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Preparation method of lignosulfonate based three-source integrated flame retardants

A technology of lignosulfonate and sodium lignosulfonate, which is applied in the direction of fireproof coatings, etc., can solve problems such as ineffective utilization of components, environmental pollution, waste of lignin resources in papermaking black liquor, etc.

Inactive Publication Date: 2019-12-03
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, most of the lignin is used for incineration, not only its components have not been effectively used, but also pollute the environment
In the pulp and paper industry, about 50 million tons of lignin by-products are obtained from plants every year. So far, more than 95% of lignin is still used as industrial pulping waste, and is directly discharged into rivers or rivers along with wastewater. Concentrated and burned, the discharge of papermaking black liquor not only causes a huge waste of lignin resources, but also pollutes the environment

Method used

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  • Preparation method of lignosulfonate based three-source integrated flame retardants
  • Preparation method of lignosulfonate based three-source integrated flame retardants

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 20g of 80% phosphoric acid solution into a 100ml three-necked flask, stir to raise the temperature, and add 5g of sodium lignosulfonate. After completely dissolving, heat up to 100°C, react for 8h, and then add 5g of dicyandiamide to the reaction solution after cooling down to room temperature For amine, the temperature was raised to 40°C, and the reaction was continued for 10 hours. Brown precipitates gradually precipitated in the system. After the reaction was completed, the product was left to stand, then filtered with suction, washed with methanol, and dried in vacuum to constant weight. Obtain lignosulfonate phosphate dicyandiamide salt.

Embodiment 2

[0021] Add 20g of 80% phosphoric acid solution into a 100ml three-neck flask, stir to raise the temperature, and add 5g of sodium lignosulfonate. After completely dissolving, heat up to 110°C, react for 8h, and then add 5g of dicyandiamide to the reaction solution after cooling down to room temperature For amine, the temperature was raised to 40°C, and the reaction was continued for 10 hours. Brown precipitates gradually precipitated in the system. After the reaction was completed, the product was left to stand, then filtered with suction, washed with methanol, and dried in vacuum to constant weight. Obtain lignosulfonate phosphate dicyandiamide salt.

Embodiment 3

[0023] Add 20g of 80% phosphoric acid solution into a 100ml three-neck flask, stir to raise the temperature, and add 5g of sodium lignosulfonate. After completely dissolving, heat up to 120°C, react for 8h, and then add 5g of dicyandiamide to the reaction solution after cooling down to room temperature For amine, the temperature was raised to 40°C, and the reaction was continued for 10 hours. Brown precipitates gradually precipitated in the system. After the reaction was completed, the product was left to stand, then filtered with suction, washed with methanol, and dried in vacuum to constant weight. Obtain lignosulfonate phosphate dicyandiamide salt.

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Abstract

The invention provides lignosulfonate which is taken as an excellent carbon source, and a renewable material with great application prospects. The lignosulfonate has a large number of hydroxyl, aromatic rings, methoxy groups and other groups, and is an amorphous macromolecule of a large network structure. The lignosulfonate has the high carbon content, requirements of three-source integrated expansion flame retardants can be met, and the lignosulfonate can be used as a carbon source to be applied to preparation of the flame retardants. The lignosulfonate is used as a raw material, first esterified by a phosphoric acid source, then heating up is conducted, reaction of prepared lignosulfonate phosphate ester is conducted by using a reagent containing a nitrogen source, and several flame retardants of three-source integrated structures are synthesized.

Description

technical field [0001] The invention relates to a preparation method of a lignosulfonate-based three-source integrated flame retardant, in particular to a method for activating the hydroxyl group of lignosulfonate phosphate and catalyzing the esterification reaction. Background technique [0002] Halogen flame retardants are widely used as flame retardants due to their high flame retardant efficiency, rich sources of raw materials, and affordable prices, but the combustion of halogen compounds produces toxic gases. In recent years, due to its unique flame retardant mechanism, halogen-free, low smoke, and low toxicity, intumescent flame retardants have met the requirements of today's era of protecting the ecological environment. [0003] Due to the synergistic effect of acid source, carbon source and gas source, the intumescent flame retardant system forms a dense porous intumescent carbon layer on the surface of the material during the combustion process. The intumescent cha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/14C09K21/12
CPCC09K21/12C09K21/14
Inventor 金立维张永贺王春鹏
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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