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Fire retardant 4-oxygen same-cage diphosphine phosphite ester compound and preparing method thereof

A technology of bisphosphorous phosphite and phosphite triester, which is applied in the field of organic phosphine flame retardant 4-oxygen co-cage bisphosphorous phosphite compound and its preparation, can solve the safety hazards of toxic gas and smoke, and halogen-based flame retardants. In order to achieve good environmental and economic benefits, easy large-scale conversion and production, and good compatibility

Active Publication Date: 2015-09-23
盐城云鹄新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogenated flame retardants are currently used in the largest amount in my country. Although they have significant advantages, the toxic gases and smoke generated during combustion also pose great safety hazards. With the promulgation of some flame retardant regulations by EU countries, halogenated flame retardants The scope of application of flame retardants is further limited

Method used

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  • Fire retardant 4-oxygen same-cage diphosphine phosphite ester compound and preparing method thereof
  • Fire retardant 4-oxygen same-cage diphosphine phosphite ester compound and preparing method thereof
  • Fire retardant 4-oxygen same-cage diphosphine phosphite ester compound and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, use nitrogen to exhaust the air in the bottle, add 14.00g (0.1mol) trishydroxymethyl phosphine oxide and 12.40g (0.1mol) Trimethyl phosphite. Under stirring, add 0.28g of triethylamine catalyst, heat and continue to feed nitrogen, heat up to 110°C for 9 hours, keep the temperature at the top of the column not higher than 65°C, and fractionally distill out the methanol produced by the reaction (recycled). Stop the reaction when the fraction reaches the theoretical amount, lower the temperature to below 20°C, add 50ml of ice water, stir for 30 minutes, disperse the white granular solid product in water, filter, rinse the filter cake with 10ml of ice water, compact and drain, and vacuum the filter cake Dry to obtain white solid 4-oxocage bisphosphorous acid ester with a yield of 92.5%, melting point: 82±2°C, and decomposition temperature: 273±5°C.

Embodiment 2

[0032] Example 2 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, use nitrogen to exhaust the air in the bottle, add 14.00g (0.1mol) trishydroxymethyl phosphine oxide and 12.40g (0.1mol) Trimethyl phosphite. Under stirring, add 0.14g of pyridine catalyst, heat and continue to feed nitrogen, heat up to 120°C for 8 hours, always control the column top temperature not higher than 65°C, fractionally distill out the methanol produced by the reaction (recycling), when the methanol fraction reaches Stop the reaction when the theoretical amount is reached, lower the temperature to below 20°C, add 45ml of ice water, stir for 30 minutes, disperse the white granular solid product in water, filter, rinse the filter cake with 10ml of ice water, compact and drain, and vacuum dry the filter cake. The white solid 4-oxocage diphosphite was obtained with a yield of 93.3%, a melting point of 82±2°C and a decomposition temperature of 2...

Embodiment 3

[0033] Example 3 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, the air in the bottle was driven out with nitrogen, and 14.00g (0.1mol) of trishydroxymethylphosphine oxide and 12.40g (0.1mol) of trihydroxymethylphosphine oxide were added. Trimethyl phosphite. Under stirring, add 0.15g of sodium methoxide catalyst, heat and continue to feed nitrogen, raise the temperature to 130°C for 7 hours, always control the column top temperature not higher than 65°C, fractionally distill out the methanol produced by the reaction (recovered for use), and use it as methanol fraction Stop the reaction when the theoretical amount is reached, lower the temperature to below 20°C, add 40ml of ice water, stir for 30 minutes, disperse the white granular solid product in water, filter, rinse the filter cake with 10ml of ice water, compact and drain, and vacuum dry the filter cake , to obtain white solid 4-oxo caged bisphosphorous acid ...

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Abstract

The invention relates to a fire retardant 4-oxygen same-cage diphosphine phosphite ester compound and a preparing method thereof. Please refer to the specification for the structural formula of the compound. According to the preparing method, tris (hydroxymethyl) phosphine oxide and phosphite triester which are equimolar are heated to 100-160 DEG C and react for 5-10 h under the protection of nitrogen and the action of a catalyst, and 4-oxygen same-cage diphosphine phosphite ester is obtained through purification. The compound is a fire retardant high in phosphorus content, excellent in fire retardance, and suitable for serving as the fire retardant of materials including polyester, polyurethane, epoxy resin, unsaturated polyester resin and polyolefin. Furthermore, manufacturing technique is simple, equipment investment is low, and industrial production is facilitated.

Description

technical field [0001] The invention relates to an organic phosphine flame retardant 4-oxo caged diphosphorous phosphite compound and a preparation method thereof, in particular to a 4-oxo-2,6,7-trioxa-1,4-diphosphorous A heterobicyclo[2.2.2]octane compound and a preparation method thereof, the compound is suitable for use as a flame retardant for polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and other materials. Background technique [0002] In recent years, organic synthetic polymer materials have been widely used in various fields of the national economy, and the fires caused by them have posed a serious threat to people's life and property safety. Adding flame retardants to these materials to reduce fire occurrence is an effective means , thus promoting the rapid development of flame retardants. Halogenated flame retardants are currently used in the largest amount in my country. Although they have significant advantages, the toxic gases and smoke g...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C08K5/5397C08L67/02
Inventor 王彦林杨珂珂
Owner 盐城云鹄新材料科技有限公司
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