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Preparation method for 3-(2-isopropyl chloride) phosphate ester fire-retardant with high resistance to hydrolysis

A chloroisopropyl, hydrolysis-resistant technology, applied in the direction of phosphorus organic compounds, etc., can solve the problems of not mentioning the hydrolysis resistance of TCPP, the method of reducing the hydrolysis resistance of TCPP, and not mentioning it.

Active Publication Date: 2013-11-27
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is not mentioned that the favorable isomer ratio is beneficial to the improvement of TCPP hydrolysis resistance, and at the same time, it is not mentioned how to further reduce the content of easily hydrolyzed components in TCPP isomers to further improve the hydrolysis resistance of TCPP

Method used

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  • Preparation method for 3-(2-isopropyl chloride) phosphate ester fire-retardant with high resistance to hydrolysis
  • Preparation method for 3-(2-isopropyl chloride) phosphate ester fire-retardant with high resistance to hydrolysis
  • Preparation method for 3-(2-isopropyl chloride) phosphate ester fire-retardant with high resistance to hydrolysis

Examples

Experimental program
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Effect test

preparation example Construction

[0033] 2. Preparation of TCPP crude product:

[0034] According to the existing known process, add aluminum trichloride catalyst into phosphorus oxychloride, stir until the catalyst dissolves, then add propylene oxide dropwise at 65°C, keep the reaction temperature at 60-70°C, after adding propylene oxide dropwise, Continue the reaction at 80°C for 1.5 hours to obtain the crude product of TCPP.

Embodiment 1

[0041] 1) Add 500 grams of TCPP crude product and 50 grams of deionized water into a 1000-liter four-neck bottle equipped with a thermometer and a dropping funnel, stir and adjust the temperature to 0°C, and drop a hydrochloric acid solution with a concentration of 0.1N from the dropping funnel , after adjusting the pH to 5, control the temperature at 0°C, and continuously stir and hydrolyze for 90 minutes under acidic conditions to obtain the reaction liquid; Adjust the pH to 8 or 9 with sodium hydroxide solution, stir for half an hour, and then separate the upper alkaline water layer after standing for half an hour; Wash twice at 90°C, remove the water layer, vacuum distill and dehydrate, and filter to obtain TCPP with high hydrolysis resistance.

Embodiment 2-7

[0043] The implementation method is as in Example 1. After adding the materials, by adjusting different reaction temperatures in step 1), adjusting different pH values, and continuously stirring and hydrolyzing different reaction times, as in Example 1, each example of high hydrolysis-resistant TCPP is prepared.

[0044] Table 2. Different preparation conditions and easily hydrolyzed isomer component content and acid value

[0045]

[0046] Note: The unit of isomer content is parts per million (ppm); the unit of acid value is milligrams of potassium hydroxide per gram (mgKOH / g).

[0047] It can be seen that the content of isomers (iii) and (iv) is greatly reduced by the method of the present invention.

[0048] Table 3. TCPP hydrolysis resistance test data

[0049]

[0050] Note: The test data of hydrolysis resistance is the acid value, and the unit is milligram potassium hydroxide per gram (mgKOH / g).

[0051] It can be seen that the hydrolysis resistance of TCPP is gr...

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Abstract

A preparation method for a 3-(2-isopropyl chloride) phosphate ester fire-retardant with high resistance to hydrolysis belongs to the technical field of chemical engineering. The method comprises the following steps: allowing phosphorus oxychloride and epoxypropare to react under the action of a Lewis acid catalyst to synthesize a TCPP crude product; allowing the TCPP crude product to be subjected to hydrolytic treatment under the acidic condition, washing, dehydrating and filtering so as to prepare the 3-(2-isopropyl chloride) phosphate ester fire retardant with high resistance to hydrolysis. Due to the adoption of the method, the content of the 3-(2-isopropyl chloride) phosphate ester in the TCPP crude product can be reduced to 100 ppm, even 10 ppm, the content of the 2-(2-propyl chloride) (2-isopropyl chloride) phosphate ester can be reduced to 5000 ppm, even 500 ppm, and accordingly, the hydrolysis resistance of the 3-(2-isopropyl chloride) phosphate ester is finally improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of a highly hydrolysis-resistant tris-(2-chloroisopropyl) phosphate flame retardant. Background technique [0002] The preparation of TCPP is well known to those skilled in the art, mainly through the reaction of phosphorus oxychloride and propylene oxide under the catalysis of Lewis acid such as aluminum trichloride, n-butyl titanate or titanium tetrachloride. The crude product of TCPP obtained by the reaction of phosphorus oxychloride and propylene oxide is then processed by alkali washing, water washing, distillation dehydration, and filtration to obtain TCPP. [0003] TCPP is a flame retardant widely used in various polymers such as polyurethane flexible foam and rigid foam. Polyurethane foam, especially rigid foam, is widely used as various energy-saving insulation materials, but it is easy to burn, so it needs to be modified by ad...

Claims

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Application Information

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IPC IPC(8): C07F9/09
Inventor 金译平周奋王秋伟
Owner ZHEJIANG WANSHENG
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