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Preparation method of flame retardant dithio pyrophosphate

A technology of dithiopyrophosphate and flame retardant, which is applied in the field of flame retardant, can solve the problems of damage and high cost, and achieve the effects of low cost, stable properties and few by-products

Pending Publication Date: 2022-07-05
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main problem to be solved by the present invention is that organic solvents such as toluene, xylene and dioxane are used in the preparation of the flame retardant DDPS in the process to cause high costs, and it avoids the use of triethylamine or pyridine acid-binding agents to produce large odors. The pressure on the environment and the defects of strong toxicity and harm to production operators provide a method for preparing phosphorus-containing flame retardant DDPS by using water as a solvent and calcium oxide as an alkali. This method is green, simple, efficient, low in cost and post-processing. easy to handle

Method used

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  • Preparation method of flame retardant dithio pyrophosphate
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  • Preparation method of flame retardant dithio pyrophosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0030] A method for preparing DDPS, comprising the following experimental steps:

[0031] Weigh 0.368g (2mmol) of DDSP into a 200ml round-bottomed flask, add 50ml of deionized water, stir at room temperature to dissolve it, start adding 0.11g (2mmol) of calcium oxide powder, stir mechanically for 24h, there will be Precipitation was precipitated, and after the reaction was completed, washed with 95% absolute ethanol, filtered and dried to obtain 314 mg of the target compound DDPS. Yield 90.7%.

[0032]

[0033] 1 H NMR (400MHz, CDCl 3 )δ4.48(d,J=10.8Hz,4H),4.04-3.94(m,4H),1.33(s,6H),0.91(s,6H). 13 C NMR (101MHz, CDCl 3 )δ79.06,79.03,78.99,77.32,77.00,76.68,32.15,32.12,32.09,21.81,19.85.

Embodiment 2

[0035] A method for preparing DDPS, a gram-level experiment, comprising the following experimental steps:

[0036] Weigh 1.84g (10mmol) of DDSP into a 500ml round-bottomed flask, add 250ml of deionized water, stir at room temperature to dissolve, start adding 0.56g (10mmol) of calcium oxide powder, stir mechanically for 24h, there will be Precipitation was precipitated, and after the reaction was completed, washed with 95% absolute ethanol, filtered and dried to obtain 1.46 g of the target compound DDPS. Yield 84.4%.

Embodiment 3

[0038] A method for preparing DDPS, the alkali is optimized, comprising the following experimental steps:

[0039] Weigh 0.368g (2mmol) of DDSP into a 200ml round-bottomed flask, add 50ml of deionized water, stir at room temperature to dissolve it, start adding 0.224g (2mmol) of potassium tert-butoxide, stir mechanically for 24h, after the reaction is completed, use Washed with 95% absolute ethanol, filtered and dried to obtain 0.138 g of the target compound DDPS. Yield 40%.

[0040]

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Abstract

The invention discloses a preparation method of a flame retardant dithio pyrophosphate, which is characterized in that the flame retardant DDPS is synthesized with high yield by using 5, 5-dimethyl-2-sulfo-2-chloro-1, 2, 3-dioxo phosphorus heterocyclic cyclohexane (DDSP) and calcium oxide under the condition that water is used as a solvent. According to the reaction, water is used as a reaction solvent, so that the defect of high cost caused by using organic solvents such as methylbenzene, dimethylbenzene and dioxane in the prior art is avoided; the defects that in a traditional process, due to the fact that triethylamine or a pyridine acid-binding agent is used, generated smell is large, pressure is caused to the environment, toxicity is high, and production operators are hurt are overcome, and the target compound DDPS is synthesized at the room temperature through a green and energy-saving method at the high yield. The method has the advantages of short reaction time, low cost, simple operation steps, simple post-treatment and less pollution, and is easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of flame retardant, and specifically relates to a method for preparing flame retardant DDPS in a green way by using water as a solvent. Background technique [0002] The flame retardant mechanism of pyrophosphate organic compounds is that fibers containing phosphide decompose and release phosphoric acid when heated, and combine into polyphosphoric acid when heated strongly. They are all strong dehydration catalysts, which can dehydrate fibers and leave only coke. . The dehydration reaction inhibits the production reaction of L-glucose, and the generated coke isolates the contact between the internal cellulose and oxygen, and suffocates the test combustion. At the same time, the coke with poor thermal conductivity can also reduce the thermal decomposition reaction of cellulose, thereby achieving the purpose of flame retardant. [0003] At present, there are few types of flame retardant viscose fibers in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65742
Inventor 王龙孙宏媛王华胡为民
Owner CHINA THREE GORGES UNIV
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