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Lignin-based polymer as well as preparation method and application thereof

A lignin-based and polymer technology, which is applied in the field of polymer controllable polymerization, can solve problems such as long reaction time, and achieve the effects of high molecular weight, low cost, and simple equipment and process.

Pending Publication Date: 2022-07-05
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

[0005] Technical problem to be solved: At present, most methods of RAFT polymerization to prepare lignin-based polymers still use expensive finished RAFT reagents, and subsequent reactions need to add initiators, and the reaction time is relatively long

Method used

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  • Lignin-based polymer as well as preparation method and application thereof
  • Lignin-based polymer as well as preparation method and application thereof
  • Lignin-based polymer as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1 Preparation of lignin dithioester chain transfer agent

[0022] Weigh 1 g of lignin (with a hydroxyl content of about 6.07 mmol) into the reaction flask, add 30 mL of DMSO and 0.73 g of 50 wt.% NaOH (1.5 equal) solution, ultrasonicate for 1 h under sealed conditions, and continue magnetic stirring for 1 to 2 h to ensure that the lignin is in DMSO 1.39g CS was added dropwise to the system under ice-water bath conditions. 2 (3 equal), after 4.5 hours of reaction at room temperature, 2.21 g of ethyl α-bromophenylacetate (1.5 equal) was added dropwise to the system, and the reaction was continued for 16 hours.

[0023] After the reaction was completed, extraction was carried out twice with n-hexane, the lower layer solution was dropped into distilled water, and the precipitate was obtained by centrifugation. The obtained precipitate was subjected to Soxhlet extraction with ether for 48 hours, and then dried in a vacuum drying oven at 40°C to obtain a brown powder...

Embodiment 2

[0024] Example 2 Preparation of lignin-acrylamide copolymer

[0025] Weigh 0.1 g of lignin-based dithioester chain transfer agent (about 0.143 mmol of dithioester group) obtained in Example 1, and 4.76 mmol of acrylamide monomers were added to contain 50 g of N,N-dimethylformaldehyde. In an airtight container of amide, after nitrogen and deoxygenation for 30 minutes, irradiated with a 365nm LED lamp for 8 hours, dropwise into ethanol for centrifugation, then washed twice with ethanol, and dried in a vacuum drying oven at 40 °C to obtain light brown lignin-acrylamide polymer. The molecular weight and molecular weight distribution of the polymer were determined by GPC. The results showed that the molecular weight of the product increased significantly after the reaction, and the molecular weight distribution index was around 1.9, showing good polymerization controllability.

Embodiment 3

[0026] Example 3 Preparation of lignin-acrylamide copolymer

[0027] Weigh 0.1 g of lignin-based dithioester chain transfer agent (about 0.143 mmol of dithioester group) prepared in Example 1, and add 23.8 mmol of acrylamide monomers containing 50 g of N,N-dimethylformaldehyde. In an airtight container of amide, after nitrogen and deoxygenation for 30 minutes, irradiated with a 365nm LED lamp for 8 hours, dropwise into ethanol for centrifugation, then washed twice with ethanol, and dried in a vacuum drying oven at 40 °C to obtain light brown lignin-acrylamide polymer. The molecular weight and molecular weight distribution of the polymer were determined by GPC. The results showed that the molecular weight of the product increased significantly after the reaction, and the molecular weight distribution index was around 1.5, showing good polymerization controllability.

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Abstract

The invention relates to a lignin-based polymer and a preparation method and application thereof, corncob lignin, carbon disulfide and ethyl alpha-bromophenylacetate are used as raw materials to react for 15-20 hours at room temperature, and a product is subjected to precipitation, centrifugation, extraction and drying to obtain brown lignin-based chain transfer agent powder; the method comprises the following steps: adding a lignin-based chain transfer agent and an acrylamide monomer into N, N-dimethylformamide, filling nitrogen for deoxidation, and irradiating at room temperature by using an LED (Light Emitting Diode) as a light source to initiate an RAFT (Reversible Addition-Fragmentation Chain Transfer) polymerization reaction, thereby obtaining the lignin-based acrylamide polymer. The lignin dithioester RAFT chain transfer agent prepared by the invention has good light initiation property, and can initiate RAFT polymerization reaction under the conditions of 365 nm and white light.

Description

technical field [0001] The invention relates to the field of polymer controllable polymerization, in particular to a lignin-based polymer and a preparation method and application thereof. Background technique [0002] Lignin is the second largest natural polymer in reserves after cellulose, accounting for about 25-30% of the total biomass materials on the earth. The annual output of lignin in the paper industry, cellulosic materials, cellulosic ethanol industry and other industries is as high as 50 million tons. As the largest renewable source of aromatic compounds in nature, lignin has great potential as a starting material for the production of bulk or functionalized aromatic compounds. Its structure has various active sites such as methoxy, phenol (alcohol) hydroxyl, carbonyl, carboxyl, and unsaturated double bonds. However, the inherent structural heterogeneity of lignin molecules and the existence of intermolecular hydrogen bonds make these active sites. The reactivit...

Claims

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Application Information

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IPC IPC(8): C08F289/00C08F220/56C08F2/48
CPCC08F289/00C08F2/48C08F2438/03C08F220/56
Inventor 许玉芝刘婧伊张代晖王春鹏储富祥
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY