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A kind of production method of phosphorus flame retardant

A technology of phosphorus-based flame retardants and production methods, applied in the direction of phosphorus organic compounds, can solve the problems of high acid value, low flash point, waste of water resources, etc., and achieve good heat storage stability

Active Publication Date: 2016-04-27
扬州晨化新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Since the current domestic industrial production methods basically require water washing, this will not only waste water resources, but also make the acid value higher, and the obtained flash point will not be very high; phosphorus-containing wastewater is difficult to treat

Method used

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  • A kind of production method of phosphorus flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] At room temperature, mix 0.25mol catalyst (aluminum triethoxide) with 1000mol POCl 3 After mixing, pump them into the kettle together.

[0021] Pump the above mixture into the closed reaction kettle, open the vent valve and fill with N 2 Displace air, close N 2 valve. Then first raise the temperature of the kettle to 50-60°C, slowly open the ethylene oxide feed valve, and start to drop 50mol ethylene oxide to induce the esterification reaction. Control the temperature of the mixed system to keep warm at 50-60°C, continue to add ethylene oxide dropwise, and keep the system temperature at 50-60°C. Slowly raise the temperature of the system to 70-80°C for aging. After 3 hours, take a sample to measure the acid value. If the acid value reaches ≤0.2mgKOH / g, close the vent valve and discharge.

Embodiment 2

[0023] At room temperature, mix 1mol catalyst (butyl titanate) with 1000mol POCl 3 After mixing, pump them into the kettle together.

[0024] Pump the above mixture into the closed reaction kettle, open the vent valve and fill with N 2 Displace air, close N 2 valve. Then first raise the temperature of the kettle to 40-50°C, slowly open the ethylene oxide feed valve, and start to drop 50mol ethylene oxide to induce the esterification reaction. Control the temperature of the mixed system to keep warm at 40-50°C, continue to add ethylene oxide dropwise, and keep the system temperature at 40-50°C. Slowly raise the temperature of the system to 60-70°C for aging. After 3 hours, take a sample to measure the acid value. If the acid value reaches ≤0.2mgKOH / g, close the vent valve and discharge.

Embodiment 3

[0026] At room temperature, mix 1.5mol of catalyst (zirconium n-propoxide) with 1000mol of POCl 3 After mixing, pump them into the kettle together.

[0027] Pump the above mixture into the closed reaction kettle, open the vent valve and fill with N 2 Displace air, close N 2 valve. Then first raise the temperature of the kettle to 40-50°C, slowly open the propylene oxide feed valve, start to drop 30mol propylene oxide to induce the esterification reaction, and control the mixing with cooling water when the reaction exothermic temperature rises. Keep the temperature of the system at 45-55°C, continue to add propylene oxide dropwise, and keep the system temperature at 45-55°C. After the addition of 3250mol of propylene oxide is completed, close the propylene oxide drop valve, and at the same time, slowly raise the temperature of the system to Aging is carried out at 60-70°C. After 3 hours, samples are taken to measure the acid value. If the acid value reaches ≤0.2mgKOH / g, clos...

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Abstract

The invention discloses a production method (b) of a phosphorus based flame retardant, which relates to the production method of a chemical product. The production method comprises the following steps: mixing POC13 and a catalyst, subsequently heating to the temperature of 40 DEG C to 60 DEG C under an oxygen-free condition, dropwise adding ethylene oxide or propylene epoxide or epoxy chloropropane under a heat insulation condition, then slowly heating to the temperature of 60 DEG C to 80 DEG C for ageing, taking an aged sample liquid 3 hours later to measure the acid value, and discharging when the acid value is smaller than or equal to 0.2mgKOH / g to obtain the phosphorus based flame retardant. By adopting the method disclosed by the invention, the production process is simple, the problem of a large number of phosphorous wastewater which is generated in water washing of a crude product and cannot be treated in the original production method is effectively improved, no sewage pollution is caused, a low acid value can be obtained without water washing and a high flash point also can be obtained; and moreover, the phosphorus based flame retardant is good in heat storage stability, the catalyst is simple to prepare and no air pollution is caused, so the production method is applicable to industrial popularization and application.

Description

technical field [0001] The invention relates to a production method of a chemical product, in particular to a production method of a phosphorus-based flame retardant. Background technique [0002] With the development of social economy, due to the needs of fire safety in electronic and electrical materials, automobiles, high-rise buildings, transportation (high-speed rail, aircraft) and other fields, the materials used must be flame-retardant, so as to reduce the occurrence of fires and protect people's lives. Property safety, and the most common flame retardants are TCEP, TCPP and TDCP, all of which are additive flame retardants, easy to use, cheap, and have great market competitiveness. [0003] Tris(2-chloroethyl)phosphate, TCEP for short. It can be used in the production of polyurethane soft foam and hard foam. It has the functions of improving water resistance, cold resistance, antistatic property and soft hand feeling. Generally, TCEP is obtained by reacting phosphor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09
Inventor 董晓红房连顺管丹
Owner 扬州晨化新材料股份有限公司
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