlet with toluene for 24 h, then concentrated, and then extracted at 40 o C vacuum drying to constant weight to obtain a blend of graft copolymer and homopolymer.

[0036] C. Dissolve the blend of graft copolymer and homopolymer in ethyl acetate to prepare a 0.8 g / mL solution, then add 10 times the volume of petroleum ether to precip...

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Abstract

The invention relates to a preparation method of a lignin graft copolymer. The method adopts a catalyst and a hydrogen peroxide redox initiator to prepare a graft copolymer of lignin and styrene monomer. The best graft copolymerization yield of this method is 96.6%, the conversion rate of styrene monomer is 96.3%, the grafting rate is 59.5%, and the grafting degree is 53.7%. Lignin graft copolymers can be widely used as thermoplastic macromolecular surface active materials.

Description

technical field [0001] The invention relates to a method for preparing lignin graft copolymer. Specifically, the present invention relates to a method for preparing a graft copolymer of lignin and styrene monomer by using a catalyst and a hydrogen peroxide redox initiator. Background technique [0002] Lignin, as the second most abundant and cheapest renewable resource after cellulose and hemicellulose, accounts for about 30% of all non-fossil resources on Earth. At present, the lignin produced by the paper industry alone in the world has reached 50 million tons per year. Most of this rich renewable resource is used as low-value fuel or directly thrown away as waste, and only 2% is used as a stabilizer. value-added products such as additives, dispersants, binders and surfactants. This not only wastes resources, but also seriously pollutes the environment. Studies have found that graft copolymers of lignin and styrene monomers can be widely used as thermoplastic macromolec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F289/00C08F212/08C08F212/12C08F212/14C08F4/40C08F6/00B01F17/52C09K23/52
Inventor 王来来李海峰
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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