Lignin-based starlike thermoplastic elastomer and preparation method thereof

A thermoplastic elastomer, lignin-based technology, applied in the field of star polymers of natural compounds, which can solve the problems of chemical modification of lignin, poor structural compatibility, limitations, etc.

Inactive Publication Date: 2015-02-18
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

At present, there are two main types of utilization of lignin resources, one is to blend lignin with traditional petroleum-based products as composite materials, but such materials are generally limited due to poor structural compatibility; the other is Chemical Modification of Lignin

Method used

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  • Lignin-based starlike thermoplastic elastomer and preparation method thereof
  • Lignin-based starlike thermoplastic elastomer and preparation method thereof
  • Lignin-based starlike thermoplastic elastomer and preparation method thereof

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preparation example Construction

[0029] A preparation method of a lignin-based star-shaped thermoplastic elastomer polymer, the steps: (1) react lignin with 2-bromoisobutyryl bromide to synthesize a lignin ATRP macroinitiator; (2) synthesize a hard monomer (such as methyl methacrylate), soft monomer (such as butyl acrylate), lignin ATRP macromolecular initiator, catalyst and ligand, and good reaction solvent are added to the reaction bottle, fully stirred and dissolved, and frozen and pumped three times The oxygen in the mixed solution is removed by the cycle process of vacuum and nitrogen filling. After reacting for 4-48 hours under the condition of 55-110 ° C, the methanol / water mixture is used as the precipitating agent, and the collected precipitate is filtered and dried to obtain UV-absorbing Properties and thermoplastic elastomer properties of lignin-based star polymers.

[0030] Lignin is alkaline lignin.

[0031] In the step (1), a catalyst is also added, which is 4-dimethylaminopyridine, N,N-lutidin...

Embodiment 1

[0039] (1) Synthesis of lignin macromolecular initiator: the basic lignin of 1.0g (hydroxyl content 9.01mmol), 0.89g (7.28mmol) of 4-diaminopyridine (DMAP) was added in the there-necked flask containing 40ml DMF, Stir to dissolve in an ice-water bath, then add 0.92ml of 2-bromoisobutyryl bromide (7.28mmol) dropwise, stir at room temperature for 12h, then raise the temperature to 50°C to continue the reaction for 12h. Finally, the reaction solution is poured into a large amount of distilled water, filtered, washed with water, and dried to constant weight to obtain a powdery lignin macromolecular initiator, and the trigger point content is 3.07mmolBr / g. The structural diagram of the lignin macromolecular initiator is as follows figure 1 with figure 2

[0040] (2) Synthesis of lignin-g-(methyl methacrylate-co-butyl acrylate) graft copolymer: [methyl methacrylate+butyl acrylate] / [initiator] / [catalyst] / [ Ligand]=(10+10):1:1:1

[0041] Lignin macromolecular initiator 0.0100g (0....

Embodiment 2

[0043] [methyl methacrylate+butyl acrylate] / [initiator] / [catalyst] / [ligand]=(40+60):1:1:1

[0044] Lignin macromolecular initiator (prepared in Example 1) 0.0100g (0.0307mmolBr), ligand N,N,N,N,N-pentamethyldiethylenetriamine (PMDETA) 8.12μL (0.0307mmol ), methyl methacrylate 0.1107 (1.228mmol), butyl acrylate 0.2241g (1.842mmol) were dissolved in 2mlTHF, and the oxygen in the mixed solution was removed through three cycles of freezing, vacuuming, and nitrogen charging. At the same time, Add 0.0054g (0.0307mmol) Cu(I)Br into the polymerization bottle, and put it in an oil bath at 80°C for 24h. 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 total conversion rate of monomer is 66% (weight method), Mn=12500g / mol (GPC)

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Abstract

The invention relates to a lignin-based starlike thermoplastic elastomer and a preparation method thereof. The preparation method comprises the following steps: (1) carrying out reaction on lignin and 2-bromoisobutyryl bromide to synthesize a lignin ATRP (atom transfer radical polymerization) macromolecular initiator; and (2) adding a hard monomer, a soft monomer, the lignin ATRP macromolecular initiator, a ligand and a good reaction solvent into a reaction bottle, fully stirring for dissolving, removing oxygen in the mixed solution by virtue of three circulating processes of freezing, vacuumizing and nitrogenization, adding a catalyst for reaction at 55-110 DEG C for 4-48 hours, filtering the collected precipitate by using a mixed liquid or methanol/water as a precipitator and drying to obtain the lignin-based starlike polymer with ultraviolet absorptivity and property of the thermoplastic elastomer. The lignin-based starlike polymer consisting of different monomers can be obtained by using the method. The mechanical property of the lignin-based starlike polymer is superior to that of a liner polymer with same compositions and the lignin-based starlike polymer can be used as a membrane material with ultraviolet absorptivity.

Description

technical field [0001] The invention relates to a lignin-based star-shaped thermoplastic elastomer and a preparation method thereof, in particular to a method for a natural compound star-shaped polymer. Background technique [0002] With the depletion of petroleum resources, the development of high-tech products using biomass resources as raw materials can not only alleviate the huge energy pressure brought about by the petrochemical energy crisis, but also fully realize the utilization of biomass resources, a huge energy source. Lignin is the second most abundant renewable resource on earth, its output is second only to cellulose, and it is cheap, biodegradable and environmentally friendly. However, most of the lignin from the paper industry is used in the form of combustion or waste, which is a huge waste of biomass resources. Therefore, it is imminent to develop a high value-added lignin material. [0003] Lignin is a mixture with an aromatic structure, and the main func...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F289/00C08F220/14C08F220/18C08F212/08C08F210/10
Inventor 王基夫俞娟储富祥王春鹏
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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