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Flame-retardant acrylic fibre and preparation thereof

A flame retardant acrylic fiber and solution technology, applied in the field of flame retardant acrylic fiber, can solve the problems of difficult mass production, high operation level, inconvenient use, etc., and achieve the effects of easy industrial production, good flame retardant effect and wide application range.

Inactive Publication Date: 2009-05-20
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the copolymerization method is the general industrialization method adopted by flame-retardant acrylic fiber at present, the method has the following defects: it is necessary to change the original polymerization and spinning production process of conventional acrylic fiber spinning, which is inconvenient to use; when using inorganic solvent spinning , it is required that the content of flame retardant monomer in polyacrylonitrile copolymer should be ≤25wt%, and such content is difficult to meet the flame retardant requirements, such as vinyl chloride or vinylidene chloride and acrylonitrile copolymer requires vinyl chloride or vinylidene chloride The content of the flame retardant comonomer is above 40wt%; when the organic solvent is used as the spinning solvent, although the content of the flame retardant comonomer can be increased to above 40wt%, it will cause the heat resistance, weather resistance, dyeability and dimensional stability of the copolymer. The decline in performance such as resistance will affect the use effect and popularization and application of the product
Using plasma to carry out surface grafting, although the flame retardancy of the acrylic fiber or its fabric after treatment is better, the plasma generator is expensive and the operation level is high, so it is difficult to realize mass production

Method used

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  • Flame-retardant acrylic fibre and preparation thereof
  • Flame-retardant acrylic fibre and preparation thereof
  • Flame-retardant acrylic fibre and preparation thereof

Examples

Experimental program
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preparation example Construction

[0020] The preparation method of the hydrazine compound is not complicated. For example, the preparation of thiophosphoryl trihydrazide is to add phosphorus trichloride and hydrazine hydrate in a three-necked flask at a molar ratio of 1:3, and simultaneously add Triethylamine with the same mole of sulfur as phosphorus, magnetically stirred, controlled temperature at 0-5°C, stopped the reaction after 4 hours of reaction, filtered to remove triethylamine hydrochloride, and obtained thiophosphoryl trihydrazine flame retardant, yield 82-76%; Another example, to prepare acryloyl hydrazide, is to add acryloyl chloride and hydrazine hydrate into a three-necked flask with a molar ratio of 1:1, and at the same time add triethylamine with the same mole as acryloyl chloride, and magnetically stir. The temperature was controlled at 0° C., the reaction was stopped after 4 hours of reaction, and the triethylamine hydrochloride was removed by filtration to obtain the acrylohydrazide flame ret...

Embodiment 1

[0027] Preparation of flame retardant acrylic fibers.

[0028] First prepare thiophosphoryl trihydrazide: add phosphorous trichloride and hydrazine hydrate into a three-necked flask at a molar ratio of 1:3, and at the same time add triethylamine with the same mole as phosphorous trichloride, stir magnetically, and control The temperature was 0° C., the reaction was stopped after 4 hours of reaction, and the triethylamine hydrochloride was removed by filtration to obtain a thiophosphoryl trihydrazide flame retardant with a yield of 82%.

[0029] Then, the conventional acrylic fiber with a denier of 3.5dtex, a breaking strength of 3.3cN / dtex, a breaking elongation of 25%, and an LOI value of 18.2% was used as a raw material to prepare a flame-retardant acrylic fiber.

[0030] Add acrylic fiber and thiophosphoryl trihydrazide solution into a 250mL three-necked flask equipped with a mechanical stirrer at a mass ratio of 1:20, heat the thiophosphoryl trihydrazide solution to 100°C,...

Embodiment 2

[0037] Preparation of flame retardant acrylic fibers.

[0038]The reaction time of the acrylic fiber and thiophosphoryl trihydrazide in this embodiment is 40 minutes, the heating temperature of the thiophosphoryl trihydrazide solution is 95° C., and the mass ratio of the acrylic fiber to the phosphorotrihydrazide solution is 1:25. All the other preparation processes are the same as in Example 1.

[0039] After testing, the denier of the acrylic fiber is 3.5 dtex, the breaking strength is 3.0 cN / dtex, the breaking elongation is 22%, and the LOI value is 30.5%. Compared with Comparative Example 1, the flame-retardant acrylic fiber of this example does not contain halogen elements, and the LOI value is increased by 5.2%.

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Abstract

The invention relates to antiflaming acrylon and a preparation method thereof. The structural formula of the antiflaming acrylon is shown on the right, wherein, R is one out of dimethyl phosphoryl, diethyl phosphoryl, dimethyl sulfo-phosphoryl, diethyl sulfo-phosphoryl, propylene acyl, methyl propylene acyl, phosphinylidyne di-hydrazino, sulfo-phosphinylidyne di-hydrazino and sulfo-formyl hydrazine; and n is 750 to 1250. The preparation method comprises the following steps of: soaking acrylon fiber in a hydrazine solution according to the mass ratio of 1:10 to 30, heating the hydrazine solution to 80 to 100 DEG C, after reaction for 20 to 90min under the condition of stirring, taking out the acrylon fiber, being washed by water for 3 to 5 times, and obtaining the antiflaming acrylon after vacuum drying; and the hydrazine solution is one of the following solutions: the solutions of dimethyl phosphoryl hydrazine, diethyl phosphoryl hydrazine, dimethyl sulfo-phosphoryl hydrazine, diethyl sulfo-phosphoryl hydrazine, propylene acyl hydrazine, methyl propylene acyl hydrazine, phosphinylidyne tri-hydrazine, sulfo-phosphinylidyne tri-hydrazine and diamino thiourea.

Description

technical field [0001] The invention relates to an acrylic fiber preparation technology, in particular to a flame-retardant acrylic fiber without halogen elements and a method for preparing the flame-retardant acrylic fiber with a non-additional flame retardant containing nitrogen, phosphorus and sulfur. Background technique [0002] At present, there are four main ways to prepare flame-retardant acrylic fibers at home and abroad: copolymerization method, blending method, finishing method and thermal oxidation method. Copolymerization is a method commonly used in the world to manufacture flame-retardant acrylic fibers. [0003] The copolymerization method is a method for preparing flame-retardant acrylic fibers by firstly copolymerizing unsaturated monomers containing flame-retardant elements with acrylonitrile, and then using the copolymer for spinning. There are many types of flame retardant monomers used in this method, including halogen-containing compounds, phosphorus-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M11/68D06M13/422D06M13/44D06M13/432D06M101/28
Inventor 程博闻任元林蒋艾兵李振环康卫民庄旭品
Owner TIANJIN POLYTECHNIC UNIV
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