Preparation method of tri(2-chloroisopropyl)phosphate (TCPP)

A technology of chloroisopropyl and phosphate esters, applied in the direction of phosphorus organic compounds, etc., can solve problems such as not mentioning the root cause

Active Publication Date: 2015-11-25
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there is no mention of the origin of TCPP ether in TCPP, and how to mo...

Method used

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  • Preparation method of tri(2-chloroisopropyl)phosphate (TCPP)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] First pump 4600 kg of phosphorus oxychloride into the 5000L stirred phosphorus oxychloride measuring kettle equipped with a solid feeder, then add 15 kg of anhydrous aluminum trichloride catalyst through the solid feeder, stir and dissolve at room temperature To obtain phosphorus oxychloride solution, propylene oxide is continuously passed through a dehydration tower filled with dehydrating agent calcium oxide and collected into a total of 5300 kilograms in a 10000L metering tank. After testing, the water content of propylene oxide in the metering tank is 28PPM. Add the phosphorus oxychloride solution containing the catalyst and the dehydrated propylene oxide into the mixture at the same time, the reaction temperature is controlled at 65°C during the feeding process, and the feeding speed of the two is controlled during the feeding process so that the weight ratio is phosphorus oxychloride: propylene oxide =1:1.152, after adding the materials at the same time in proporti...

Embodiment 2-5

[0036] Except using propylene oxide with different water content after dehydration by different dehydrating agents, other operations repeat Example 1, and the final results are shown in the following table:

[0037] Table 1. Effect of propylene oxide water content on product yield and TCPP ether content

[0038]

[0039] As can be seen from the data of Examples 1-5 of the present invention and comparative examples, after adopting the method of the present invention, TCPP ether in the product obtained obviously reduces, and product yield also has certain improvement simultaneously.

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Abstract

The invention relates to a preparation method of tri(2-chloroisopropyl)phosphate (TCPP). The TCPP is prepared by reacting dehydrated epoxypropane and phosphorus oxychloride. The invention particularly relates to a preparation method of TCPP with low TCPP ether impurity content and high product yield. The method comprises the following steps: before adding the epoxypropane to react, adding a dehydrating agent into the epoxypropane or passing the epoxypropane through a dehydrating-agent-filled dehydration tower to perform deep dehydration on the epoxypropane until the water content in the epoxypropane is less than 100 ppm, and reacting with the phosphorus oxychloride to obtain the TCPP. The TCPP ether content in the TCPP product is less than 1000 ppm. Compared with the TCPP obtained in the prior art, the method greatly lowers the TCPP ether content in the product and enhances the product yield.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, in particular to a method for preparing tris-(2-chloroisopropyl) phosphate with low TCPP ether content, which reacts dehydrated propylene oxide with phosphorus oxychloride to prepare tris -(2-Chloroisopropyl)phosphate. Background technique [0002] Tris-(2-chloroisopropyl) phosphate, referred to as 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 adding flame retardants. [0003] 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 r...

Claims

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Application Information

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IPC IPC(8): C07F9/09
Inventor 沈高波王福兵金译平
Owner ZHEJIANG WANSHENG
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