Preparation method of spirocyclic phosphate flame retardant for spandex fiber and flame-retardant spandex fiber based on spirocyclic phosphate flame retardant

A spirocyclic phosphoric acid and spandex fiber technology, applied in the field of flame-retardant textile fibers, can solve the problems of difficulty in fully releasing flame-retardant efficiency, poor air and moisture permeability of textiles, poor compatibility and spinnability, and achieve good spinnability, Excellent washing resistance, flame retardant and long-lasting effect

Pending Publication Date: 2021-12-10
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ordinary flame retardants are prone to problems of poor compatibility and spinnability
At present, there are three main methods of introducing flame retardants into spandex fibers: one is post-fiber treatment, but this method easily leads to poor air and moisture permeability and poor durability of textiles, which limits its application fields; the other is to use flame retardants , dyeing auxiliaries, other auxiliaries, etc. are blended and added to the polyurethane matrix, and then spun to obtain flame-retardant spandex
For example, the patent CN201511003945.X reports a preparation method of flame-retardant spandex fiber. The flame retardant used can endow the spandex with anti-dripping properties, but the realization of the flame-retardant effect is achieved by compounding flame retardants (phenyl phosphonates) Halogen-free phosphorus-based flame retardants / non-metal oxide synergistic flame retardants) and dyeing aids are mixed in polyurethane polymer solutions for ripening and spinning, and the flame retardant efficiency is difficult to release completely; patent CN201610808145.3 reports a microscopic Preparation method of uniformly dispersed zirconium phosphate synergistic flame-retardant spandex, the limiting oxygen index LOI of the obtained flame-retardant spandex is > 28
The third is to use reactive flame retardants, that is, to participate in the polymerization reaction of monomers containing flame retardant components, so that spandex has durable flame retardant properties, but the flame retardants have the risk of affecting the physical properties of spandex reaction process
However, whether the flame retardant is suitable for flame retardant spandex fiber has not been verified
In addition, the commonly used polytetrafluoroethylene anti-dripping agent is expensive and has the problem of uneven dispersion

Method used

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  • Preparation method of spirocyclic phosphate flame retardant for spandex fiber and flame-retardant spandex fiber based on spirocyclic phosphate flame retardant
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  • Preparation method of spirocyclic phosphate flame retardant for spandex fiber and flame-retardant spandex fiber based on spirocyclic phosphate flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A stirrer, a thermometer and a condenser are installed in a dry reactor. Stir 54.1g of benzoquinone and 27.2g of pentaerythritol evenly, add 2.1g of anhydrous aluminum chloride, heat to 90°C, then slowly add 68.7g of phosphorus oxychloride, react at 90°C for 5 hours, cool to room temperature after the reaction is completed , using sodium hydroxide with a mass concentration of 10% to adjust the pH of the flame retardant to 7, and distilling under reduced pressure at 150° C. for 8 hours to obtain a transparent viscous liquid, which is a spirocyclic phosphate flame retardant. The whole reaction process is carried out under the condition of stirring (speed 400r / min).

Embodiment 2

[0025] A stirrer, a thermometer and a condenser are installed in a dry reactor. Stir 47.1g of phenol and 27.2g of pentaerythritol evenly, add 1.5g of anhydrous aluminum chloride, heat to 90°C, then slowly add 83.7g of phosphorus oxychloride, react at 90°C for 5 hours, cool to room temperature after the reaction is completed, Using sodium hydroxide with a mass concentration of 10% to adjust the pH of the flame retardant to 7, distilling under reduced pressure at 150° C. for 8 hours to obtain a transparent viscous liquid, which is a spirocyclic phosphate flame retardant. The whole reaction process is carried out under the condition of stirring (speed 300r / min).

Embodiment 3

[0027] A stirrer, a thermometer and a condenser are installed in a dry reactor. Stir 55.2g of hydroquinone and 27.2g of pentaerythritol evenly, add 1.8g of anhydrous aluminum chloride, heat to 90°C, then slowly add 93.2g of phosphorus oxychloride, react at 90°C for 5 hours, after the reaction is completed Cool down to room temperature, use 10% sodium hydroxide to adjust the pH of the flame retardant to 7, and distill under reduced pressure at 150°C for 8 hours to obtain a transparent viscous liquid, which is a spirocyclic phosphate flame retardant. Whole reaction process all carries out under the condition of stirring (speed 500r / min).

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PUM

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Abstract

The invention discloses a preparation method of a spirocyclic phosphate flame retardant for spandex fiber and flame-retardant spandex fiber based on the spirocyclic phosphate flame retardant . The preparation method comprises the following steps: firstly, uniformly stirring a macromolecular regulator and pentaerythritol, then slowly adding anhydrous aluminum chloride, heating to 80-120 DEG C, then slowly adding phosphorus oxychloride, reacting for 2-7 hours under the condition of 80-120 DEG C, and after the reaction is completed, cooling to room temperature, adjusting the pH value of the flame retardant to 7, and carrying out reduced pressure distillation at 100-150 DEG C for 4-10 hours to obtain a transparent viscous liquid, namely the spirocyclic phosphate flame retardant. The flame retardant is high in flame retardant efficiency, effectively prevents molten drops and can meet high-temperature melting of spandex fibers, and the method is free of waste solvent and waste gas emission, simple in production process and controllable in cost.

Description

technical field [0001] The invention relates to the technical field of flame-retardant textile fibers, in particular to a preparation method of a spirocyclic phosphate flame retardant for spandex fibers. Background technique [0002] Textiles are an important basic material for the national economy and people's livelihood, and its application scope covers many fields such as daily life, medical protection, aerospace, transportation and so on. In recent years, the ignition or combustion of textiles has brought huge losses to people's lives and property safety, and has become a serious social problem. Scholars at home and abroad have done a lot of research work on the flame retardancy of fibers and their textiles. Polyurethane fiber (referred to as spandex) has the properties of high elasticity and high elongation similar to rubber, and can be used to meet the requirements of comfort and also require clothing with stretch elasticity, such as professional sportswear, fitness c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574D01F1/07D01F6/94
CPCC07F9/657172D01F1/07D01F6/94
Inventor 曾少华汪启明朱启免柯许麟陈鹏鹏聂王焰徐颖周艺峰
Owner ANHUI UNIVERSITY
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