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Hydroxymethylphosphonothioheterocyclic phenylthiophosphonate compound and preparation method thereof

A technology of phenylphosphonothioate and hydroxymethylphosphonothioate, which is applied in the field of hydroxymethylphosphonothiophosphono heterocyclic phenylthiophosphonate compounds and their preparation, and can solve problems such as hazards , to achieve the effects of simple process, high performance of phosphorus and sulfur synergistic flame retardant, and convenient operation

Active Publication Date: 2017-04-12
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, people have gradually realized that halogen-based flame retardants will decompose and produce toxic and corrosive gases that cause serious harm to the environment and human body when they are burned. an important topic in

Method used

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  • Hydroxymethylphosphonothioheterocyclic phenylthiophosphonate compound and preparation method thereof
  • Hydroxymethylphosphonothioheterocyclic phenylthiophosphonate compound and preparation method thereof
  • Hydroxymethylphosphonothioheterocyclic phenylthiophosphonate compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and connected to a hydrogen chloride absorbing device on the condenser, the air in the bottle was driven away with nitrogen, and 15.60g (0.1mol) of three Hydroxymethylphosphine sulfide, under stirring, at 20°C, add 21.10g (0.1mol) phenylphosphonothiodichloride dropwise, make it fully mixed, heat up to 80°C, hydrogen chloride begins to be released, heat up to 110°C Insulate for 3 hours, then raise the temperature to 160°C for 9 hours, wait until no hydrogen chloride is released, then vacuum the hydrogen chloride to exhaust, cool down to below 10°C, add 50ml of ice water, stir, and add 5% sodium carbonate solution dropwise to make the reaction system pH = 7, standing for stratification, separating the lower layer material liquid, and removing a small amount of water in the material by distillation under reduced pressure to obtain the product hydroxymethylphosph...

Embodiment 2

[0030] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and connected to a hydrogen chloride absorbing device on the condenser, the air in the bottle was driven away with nitrogen, and 15.60g (0.1mol) of three Hydroxymethylphosphine sulfide, under stirring, at 20°C, add 21.10g (0.1mol) phenylphosphonothiodichloride dropwise, make it fully mixed, heat up to 80°C, hydrogen chloride begins to be released, heat up to 110°C Keep warm for 3 hours, then raise the temperature to 130°C and keep it warm for 12 hours, wait until no hydrogen chloride is released, then vacuum the hydrogen chloride to exhaust, lower the temperature to below 10°C, add 40ml of ice water, add 5% sodium carbonate solution dropwise under stirring, and make the reaction system pH = 7, standing for stratification, separating the lower layer material liquid, and removing a small amount of water in the material by distillation under reduced pressure to ...

Embodiment 3

[0031]Example 3 In a 150ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and connected to a hydrogen chloride absorption device on the condenser, the air in the bottle was driven away with nitrogen, and 50ml xylene was added, and 15.60g ( 0.1mol) trimethylol phosphine sulfide, under stirring, at 20°C, add dropwise 21.10g (0.1mol) phenylphosphonothioate dichloride, make it fully mixed, heat up to 80°C, hydrogen chloride begins to be released, Raise the temperature to 110°C for 3 hours, then raise the temperature to 140°C for 9 hours, wait for no hydrogen chloride to be released, remove xylene (recycled) by distillation under reduced pressure, cool down to below 10°C, add 40ml of ice water, stir, and drop 5 % sodium carbonate solution to make the pH of the reaction system=7, let it stand for stratification, separate the lower layer material liquid, and distill under reduced pressure to remove a small amount of water in the material t...

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Abstract

The invention relates to a 5-(hydroxymethyl)-2-phenyl-1,3,2,5-dioxadiphosphorinane 2,5-disulfide compound and a preparation method thereof. Please see the structure of the compound in the specifications. The preparation method of the compound comprises the steps that under the protection of nitrogen, tris (hydroxymethyl) phosphine sulfide and phenylthiophosphonic dichloride which are equal in molar weight are fully and evenly mixed, the temperature is raised to 110 DEG C, a reaction is conducted for 3 h, the temperature is raised to 130-160 DEG C again, a reaction is conducted for 7-12 h, hydrogen chloride is completely exhausted, purification is conducted, and then 5-(hydroxymethyl)-2-phenyl-1,3,2,5-dioxadiphosphorinane 2,5-disulfide is obtained. The phosphorus content of the compound is high, phosphorus and sulfur synergistic flame retardant performance is excellent, and the compound is suitable for being used as a flame retardant of unsaturated polyester resin, polyving akohol, polyurethane, epoxy resin and the like. The preparation method of the compound is a one-step reaction method, the technology is simple, equipment investment is small, and industrial production can be easily achieved.

Description

technical field [0001] The invention relates to an organic phosphine flame retardant hydroxymethylphosphonothiocyclic phenylthiophosphonate compound and a preparation method thereof, in particular to a 1,4-dithio-1-phenyl- 4-hydroxymethyl-2,6-dioxa-1,4-diphosphorinane compound and its preparation method, the compound is suitable for use as flame retardant of unsaturated resin, polyvinyl alcohol, epoxy resin, etc. It is used as a reactive flame retardant for polyurethane; it can also be used as an intermediate in organic synthesis. Background technique [0002] With the development of polymer material science, various polymer composite materials have gradually replaced the status of traditional materials due to their excellent comprehensive properties, and have been widely used in all aspects of social production and life. However, due to the flammability of polymer materials, while bringing great convenience to people, it also brings potential fire safety hazards. Therefor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5398C08L101/02
CPCC08K5/5398
Inventor 王玉霞杨珂珂王彦林
Owner HENAN UNIVERSITY
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