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A kind of chitosan tetramethylene phosphine sulfate flame retardant and its preparation method and application

A technology of chitosan tetramethylene sulfuric acid and tetrahydroxymethyl phosphorus sulfate is applied in the field of halogen-free flame retardants, which can solve the problems of poor compatibility, small molecular weight of flame retardants, poor degradability, etc., and achieve antibacterial properties. performance, good water resistance persistence, good interface compatibility

Active Publication Date: 2020-01-10
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Tetrahydroxymethyl phosphorus sulfate can be used as a permanent flame retardant for polyester-cotton fabrics, and can be used to prepare flame retardants with amines such as urea, thiourea, and melamine, but these flame retardants have small molecular weights, poor compatibility, and Poor degradability

Method used

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  • A kind of chitosan tetramethylene phosphine sulfate flame retardant and its preparation method and application
  • A kind of chitosan tetramethylene phosphine sulfate flame retardant and its preparation method and application
  • A kind of chitosan tetramethylene phosphine sulfate flame retardant and its preparation method and application

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[0024] The invention provides a kind of preparation method of chitosan tetramethylene phosphine sulfate flame retardant, comprising following preparation steps:

[0025] Carry out electrostatic adsorption of tetrakis hydroxymethyl phosphorus sulfate and chitosan in water, obtain tetrakis hydroxymethyl phosphorus sulfate / chitosan complex;

[0026] Dehydrating and covalently grafting the tetrakis phosphine hydroxymethyl sulfate / chitosan complex to obtain the chitosan tetramethylene phosphine sulfate flame retardant.

[0027] In the invention, tetrakis hydroxymethyl phosphorus sulfate and chitosan are electrostatically adsorbed in water to obtain tetrakis hydroxymethyl phosphorus sulfate / chitosan complex. In the present invention, the mass ratio of tetrakis hydroxymethyl phosphorus sulfate to chitosan is preferably 1:1 to 5:1, more preferably 2:1 to 4:1; the mass ratio of chitosan to water is The ratio is preferably 1:0.5 to 1:1, more preferably 1:1. In the present invention, t...

Embodiment 1

[0039]At room temperature, weigh 10 g of chitosan, and weigh tetrakis hydroxymethyl sulfate according to the mass ratio of tetrakis hydroxymethyl phosphorus sulfate to chitosan is 5:1, and the mass ratio of water to chitosan is 1:1. Phosphorus, chitosan (viscosity-average molecular weight is 150,000) and water are added to the reaction kettle, stirred until the chitosan is completely dissolved, heated to 90°C, kept stirring for 2 hours, unloaded, and then left to react in an oven. Reaction conditions: 150°C, keep warm for 2h. After that, the temperature was lowered to 80° C., and dried for 12 hours to obtain 40.61 g of chitosan tetramethylene phosphine sulfate solid powder.

Embodiment 2

[0041] At room temperature, weigh 10 g of chitosan, and weigh tetrakis hydroxymethyl sulfate according to the ratio of tetrakis hydroxymethyl phosphorus sulfate to chitosan mass ratio of 4:1 and water to chitosan mass ratio of 1:1. Phosphorus, chitosan (viscosity-average molecular weight is 30,000) and water are added to the reaction kettle, stirred until the chitosan is completely dissolved, heated to 80°C, kept stirring for 3 hours, unloaded, and then left to react in an oven. 140°C, keep warm for 4h. Afterwards, the temperature was lowered to 60° C., and dried for 12 hours to obtain 34.31 g of chitosan tetramethylene phosphine sulfate solid powder.

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Abstract

The invention provides a preparation method for a chitosan tetramethylene phosphonium sulphate flame retardant. The preparation method comprises the following steps: performing electrostatic adsorption on tetrakis hydroxymethyl phosphonium sulphate and chitosan in water to obtain a tetrakis hydroxymethyl phosphonium sulphate / chitosan compound; performing dehydration covalent graft reaction on thetetrakis hydroxymethyl phosphonium sulphate / chitosan compound to obtain the chitosan tetramethylene phosphonium sulphate flame retardant. The chitosan tetramethylene phosphonium sulphate flame retardant prepared by the method provided by the invention does not contain halogen, has an antibacterial effect, and is non-toxic, degradable, green and environmentally friendly; the flame retardant is highin molecular weight, keeps linearity, does not have volatility, and has water washing resistance, migration resistance, good compatibility, high stability and good flame retarding effect.

Description

technical field [0001] The invention relates to the technical field of halogen-free flame retardants, in particular to a chitosan tetramethylene phosphine sulfate flame retardant and a preparation method and application thereof. Background technique [0002] Polyacrylonitrile is a flammable polymer material, and it emits toxic cyanide when burned. The flame-retardant polyacrylonitrile materials that have been industrialized in the world are mainly modified by copolymerization of vinyl chloride monomer to improve the flame-retardant performance. However, the halogen flame retardants generate a large amount of smoke during the flame-retardant process and produce a large amount of harmful gases. Environmentally friendly products. [0003] Intumescent flame retardants are usually monomolecular or molecular composite flame retardants based on phosphorus, nitrogen, and carbon elements, of which carbon is the source of carbonization; phosphorus is the source of acid, which acts as...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L33/20C08L5/08C08B37/08
Inventor 刘群丁斌郝凤岭关昶李祥王海东孙晓竹耿伟涛宋传捷宋钰
Owner JILIN INST OF CHEM TECH
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