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Comprehensive recycling method of organic phosphine production by-product phosphorus-containing composite salt

A technology of compound salt and hydrochloric acid, applied in the field of comprehensive utilization of phosphorus-containing compound salt, can solve problems such as failure to meet standard requirements, program errors, pollution, etc., and achieve the effect of solving comprehensive utilization problems, low recovery cost, and efficient recovery

Active Publication Date: 2021-03-26
HONGHU YITAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has been verified and indeed can separate sodium chloride and aluminum chloride, yet, there is an error in the reported scheme of this patent, specifically, in its step (1), what obtain at first is not aluminum chloride hexahydrate, but It is sodium chloride, and the sodium chloride and aluminum chloride finally obtained cannot meet the standard requirements due to the pollution from phosphorus-containing compounds in the solid residual mother liquor.
[0011] In summary, in the prior art, the use of the compound salt produced in the production process of methyl dichlorophosphine cannot be fully and effectively used, and some utilization methods still have problems such as complicated process and high difficulty in control

Method used

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  • Comprehensive recycling method of organic phosphine production by-product phosphorus-containing composite salt
  • Comprehensive recycling method of organic phosphine production by-product phosphorus-containing composite salt
  • Comprehensive recycling method of organic phosphine production by-product phosphorus-containing composite salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0086] This example provides a kind of recycling method of phosphorus-containing compound salt, implements as follows:

[0087] S1. Weigh 1000 grams of the same batch of phosphorus-containing compound salt as the test sample, control the temperature, add in batches to 2100 grams of 4% hydrochloric acid solution containing 0.5 grams of azobisisobutyronitrile, and simultaneously add cyclohexene 52 gram, keep system temperature about 80-85 degrees centigrade in the adding process, obtain the first mixture, and the aforementioned reaction equation involved is as follows:

[0088]

[0089] S2. Pass 105 grams of hydrogen chloride into the first mixture, continue to stir for 30 minutes, rise to 80 degrees Celsius, keep warm for 1 hour, filter, filter the cake with 650 grams of 20% hydrochloric acid, wash it, filter and dry to obtain 297.5 grams of sodium chloride Detecting sodium ion calibration sodium chloride content with ion chromatography is 99.56%, and ammonium molybdate spec...

Embodiment 2

[0093] This example provides a kind of recycling method of phosphorus-containing compound salt, implements as follows:

[0094] S1. Weigh 1000 grams of the same batch of phosphorus-containing compound salt as the test sample, control the temperature, and add it to 2100 grams of 3.5% hydrochloric acid solution in batches. When the phosphorus-containing compound salt is completely added, add 1 gram of di-tert-butyl peroxide , feed ethylene to keep the system pressure at 0.05MPa, until the system pressure does not change, continue to stir for 30 minutes, emit residual ethylene, and obtain the first mixture, the aforementioned reaction equation involved is as follows:

[0095]

[0096] S2. Pass 105 grams of hydrogen chloride into the first mixture, continue to stir for 30 minutes, rise to 75 degrees Celsius, keep warm for 1.5 hours, filter, filter the cake with 650 grams of 20% hydrochloric acid, wash it, filter and dry to obtain 296.7 grams of sodium chloride , it is 99.46% to...

Embodiment 3

[0101] The methylcyclohexylphosphinic acid (compound I-1) that embodiment 1 obtains is dissolved in 500 grams of water, adds sodium hydroxide to neutralize to neutrality, adds the solution that 66 grams of aluminum sulfate octadecahydrate is dissolved in 300 grams of water , stirred and reacted for 2 hours, filtered, washed with water, and dried to obtain 98.5 grams of aluminum methylcyclohexylphosphinate flame retardant, with a yield of 98.3%. The reaction equation is as follows:

[0102]

[0103] The resulting product was subjected to RSC thermal analysis, and the results were as follows: figure 1 Shown, this spectrogram and the RSC figure (such as figure 2 Shown) contrast, it can be seen that: the aluminum methylcyclohexyl hypophosphite obtained by the inventive method is consistent with the product of normal production.

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Abstract

The invention discloses a comprehensive recycling method of organic phosphine production by-product phosphorus-containing composite salt; the phosphorus-containing composite salt comprises sodium chloride, aluminum chloride composite salt and alkyl dichlorophosphine, and the method comprises the steps: reacting an olefin compound with alkyl dichlorophosphine in the phosphorus-containing compositesalt to generate a phosphorus-containing flame retardant or an intermediate thereof, and obtaining a mixture after reaction; and then gradually separating out sodium chloride and precipitates in the form of aluminum trichloride hydrate by increasing the content of hydrogen chloride in the system step by step in a grading manner, obtaining a mixture containing a phosphorus-containing flame retardant or an intermediate thereof, a small amount of aluminum chloride, sodium chloride and hydrochloric acid, distilling and concentrating, adding sodium hydroxide, filtering, acidifying and concentratingthe filtrate, extracting and purifying. According to the method, pure sodium chloride and pure aluminum chloride hydrate are obtained, the phosphorus-containing flame retardant or the intermediate ofthe phosphorus-containing flame retardant is obtained, the steps are clear, the function is definite, the method is simple and easy to control, and the problem of comprehensive utilization of composite salt in the production process of methyl dichlorophosphine is completely solved.

Description

technical field [0001] The invention relates to the technical field of recovery and utilization of phosphorus-containing by-products in the production process of organic phosphine intermediates, in particular to a method for comprehensive utilization of phosphorus-containing compound salts. Background technique [0002] Alkyl dichlorophosphine, also known as alkyl dichloride, is an important intermediate of organic phosphine compounds, especially methyl dichlorophosphine, which is the core of the synthesis of the herbicide glufosinate-ammonium intermediate, diethyl methylphosphonite raw material. At present, the mainstream production methods of methyl dichlorophosphine mainly include the following three methods: [0003] 1. Phosphorus trichloride and methane are obtained through a tubular reactor, condenser and fractionation device in the presence of a high-temperature and high-pressure catalyst to obtain methyl dichlorophosphine. This method is prone to deposits that lead ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C01F7/62C01F7/56C01D3/04
CPCC07F9/303C01D3/04C01F7/62C01F7/56C07F9/301C01D3/14C01B7/0706C01P2006/80Y02P20/584
Inventor 成贞辉曹凌云颜新天孙素丽蔡华胜
Owner HONGHU YITAI TECH CO LTD
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