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A kind of modified lignin flame retardant and preparation method thereof

A technology of lignin and flame retardant, applied in the field of modified lignin flame retardant and its preparation, can solve the problems of unreasonable selection of raw materials, low content of flame retardant elements, and high equipment requirements, and achieve unaffected physical and mechanical properties , Excellent flame retardant and fire resistance, and the effect of overcoming interface incompatibility

Active Publication Date: 2020-08-25
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above research work has achieved certain results in improving the performance of flame retardants, but there are also the following shortcomings: unreasonable selection of raw materials, resulting in low phosphorus and nitrogen content in flame retardants, and poor intumescent flame retardant effects, such as hexamethylol The cost of melamine-based melamine is high, the content of flame retardant elements in imidazole is low, and there is a safety risk in the severe moisture absorption and hydrolysis of phosphorus oxychloride in the air; in addition, the production process is complicated, the operation is cumbersome, the requirements for equipment are high, and multiple separations are required Purification leads to low flame retardant yield

Method used

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  • A kind of modified lignin flame retardant and preparation method thereof
  • A kind of modified lignin flame retardant and preparation method thereof
  • A kind of modified lignin flame retardant and preparation method thereof

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Effect test

Embodiment 1

[0046] A kind of preparation method of modified lignin flame retardant of the present invention, comprises the following steps:

[0047] (1) Preparation of phosphorylated lignin: Add 50g of lignin into the three-necked flask A, and continue to add 10.0mL of H with a mass fraction of 85% under stirring 3 PO 4 solution, 0.85g urea and 1.2 mL of 3% hydrogen peroxide, and then stirred at 70°C to make the material in the three-necked flask A undergo dry phosphorylation reaction for 2 hours to obtain phosphorylated lignin;

[0048] Preparation of melamine-formaldehyde prepolymer: Add 8.0mL of 37% formaldehyde and 2.0mL of 0.4mol / L NaOH solution into a three-necked flask and stir evenly, add 7.0g of melamine under stirring, heat up to 60°C and stir and reflux for 120min to obtain Melamine formaldehyde prepolymer;

[0049] (2) Mix the phosphorylated lignin obtained in step (1) with the melamine formaldehyde prepolymer, stir and raise the temperature to 75°C for reflux reaction, the ...

Embodiment 2

[0053] A kind of preparation method of modified lignin flame retardant of the present invention, comprises the following steps:

[0054] (1) Preparation of phosphorylated lignin: Add 50g of lignin into the three-neck flask A, and continue to add 15.0mL of H with a mass fraction of 85% under stirring 3 PO 4 Solution, 0.85g urea and 1.2 mL hydrogen peroxide with a mass fraction of 3%, and then stirred at 80°C to make the material in the three-necked flask A undergo dry phosphorylation reaction for 3 hours to obtain phosphorylated lignin;

[0055] Preparation of melamine-formaldehyde prepolymer: Add 8.0mL of 37% formaldehyde and 2.0mL of 0.4mol / L NaOH solution into a three-necked flask, stir evenly, add 15.0g of melamine under stirring, heat up to 60°C, stir and reflux for 120min, Obtain melamine formaldehyde prepolymer;

[0056] (2) Mix the phosphorylated lignin obtained in step (1) with the melamine formaldehyde prepolymer, stir and raise the temperature to 80°C for reflux re...

Embodiment 3

[0060] A kind of preparation method of modified lignin flame retardant of the present invention, comprises the following steps:

[0061] (1) Preparation of phosphorylated lignin: Add 50g of lignin into the three-necked flask A, and continue to add 12.0mL of H with a mass fraction of 85% under stirring. 3 PO 4 solution, 0.85g urea and 1.2 mL of 3% hydrogen peroxide, and then stirred at 90°C to make the material in the three-necked flask A undergo dry phosphorylation reaction for 3 hours to obtain phosphorylated lignin;

[0062] Preparation of melamine-formaldehyde prepolymer: Add 13.0g of melamine and 2.0mL of 0.4mol / L NaOH solution into a three-necked flask, stir evenly, add 8.0mL of 37% formaldehyde drop by drop under stirring, heat up to 60°C and stir to reflux reaction 120min, obtain melamine formaldehyde prepolymer;

[0063] (2) Mix the phosphorylated lignin and melamine formaldehyde prepolymer obtained in step (1), stir and raise the temperature to 90°C for reflux react...

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Abstract

The invention provides a modified lignin flame retardant which is prepared from raw materials through phosphate esterification reaction and melamine grafting reaction. The raw materials include, by weight, 200-600 parts of lignin, 100-150 parts of melamine, 100-120 parts of H3PO4 solution, 60-100 parts of formaldehyde solution, 15-25 parts of NaOH solution, 5-10 parts of urea and 10-50 parts of hydrogen peroxide. The modified lignin flame retardant has excellent flame resistance and is characterized in that the flame retardant is low in smoke and toxicity and the like, and the flame retardantis applicable to flame resistance of wood, plastics, wood plastic composite materials and coatings. The invention further provides a preparation method of the modified lignin flame retardant. The method is simple in process, convenient to operate and high production efficiency and achieves the environmental protection concept that waste is turned into wealth.

Description

technical field [0001] The invention belongs to the technical field of flame retardant materials and their preparation, and in particular relates to a modified lignin flame retardant and a preparation method thereof. Background technique [0002] Intumescent flame retardant (IFR) is a compound flame retardant mainly composed of nitrogen and phosphorus. It does not contain halogen and does not use antimony oxide as a synergist. This type of flame retardant foams and expands when heated , so it is called intumescent flame retardant, which is a kind of high-efficiency, low-toxic and environmentally friendly flame retardant. After the 1990s, the research on intumescent flame retardants gradually became active, and it was recognized as one of the effective ways to realize the non-halogenation of flame retardants. [0003] Intumescent flame retardants have three basic elements, namely acid source, carbon source and gas source. Acid sources are also called dehydrating agents or c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08H7/00C08L63/00C08L77/00C08L87/00
CPCC08G81/00C08H6/00C08L63/00C08L77/00C08L2201/02C08L2205/03C08L87/005
Inventor 胡云楚王琼文瑞芝黄自知王文磊袁利萍胡进波吴袁泊邓明向李慧陈秋菊
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY