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A piperazine-modified lignin/aluminum phosphate double-coated red phosphorus flame retardant and its application in hips

A technology for coating red phosphorus and lignin, which is applied in the field of piperazine modified lignin/aluminum phosphate double-coated red phosphorus flame retardants, can solve the problem of high flammability of HIPS, high cost of flame retardants, and low flame retardant efficiency and other problems, to achieve the effect of low price, high cost of solution, and improvement of moisture absorption

Active Publication Date: 2020-04-10
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a piperazine modified lignin / aluminum phosphate double-coated red phosphorus flame retardant and its application in HIPS, to solve the problem of high flammability, difficulty in flame retardancy and high cost of existing flame retardants in HIPS , low flame retardant efficiency and other issues

Method used

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  • A piperazine-modified lignin/aluminum phosphate double-coated red phosphorus flame retardant and its application in hips
  • A piperazine-modified lignin/aluminum phosphate double-coated red phosphorus flame retardant and its application in hips
  • A piperazine-modified lignin/aluminum phosphate double-coated red phosphorus flame retardant and its application in hips

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) Dissolve 10 g of enzymatic lignin in 100 mL of 5 wt% NaOH solution, pour it into a three-necked round-bottomed flask containing a condenser tube and a magnet, and heat the reaction device to 90 °C in a water bath , followed by adding 16 mL of 40wt% formaldehyde aqueous solution and magnetically stirring for 1 h to obtain lignin hydroxymethylation products.

[0031] (2) Add 4.3 g of anhydrous piperazine to (1) quickly, raise the temperature of the water bath to 90 °C, and continue the magnetic stirring reaction for 2 h to obtain the lignin amine methylated product.

[0032] (3) Add 60 mg sodium dodecylbenzenesulfonate and 6 g red phosphorus to (2), continue stirring and dispersing at 90 °C for 10 min, then add 15.6 g Al(NO 3 ) 3 9H 2 O, a reddish-brown precipitate was obtained, and the reaction was continued at 90 °C for 30 min, and then 5.0 g of 85% phosphoric acid was added. Stand still for 12 hours, filter and wash, and dry at 60°C to constant weight to obtain ...

Embodiment 2

[0034] (1) Dissolve 10 g of enzymatic lignin in 100 mL of 5 wt% KOH solution, pour it into a three-necked round-bottomed flask containing a condenser tube and a magnet, place the device in a water bath and heat it to 60 °C, Subsequently, 16 mL of 40 wt% acetaldehyde aqueous solution was added, and the reaction was performed under magnetic stirring for 1 h to obtain lignin hydroxymethylation products.

[0035] (2) Add 4.3 g of anhydrous piperazine to (1) quickly, raise the temperature of the water bath to 90 °C, and continue the magnetic stirring reaction for 2 h to obtain the lignin amine methylated product.

[0036] (3) Add 40 mg sodium dodecylbenzenesulfonate, 40 mg sodium hexametaphosphate and 8 g red phosphorus to (2), continue stirring and dispersing at 90 °C for 10 min, then add 10.1 g AlCl to the solution 3 ·6H 2 O, a reddish-brown precipitate was obtained, and the reaction was continued at 90 °C for 30 min, and then 5.0 g of 85% phosphoric acid was added. Stand for 1...

Embodiment 3

[0038] (1) Dissolve 10 g of alkali lignin in 100 mL of 5 wt% NaOH solution, and pour it into a three-neck round-bottomed flask containing a condenser tube and a magnet, place the device in a water bath and heat it to 90 °C, and then Add 16 mL of 40wt% formaldehyde aqueous solution, and magnetically stir the reaction for 1 h to obtain lignin hydroxymethylation products.

[0039] (2) Quickly add 9.7 g of piperazine hexahydrate to (1), raise the temperature of the water bath to 90 °C, and continue the magnetic stirring reaction for 2 h to obtain the lignin amine methylated product.

[0040] (3) Add 100 mg sodium lauryl sulfate and 10 g red phosphorus to (2), continue stirring and dispersing at 90 °C for 10 min, then add 8.5 g aluminum acetate to the solution to obtain a reddish-brown precipitate, continue stirring at 90 °C After reacting for 30 min, 5.0 g of 85% phosphoric acid was added. Stand for 12 h, filter and wash, and dry at 60 °C to constant weight to obtain a piperazine-m...

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Abstract

The invention provides a piperazine modified lignin / aluminum phosphate double-coated red phosphorus flame retardant and an application thereof in HIPS, and belongs to the field of high molecular material additives. A preparation method for the piperazine modified lignin / aluminum phosphate double-coated red phosphorus flame retardant comprises the following steps: using lignin as a raw material, performing a methylolation reaction with formaldehyde in an alkaline condition, through a Mannich reaction, grafting a piperazine molecule to a lignin macromolecule; and adding a dispersing agent, red phosphorus and aluminum salt into reaction solution and neutralizing alkali, adding phosphoric acid for reacting, separating out the macromolecule and coating the red phosphorus, forming a microcapsule-like structure. The piperazine modified lignin / aluminum phosphate double-coated red phosphorus flame retardant can be applied for flame retardance of most polymers. The piperazine modified lignin / aluminum phosphate double-coated red phosphorus flame retardant provided by the invention is capable of effectively improving problems that the red phosphorus absorbs moisture, and compatibility with a high molecular material is not good and the like, adequately using high phosphorus content of the red phosphorus, and enabling the high molecular material to acquire excellent flame retardant property.

Description

technical field [0001] The invention belongs to the technical field of preparation of halogen-free intumescent flame retardants, and more specifically relates to a piperazine-modified lignin / aluminum phosphate double-coated red phosphorus flame retardant and its application in HIPS. Background technique [0002] Red phosphorus is a traditional halogen-free high-efficiency flame retardant, but red phosphorus will react with water in the air to produce highly toxic phosphine, and it has poor thermal stability and low compatibility. Current research has found that some materials will coat red phosphorus to form a microencapsulated structure, which can effectively improve the shortcomings of red phosphorus. This structure has good moisture resistance and fluidity, and can make full use of the high phosphorus content of red phosphorus. The most commonly used charring agents in intumescent flame retardant systems for thermoplastics are polyalcohols, such as pentaerythritol, manni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/10C08K3/02C08L51/04C08H7/00
CPCC08H6/00C08K3/02C08K9/10C08K2003/026C08L2201/02C08L51/04
Inventor 靳艳巧黄少淮钟柔潮赖春梅熊雷
Owner FUZHOU UNIV
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