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Preparation method of mixed flame retardant used for spinning

A flame retardant, textile technology, applied in the field of preparation of phosphonate mixed flame retardants for textiles, to achieve the effects of wide application prospects, good mixing uniformity, and simple process

Inactive Publication Date: 2016-03-30
传化智联股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the defects of the above-mentioned prior art, and provide a preparation method of a mixed flame retardant for textiles, which uses non-flame retardant raw materials to obtain a mixed flame retardant through a chemical synthesis method, and completes the chemical synthesis simultaneously. Synthesis and physical blending to address issues with physical compounding of existing hybrid flame retardants

Method used

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  • Preparation method of mixed flame retardant used for spinning
  • Preparation method of mixed flame retardant used for spinning
  • Preparation method of mixed flame retardant used for spinning

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a four-necked flask equipped with a stirrer, a distillation device, a thermometer, and an air duct, add 0.160mol trimethylolpropane, 0.160mol dipentaerythritol, 0.528mol trimethyl phosphite, and 0.006mol phosphoric acid, heat and ventilate nitrogen, Slowly raise the temperature to 85°C, and react at this temperature for 5h to obtain the intermediate and methanol, and distill the methanol out. Then add 0.336mol dimethyl methylsulfate and 0.007mol butyl bromide to the intermediate, react at 185°C for 16h, and remove excess dimethylmethylsulfate (applied mechanically) under reduced pressure to obtain a free Color transparent viscous liquid 110.362g, yield 95.8%.

Embodiment 2

[0024] In a four-neck flask equipped with a stirrer, a distillation device, a thermometer, and an air duct, add 0.100mol trimethylolethane, 0.200mol dipentaerythritol, 0.55mol triethyl phosphite, and 0.002mol polyphosphoric acid, heat and Nitrogen was blown, and the temperature was slowly raised to 85° C., and reacted at this temperature for 5 hours to obtain the intermediate and ethanol, and the ethanol was distilled off. Then add 0.350mol triethyl phosphate and 0.008mol bromoisobutane to the intermediate, react at 185°C for 16h, remove excess triethyl phosphate under reduced pressure (applicable), and obtain a colorless transparent viscous liquid 126.275 g, yield 96.1%.

Embodiment 3

[0026] In a four-necked flask equipped with a stirrer, a distillation device, a thermometer, and an air duct, add 0.110mol of dipentaerythritol, 0.230mol of trimethylolpropane, 0.495mol of tributyl phosphite, and 0.011mol of sulfuric acid, heat and ventilate nitrogen, Slowly raise the temperature to 85°C, and react at this temperature for 5h to obtain the intermediate and butanol, and distill the butanol out. Add 0.385 mol of trimethyl phosphate and 0.009 mol of bromopentane to the intermediate, react at 185°C for 16 hours, remove excess trimethyl phosphate under reduced pressure (applicable), and obtain 113.726 g of a colorless transparent viscous liquid. Yield 95.6%.

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Abstract

The invention discloses a preparation method of a mixed flame retardant used for spinning. The mixed flame retardant is prepared through physical mixing at present. As cyclic phosphonate compounds generally have higher viscosity, and the lower the temperature is, the poorer the flow is, not only is the operation inconvenient to carry out during physical compounding but also the problems of poor mixing uniformity and difficulty in filtration also exist. Raw materials used in reaction include raw materials A, a raw material B and a raw material C, wherein the raw materials A are two or more of trimethylolethane, trimethylolpropane and dipentaerythritol; the raw material B is one of trimethyl phosphite, triethyl phosphite and tributyl phosphite; the raw material C is one of dimethyl methylphosphonate, trimethyl phosphate and triethyl phosphate; a mixture formed by at least two cyclic phosphonate compounds is directly obtained through reaction among the three kinds of raw materials. The preparation method has the beneficial effects that the mixed flame retardant with different components and ratios is directly prepared by controlling the ratio of the reactant raw materials and has the advantages of simple process, good mixing uniformity of the product, easiness in control of chemical components, and the like.

Description

technical field [0001] The invention relates to the preparation of a mixed flame retardant, in particular to a preparation method of a phosphonate mixed flame retardant for textiles. Background technique [0002] With the development of modern science and technology and the progress of the textile industry, the types of textiles continue to increase, and their application scope continues to expand and extend to all aspects of people's production and life. However, textile materials are generally flammable or combustible, which can easily cause fire accidents. According to statistics, more than 20% of the fire accidents in the world are caused or expanded due to the burning of textiles, especially residential fires. Therefore, the flame-retardant finishing of textiles has become an urgent issue. [0003] In recent years, countries around the world have invested a lot of technical force in the field of textile flame retardant research, and have developed a series of flame re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574D06M13/288
CPCC07F9/657181D06M13/288D06M2200/30
Inventor 徐会志沈伟胡娟王胜鹏傅幼林
Owner 传化智联股份有限公司
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