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A kind of synthetic method of brominated lignin

A synthesis method and lignin technology are applied in the field of modification of natural polymer materials, which can solve the problems of poor flame retardancy, large-scale application limitation, low glass transition temperature, etc., and achieve easy control of reaction conditions, low cost of raw materials, The effect of mild reaction conditions

Active Publication Date: 2020-03-17
SHANDONG RUNKE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its low glass transition temperature and poor flame retardancy, traditional bisphenol A epoxy resin does not meet the requirements of high-frequency high-performance electronics industry and aerospace industry
Tetrabromobisphenol A is widely used in the electronics industry and aerospace industry due to its excellent flame retardant properties, but the high cost of this product limits its large-scale application, and its raw materials come from the petrochemical industry to increase environmental load
At present, organic solvents are mostly used in the synthesis process of modified brominated lignin, and the synthesis cost is high, and the transparency of the modified brominated lignin is poor, which limits its application in the field of flame retardants.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 300ml of water to a 2000ml four-necked bottle, add 100g of natural lignin under stirring, slowly add 5g of concentrated sulfuric acid to the four-necked bottle, raise the temperature to 40°C, add 500g of bromine dropwise to the four-necked bottle, and control the dropping port Protrude below the liquid level, dropwise is completed, keep warm for 2 hours, continue to slowly raise the temperature to 60°C, keep warm for 5 hours, and after the reaction is over, change to a distillation device, and heat up the steam to distill out the unreacted remaining bromine. The bromine temperature is 80°C, until no obvious bromine is evaporated at the condenser mouth, stop heating, and then use 10% sodium thiosulfate aqueous solution to remove a small amount of residual bromine in the water, then use 10% sodium thiosulfate aqueous solution to adjust the pH to neutral. Continue natural cooling, add 30g of 26% hydrogen peroxide, stir at 45°C for 0.5h, oxidize to remove colored organi...

Embodiment 2

[0027] Add 500ml of water into a 2000ml four-necked bottle, add 100g of natural lignin under stirring, slowly add 10g of concentrated hydrochloric acid into the four-necked bottle, and raise the temperature to 50°C. Add 1000g of bromine dropwise to the four-necked bottle, control the dropping port to extend below the liquid surface, after the dropwise addition, keep warm for 4 hours, continue to slowly raise the temperature to 70°C, keep warm for 8 hours, and after the reaction is over, change to a distillation device, Raise the temperature by steam stripping to distill unreacted remaining bromine. The bromine temperature is 100°C. When there is no obvious bromine steaming out at the condenser mouth, stop heating, and then use 10% sodium thiosulfate aqueous solution to remove a small amount of bromine in the water. After residual bromine, the pH was adjusted to neutral with 10% aqueous sodium hydroxide solution. Continue natural cooling, add 50g of 33% hydrogen peroxide, stir ...

Embodiment 3

[0030] Add 400ml of water into a 2000ml four-necked bottle, add 100g of natural lignin under stirring, slowly add 7.5g of concentrated nitric acid into the four-necked bottle, and raise the temperature to 45°C. Add 750g of bromine dropwise to the four-neck bottle, control the dropping port to extend below the liquid surface, after the dropwise addition, keep warm for 3 hours, continue to slowly raise the temperature to 65°C, keep warm for 6.5 hours, after the reaction is over, change to a distillation device , heating up water steam stripping to distill unreacted remaining bromine, the bromine temperature is 90°C, until there is no obvious bromine steaming out at the condenser mouth, stop heating, and then use 10% sodium thiosulfate aqueous solution to remove the bromine from the water After a small amount of residual bromine, adjust the pH to neutral with 10% aqueous sodium methoxide. Continue natural cooling, add 45g of 30% hydrogen peroxide, stir at 50°C for 1 hour, oxidize...

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PUM

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Abstract

The invention relates to a synthesizing method for brominated lignin. According to the synthesizing method, technical problems like adoption of an organic solvent, high synthesis cost and poor transparency of synthetic brominated lignin in modified brominated lignin synthesis processes in the prior art are solved. The invention discloses a synthesizing method for brominated lignin, which comprisesthe following steps: adding lignin, water and an inorganic strong acid catalyst to a reaction vessel; heating to 40-50 Celsius system; adding excess bromine to react for 2 to 4 hours; heating continually to 60-70 Celsius system; reacting 5-8h; after the end of the reaction, removing the remaining bromine; adjusting the pH of the system to neutral with alkaline substances; adding peroxide; stirring, filtering, washing, drying, and obtaining a brominated lignin product. The invention is widely applied to the field of modification of natural polymer materials.

Description

technical field [0001] The invention relates to the modification of a natural polymer material, in particular to a synthesis method of brominated lignin. Background technique [0002] Lignin is the third most abundant organic matter after cellulose and chitin on the earth. It is a precious resource bestowed by nature to human beings, but it has not been widely used so far. pollute. As a natural polymer material, lignin has many functional groups and has excellent chemical activity. It can react with aldehydes, epichlorohydrin and isocyanate to obtain modified products of lignin, which can replace some petrochemical raw materials for The modification of polymer materials is beneficial to the comprehensive utilization of renewable resources. [0003] Tetrabromobisphenol A is an excellent flame retardant prepared from polymer materials with the largest output and consumption. It can endow various resin materials with excellent combustion resistance and self-extinguishing prop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00
CPCC08H6/00
Inventor 王东全吴多坤秦善宝
Owner SHANDONG RUNKE CHEM
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