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Method for synthesizing dithio dineopentyl phosphate fire retardant

A technique for the synthesis of neopentyldithiophosphoric acid ester, which is applied in the fields of chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problem of using toxic solvents, high cost and technical process Long-term problems, to achieve the effect of low price, low toxicity and simple process

Active Publication Date: 2011-01-19
HEBEI JIGAO CHEM FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The purpose of the present invention is to provide a molecular formula C 10 h 20 o 5 P 2 S 2 , the structural formula is:

Method used

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  • Method for synthesizing dithio dineopentyl phosphate fire retardant
  • Method for synthesizing dithio dineopentyl phosphate fire retardant
  • Method for synthesizing dithio dineopentyl phosphate fire retardant

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Embodiment 1

[0032] Add 180g of cyclohexane into a 1500ml round bottom flask, add 25g of neopentyl glycol and stir evenly, then add 45g of phosphorus trichloride, fully dissolve at 52°C, then add 80g of triethylamine dropwise, heat up to 58°C and keep After 2 hours, add 25 g of triethylamine and 1.3 g of water, raise the temperature to 71° C. and keep for 10 hours to obtain the product of the present invention, the phosphorothioate flame retardant, with a molecular formula of C10Hz0O5P2S2 and a yield of 81.1%. After filtering and grinding, the product of the present invention is obtained. The phosphorothioate flame retardant suspension has a particle size of 0.82 μm as detected by a particle size tester.

Embodiment 2

[0034] Add 250g of cyclohexane into a 1500ml round bottom flask, add 25g of neopentyl glycol and stir evenly, then add 38g of phosphorus trichloride, fully dissolve at 40°C, then add 85g of triethylamine dropwise, heat up to 50°C and keep After 2.5 hours, add 40 g of triethylamine and 13 g of water, raise the temperature to 60° C. and keep for 12 hours to obtain the product sulfur phosphoric acid ester flame retardant of the present invention, the molecular formula is C10H20O5P2S2, and the yield is 81.3%. The phosphate ester flame retardant suspension has a particle size of 0.81 μm as detected by a particle size tester.

Embodiment 3

[0036] Add 115g of cyclohexane into a 1500m] round bottom flask, add 25g of neopentyl glycol and stir evenly, then add 62g of phosphorus trichloride, fully dissolve at a temperature of 55°C, then add 70g of triethylamine dropwise, and heat up to 65°C Keep at ℃ for 1.5 hours, then add 15g of triethylamine and 2g of water, raise the temperature to 75℃ and keep for 8 hours to obtain the product of the present invention, the sulfur phosphoric acid ester flame retardant, the molecular formula is C10H20O5P2S2, and the yield is 81.3%. After filtering and grinding, the present invention is obtained. The product phosphorothioate flame retardant suspension has a particle size of 0.79 μm as detected by a particle size tester.

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Abstract

The invention discloses a method for synthesizing dithio dineopentyl phosphate fire retardant. The synthesis process comprises: (a) filling a solvent A in a stirred vessel, adding dineopentyl alcohol, fully stirring, adding phosphorus thiochloride, and fully dissolving at a constant temperature of 40 to 55 DEG C; (b) dripping solvent B, heating to 50 to 65 DEG C, and keeping the temperature for 1.5 to 2.5 hours; (c) adding a solvent C and water, heating to 60 to 75 DEG C and keeping the temperature for 8 to 12 hours; and (d) filtering and grinding to obtain dithio dineopentyl phosphate fire retardant suspension, which is the product of the invention. The solvent A is cyclohexane, the solvent B is triethylamine or the mixed solution of cyclohexane and triethylamine, and the solvent C is triethylamine. In the invention, the process is simple and short in process, the raw materials are widely available and cheap, the yield is high and the industrial prospect is promising; the dithio dineopentyl phosphate fire retardant contains the phosphorus and sulfur high-efficiency fire-retarding elements at the same time, so the fire retarding performance of cellulose is improved considerably under the synergistic effect of the phosphorus and sulfur; and the dithio dineopentyl phosphate fire retardant is high-efficiency and durable fire retardant.

Description

technical field [0001] The invention relates to a method for synthesizing a flame retardant, in particular to a method for synthesizing a flame retardant which contains high-efficiency flame-retardant elements phosphorus and sulfur and is specially used for viscose fibers. Background technique [0002] Viscose fiber, like natural cellulose fiber, has excellent comfort performance, which is incomparable to other fibers and is widely favored by consumers. But whether it is natural cellulose fibers such as cotton and hemp, or chemical cellulose fibers such as viscose, all cellulose fibers have a biggest weakness, that is, they are flammable! Flammability limits the further development and wider application of cellulose fiber products, so developing cellulose fibers and their derivatives with good flame-retardant properties is an important research task. [0003] As early as the 1930s, fire retardants had been applied to the flame retardant treatment of cellulose fibers. These...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
Inventor 张志伟
Owner HEBEI JIGAO CHEM FIBER
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