Preparation method of cellulose-g-resin acid grafted copolymer

A technology of graft copolymer and resin acid, which is applied in the field of preparation of cellulose-g-resin acid graft copolymer, can solve the problems of easy destruction of cellulose skeleton, application limitation, uncontrollable molecular weight and molecular weight distribution, etc.

Inactive Publication Date: 2013-06-12
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Abstract
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Problems solved by technology

[0004] Graft copolymerization is a commonly used method for chemical modification of cellulose. At present, it is mainly through chemical method (cerium ion initiation), ultraviolet radiation, gamma ray and plasma radiation, etc. The method initiates the generation of free radicals on the cellulose macromolecular chain, and then carries out the graft copolymerization reaction, but this method is easy to destroy the cellulose skeleton, and its application is limited
On the other hand, the molecular weight and molecular weight distribution of side chains grafted by free radical polymerization are not controllable

Method used

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  • Preparation method of cellulose-g-resin acid grafted copolymer

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preparation example Construction

[0032] A kind of preparation method of cellulose-g-resin acid graft copolymer, the steps are:

[0033] (1) Reaction of cellulose with 2-bromoisobutyryl bromide in a homogeneous solution system to synthesize a cellulose atom transfer radical polymerization (ATRP) macroinitiator; (2) Resin acid-based monomer, cellulose ATRP Macromolecular initiators, catalysts and ligands are added to the reaction flask with a certain molar ratio and solvent, fully stirred and dissolved, and the oxygen in the mixed solution is removed through three (freezing-vacuum-nitrogen) cycle processes. o After reacting in C for 1-24 h, the polymer was precipitated in methanol, then filtered and dried to obtain the cellulose-g-resin acid graft copolymer. Cellulose-g-resin acid graft copolymers with different molecular weights and molecular weight distributions can be obtained by this method.

[0034] Cellulose is microcrystalline cellulose with low crystallinity;

[0035] The homogeneous solution syste...

Embodiment 1

[0046] (1) Cellulose pretreatment

[0047] First, put 2.0g of microcrystalline cellulose in a vacuum drying oven, and dry it under vacuum at 110°C for 24 hours to remove residual small molecule impurities in the microcrystalline cellulose, and then disperse the pre-dried microcrystalline cellulose into 100ml of distilled water Water activation treatment, after stirring for 30 minutes, filter to remove water, and repeat the water activation treatment three times; the dehydrated microcrystalline cellulose is then dispersed in 100ml methanol for methanol activation treatment, after stirring for 30 minutes, filter and remove water, and the methanol activation treatment is repeated three times; Finally, the microcrystalline cellulose was dried in a vacuum oven at 50° C. for 3 hours to complete the cellulose pretreatment.

[0048] (2) Preparation of cellulose homogeneous solution

[0049] Dissolve 2.0 g of the above-mentioned pretreated cellulose in 120 ml of dimethylacetamide, h...

Embodiment 2

[0057] [Monomer] / [Initiator] / [Catalyst] / [Ligand]=100:1:2:1 (molar ratio)

[0058] The cellulose macroinitiator (prepared in Example 1) 2.65mg (0.0125mmol Br), the ligand N,N,N,N,N-pentamethyldiethylenetriamine (PMDETA) 2.6μL (0.0125 mmol), monomer (DAME) 0.515 g (1.25 mmol) was dissolved in 2 mL tetrahydrofuran (THF), and the oxygen in the mixed solution was removed through three cycles (freezing-vacuumizing-nitrogen filling). At the same time, 4.25mg Cu(I)Br (2.5mmol) was weighed into the polymerization bottle, filled with nitrogen and deoxygenated, then the mixed solution was transferred to the polymerization bottle, and put into 80 o C in an oil bath for 12 hours. After the reaction, the reactant was passed through a neutral aluminum oxide column to remove the copper catalyst, dropped into a large amount of methanol for precipitation, filtered to collect the precipitate, and finally dried in a vacuum oven at room temperature for 24 hours. The monomer conversion rate is 35...

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Abstract

The invention relates to a preparation method of cellulose-g-resin acid grafted copolymer. The preparation method of the cellulose-g-resin acid grafted copolymer comprises the steps that cellulose atom transfer radical polymerization (ATRP) macroinitiator is synthesized by reaction of cellulose and 2-Bromoisobutyryl bromide in a homogeneous solution system; resin acid monomer, cellulose ATRA macroinitiator, catalytic agents, ligand and rosinyl monomer good solvent are added to a reaction bulb, fully stirred, and dissolved, freezing is carried out for three times, oxygen in the mixed solution is removed in a circulation process of vacuum pumping and nitrogen filling, after the reaction is carried out for 1-24 hours at the temperature of 50-120 DEG C, the polymer is enabled to be deposited in methanol, filtered, and dried, and finally the cellulose-g-resin acid grafted copolymer is obtained. According to the preparation method of the cellulose-g-resin acid grafted copolymer, cellulose-g-resin acid grafted copolymer with different molecular weights and different molecular weight distributions can be obtained. The cellulose-g-resin acid grafted copolymer can be used for improving tenacity of materials by serving as functional additive agents.

Description

technical field [0001] The invention relates to a preparation method of a cellulose-g-resin acid graft copolymer, in particular to a compound method of a natural compound and a natural polymer. [0002] Background technique [0003] Cellulose is the most abundant and oldest natural polymer in the world, and it is the main component of plant skeleton. The annual cellulose content produced by plants on the earth is about 1.5×10 12 Ton, it has the advantages of wide source, degradable, non-toxic, good biocompatibility, etc., and has a good application prospect in the field of new materials. The molecular formula of cellulose macromolecule is: (C 6 h 10 o 5 ) n , is a macromolecular polysaccharide composed of D-glucose with β-1,4 glycosidic bonds, with a molecular weight of about 50,000 to 2,500,000. There are three polar hydroxyl groups in each glucose unit in the cellulose macromolecule, and there are no branches in the main chain of the macromolecule. The phenomenon o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F251/02
Inventor 储富祥王基夫俞娟王春鹏唐传兵
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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