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A kind of preparation method of high-purity phosphate flame retardant tris (2-chloropropyl) phosphate

A technology of tris and chloropropyl phosphates, applied in chemical instruments and methods, phosphorus organic compounds, compounds of elements of Group 5/15 of the periodic table, etc., can solve the problem of unstable product quality, affecting product yield, and long contact time. and other problems, to achieve the effect of light product smell, short reaction time and fast reaction speed

Active Publication Date: 2019-06-14
福建新安科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The traditional post-processing method not only has a small device capacity, but also has unstable product quality. More importantly, due to the hydrolyzability of phosphate itself, the product will be in contact with acid, alkali and water for too long during the post-processing process, which will affect the quality of the product. yield

Method used

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  • A kind of preparation method of high-purity phosphate flame retardant tris (2-chloropropyl) phosphate
  • A kind of preparation method of high-purity phosphate flame retardant tris (2-chloropropyl) phosphate
  • A kind of preparation method of high-purity phosphate flame retardant tris (2-chloropropyl) phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 5000L reactor, 600kg of the last batch of materials was left at the bottom, and 2600kg of phosphorus oxychloride was put in. After adding 6kg of phosphorus trichloride, 6kg of pyrophosphoryl chloride, and 7kg of aluminum trichloride, propylene oxide was passed again, and the temperature was Control the flow at 50-100kg / h at 35-40°C (initial stage of reaction); control at 100-300kg / h at temperature at 45-50°C (middle stage of reaction); control at 300-400kg at temperature at 50-55°C / h (late stage of reaction). At the end of the reaction, when the temperature drops by 3°C / min, the automatic chain will automatically close the propylene oxide feed valve, keep it warm for 1 hour, and test the acid value ≤ 0.3, which is qualified, and put into the crude product tundish.

[0029] Such as figure 1As shown, put 5.5 tons of crude product intermediate tank into the caustic washing kettle, turn on the stirring, start to heat up and turn on the vacuum, the temperature rises t...

Embodiment 2

[0033] 5000L reactor, keep 600kg of the last batch of material, put in 2600kg of phosphorus oxychloride, add 12kg of phosphorus trichloride, 7kg of aluminum trichloride, then pass through propylene oxide, the temperature is 20-40℃, the flow rate Control at 50-80kg / h (initial stage of reaction); temperature at 45-55°C, flow control at 100-200kg / h (middle stage of reaction); temperature at 60-65°C, flow control at 300-400kg / h (late reaction ). At the end of the reaction, when the temperature drops by 0.1°C / min, the automatic chain will automatically close the propylene oxide feed valve, keep it warm for 1 hour, and test the acid value ≤ 1, which is qualified, and put into the crude product tundish.

[0034] Such as figure 1 As shown, put 5.5 tons of crude product intermediate tank into the caustic washing kettle, turn on the stirring, start to heat up and turn on the vacuum, the temperature rises to 70-80°C, pull the vacuum for 10-30min, then add 1.5 tons of washing water, add ...

Embodiment 3

[0038] The difference with Example 2 is the preparation of the crude product: 5000L reactor, the last batch of material left 600kg at the bottom, dropped into 2600kg of phosphorus oxychloride, added 12kg of pyrophosphoryl chloride, 7kg of aluminum trichloride, and then passed Propylene oxide, temperature at 50-60°C, flow control at 50-120kg / h (initial stage of reaction); temperature at 60-70°C, flow control at 100-250kg / h (middle stage of reaction); temperature at 70-80°C , the flow rate is controlled at 300-400kg / h (late stage of reaction). At the end of the reaction, when the temperature drops by 0.1°C / min, the automatic chain will automatically close the propylene oxide feed valve, keep it warm for 1 hour, and test the acid value ≤ 1, which is qualified, and put into the crude product tundish.

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Abstract

The invention discloses a preparation method of high-purity tris(clorisopropyl) phosphate as a phosphate flame retardant. The product obtained by the existing method is dark in color, high in color number, unstable in acid value, low in purity and high in content of isomeride as a secondary component; the high-content aldehydes are also produced, so that the product has thick pungent smell. The preparation method of high-purity tris(clorisopropyl) phosphate comprises the following steps: adding catalysts and additives into phosphorus oxychloride, then slowly dropwise adding epoxypropane, obtaining a crude product of tris(clorisopropyl) phosphate after the reaction is ended, removing low-boiling-point materials, washing with alkali, washing with water, distilling, dewatering and filtering to obtain the product which is tris(clorisopropyl) phosphate; and controlling the temperature reduction speed or the flow of cooling medium to achieve automatic control of reaction endpoint. According to the preparation method of high-purity tris(clorisopropyl) phosphate as the phosphate flame retardant, the reaction speed is rapid, the reaction time is short, the automatic control of the reaction endpoint is achieved, the prepared TCPP product is higher in purity, the ratio of main components in the product is obviously increased, and the flame-retardant performance is improved.

Description

technical field [0001] The invention relates to the field of preparation of phosphate flame retardants, in particular to a preparation method of high-purity phosphate flame retardant tris(2-chloropropyl) phosphate (TCPP). Background technique [0002] Tris (2-chloropropyl) phosphate, also known as tris (chloroisopropyl) phosphate, namely TCPP, English name: Tris (clorisopropyl) Phosphate, mainly has three isomers, namely: phosphate tris ( 1-chloro-2-propyl) ester, English name Tris(1-chloro-2-propyl)phosphate; Phosphate di(2-chloro-2-propyl)(1-chloro-2-propyl)ester, English name Bis(2-chloro-2-propyl)-2-chlor opropyl phosphate; bis(1-chloro-2-propyl)(2-chloropropyl) phosphate, English name Bis(2-chloropropyl)-1- Chloro-2-propyl phosphate, the first isomer is the main component, which plays a key role in the flame retardant performance, so its content directly affects the flame retardant performance of the product; the second and third isomers Isomers are minor components. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09
CPCC07F9/091
Inventor 揭少卫许自华高勇民王绍龙钱广滨
Owner 福建新安科技有限责任公司
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