A kind of preparation method of triisooctyl phosphate

A technology of triisooctyl phosphate and isooctyl alcohol, which is applied in the field of preparation of triisooctyl phosphate, can solve the problems of high by-products and low yield, and achieve the goals of reducing pollution, increasing reaction yield, and saving production costs Effect

Active Publication Date: 2018-12-28
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above several preparation methods have higher by-products and lower yields

Method used

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  • A kind of preparation method of triisooctyl phosphate
  • A kind of preparation method of triisooctyl phosphate
  • A kind of preparation method of triisooctyl phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0017] A 250 mL four necked round bottom flask equipped with a mechanical stirrer, constant pressure funnel, thermometer, condenser, and vacuum connection with control valve was placed in the ultrasonic apparatus. Nitrogen purging, isooctyl alcohol (148.2g, 1.14mol) is dropped in the flask, stirs, magnesium chloride (0.25g, 0.005g / g phosphorus oxychloride), then drops into phosphorus oxychloride (50g, 0.3257mol) to constant Press the funnel, pull vacuum, turn on the ultrasonic instrument, cool to 20°C, start to slowly add phosphorus oxychloride dropwise, the system exothermic obviously. After dropping, keep the temperature for 1 hour, slowly raise the temperature to 40°C, keep the temperature for 1 hour, and finally raise the temperature to 60°C, and keep the temperature until the end of the reaction. According to gas chromatography analysis, the content of chloroisooctane is 0.3483%. The control conditions in the reaction are shown in Table 1-1, and the gas chromatography an...

Embodiment 2

[0026] A 250 mL four necked round bottom flask equipped with a mechanical stirrer, constant pressure funnel, thermometer, condenser, and vacuum connection with control valve was placed in the ultrasonic apparatus. Nitrogen purging, phosphorus oxychloride (50g, 0.3257mol) was dropped into the constant pressure funnel, then isooctyl alcohol (156.7g, 1.2052mol), magnesium chloride (0.25g, 0.005g / g phosphorus oxychloride) was dropped into the flask Inside, stirring, vacuuming, turning on the ultrasonic instrument, cooling to 10°C, and slowly adding phosphorus oxychloride dropwise, the system exothermic obviously. After dropping, keep the temperature for 1 hour, slowly raise the temperature to 40°C, keep the temperature for 1 hour, and finally raise the temperature to 60°C, and keep the temperature until the end of the reaction. According to gas chromatography analysis, the content of chloroisooctane is 0.3494%. The control conditions of the reaction are shown in Table 2-1, and th...

Embodiment 3

[0033] A 250 mL four necked round bottom flask equipped with a mechanical stirrer, constant pressure funnel, thermometer, condenser, and vacuum connection with control valve was placed in the ultrasonic apparatus. Nitrogen purging, phosphorus oxychloride (50g, 0.3257mol) was dropped into the constant pressure funnel, then isooctyl alcohol (169.4g, 1.3029mol), magnesium chloride (0.25g, 0.005g / g phosphorus oxychloride) was dropped into In the flask, stir, pull vacuum, turn on the ultrasonic instrument, cool to 10°C, start to slowly add phosphorus oxychloride dropwise, and the system exotherms obviously. After dropping, keep the temperature for 1 hour, slowly raise the temperature to 40°C, keep the temperature for 1 hour, and finally raise the temperature to 60°C, and keep the temperature until the end of the reaction. According to gas chromatography analysis, the content of chlorinated isooctane is 0.3496%. The control conditions in the reaction are shown in Table 3-1. The gas ...

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Abstract

The invention provides a preparation method of tri-iso-octyl phosphate, and in particular relates to a method of utilizing phosphorus oxychloride and isooctyl alcohol under negative pressure and simultaneously carrying out ultrasonic-assisted chlorine hydride gas removal to prepare tri-iso-octyl phosphate. The invention utilizes the method of ultrasonic-assisted chlorine hydride gas removal to prepare tri-iso-octyl phosphate, under the action of ultrasonic wave, violent impact occur between liquid particles, thus being conducive to accelerated reaction. Also, after ultrasonic wave acts on the reaction feed liquid, a lot of small bubbles can be produced, tensile stress can appear locally in the liquid so as to form negative pressure, the pressure reduction brings about supersaturation of gas originally dissolved in the feed liquid, so that the gas escapes from the liquid to form bubbles, and then by means of vacuum pumping and under an ultrasonic assisted condition, the escaped hydrogen chloride gas can break away directly, thus greatly reducing the generation of the byproduct iso-octane chloride. The method not only improves the reaction yield, but also reduces environmental pollution, and saves the production cost.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of triisooctyl phosphate, which comprises phosphorus oxychloride and isooctyl alcohol under negative pressure conditions, and utilizes the method of ultrasonic-assisted dehydrochlorination gas to prepare triisooctyl phosphate ester. Background technique [0002] A large amount of hydrogen chloride gas is produced in the process of preparing triisooctyl phosphate, and hydrogen chloride easily generates chloroisooctane with components in the reaction solution. The recovery of chloroisooctane is relatively difficult, which increases the cost and pollutes the environment. The by-product chloroisooctane produced by the current preparation technology is high and the yield is low. Patents CN 105503941 A and CN 104592294 A provide dropwise addition of phosphorus oxychloride under normal pressure, and the hydrogen chloride gas produced by the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/11
CPCY02P20/584
Inventor 沈高波
Owner ZHEJIANG WANSHENG
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