Method for preparing TCPP (Tris(Chloroisopropyl)Phosphate) flame retardant

A flame retardant and oxidant technology, applied in the field of TCPP flame retardant preparation, can solve problems such as affecting product quality, reducing TCPP yield, increasing product acid value, etc., and achieving the effects of convenient operation, low odor and favorable production.

Active Publication Date: 2010-07-14
雅克(上海)化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can reduce the content of aldehyde compounds, it is found that the addition of hydroxylamine hydrochloride will cause a small amount of decomposition of TCPP, which reduces the yield of TCPP, and also increases the acid value of the product, affecting product quality.

Method used

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  • Method for preparing TCPP (Tris(Chloroisopropyl)Phosphate) flame retardant
  • Method for preparing TCPP (Tris(Chloroisopropyl)Phosphate) flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: in the 1000ml four-necked flask that thermometer, stirrer are housed, add 600g above-mentioned TCPP crude products that make, stir and heat up to 50 ℃, add 100g concentration and be the potassium perchlorate solution acidified with sulfuric acid of 0.1%, keep 50 ℃ The mixture was stirred and reacted for 30 minutes. After liquid separation, it was washed once with alkali and twice with water. The water layer was separated, and the water was removed by vacuuming to obtain the finished product TCPP. The aldehyde content was determined to be 7.4 ppm by gas chromatography. Gas Chromatography See figure 2 , see Table 2 for the peak data.

Embodiment 2

[0017] Embodiment 2: in the 1000ml four-necked flask that thermometer is housed, add 600g above-mentioned TCPP crude products that make above, stir and be warmed up to 60 ℃, add the potassium chlorate solution that 129g concentration is 0.1% sulfuric acid acidification, keep stirring under 60 ℃ React for 30 minutes, wash with alkali and water after liquid separation, separate the water layer, and vacuumize to remove water to obtain the finished product TCPP. The aldehyde content measured by gas chromatography is 5.3 ppm.

Embodiment 3

[0018] Embodiment 3: in the 1000ml four-necked flask that thermometer is housed, add 600g above-mentioned TCPP crude products that make above, stir and be warming up to 70 ℃, add the sodium chlorate solution that 290g concentration is 0.05% sulfuric acid acidification, keep 70 ℃ Stir and react for 30 minutes, after liquid separation, wash with alkali and water, separate the water layer, and vacuumize to remove water to obtain the finished product TCPP. The aldehyde content measured by gas chromatography is 0.7ppm.

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Abstract

The invention relates to a preparation method which can effectively eliminate odor ingredients (mainly aldehydes compounds) in TCPP (Tris(Chloroisopropyl)Phosphate). The method is characterized by comprising the following steps of: adding excessive oxidant solution relative to the aldehydes compound for reaction after a TCPP crude product is obtained through reaction, standing, separating liquid, then alkaline washing, water washing and distilling. The aldehyde compound which has favorable compatibility with the TCPP and is not separated easily can be removed, the aldehyde content in the TCPP is reduced to below 10 ppm from the previous 100 ppm or more and can be reduced to 0.7 ppm in the maximum degree, the odor of the TCPP and the prepared product is less, and the mild odor of the TCPP flame retardant is realized; and oxidant aqueous solution converting aldehyde into acid is added to react, wash and remove the odor, the method has convenient operation as well as simple, convenient and easy implementation, is beneficial to operation in production and does not affect the TCPP yield (the yield can increase by 0.5-1%) and an acid value compared with the previous patents; the aldehyde content can be reduced to a lower degree, and the obtained TCPP product is more stable.

Description

technical field [0001] The present invention relates to the improvement of the method for preparing phosphate flame retardants by reacting epoxy compounds with phosphorus oxychloride, especially the improvement of the applicant's prior application for patent CN200610038132.9 to further reduce the odor. Background technique [0002] Tris(chloroisopropyl)phosphate (TCPP for short) is a low molecular weight phosphorus halogen flame retardant widely used in polyurethane soft foam, rigid foam and plastic products. The current preparation method of TCPP is to obtain the crude product of TCPP by reacting phosphorus oxychloride with propylene oxide under the catalysis of Lewis acid catalyst, remove the catalyst by alkali washing, separate liquid, then wash to neutrality by water, separate the water layer, and distill to get the finished product. In this production process, some propylene oxide will be oxidized by phosphorus oxychloride to generate valeraldehyde or aldehyde compound...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C09K21/12
Inventor 沈琦褚昭宁赵毅周乐群
Owner 雅克(上海)化工新材料有限公司
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