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A method for synthesizing methyl phosphorus dichloride based on carbon microsphere-supported iron-nickel-cerium catalyst

A technology of methyl phosphorus dichloride and carbon microspheres, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., and can solve problems such as few researches, high reaction temperature, and cumbersome separation operations

Active Publication Date: 2021-12-14
潍坊新绿化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The gas phase method has significant advantages in terms of economic cost, and is the preferred method for the industrialization of methyl phosphorus dichloride. There are not many domestic researches. The breakthrough point is to develop a new catalyst that can efficiently catalyze the reaction between methane and phosphorus trichloride at a lower temperature. Chinese patent CN112409406A discloses a series of halogenated hydrocarbon catalysts, methane and phosphorus trichloride synthesize methyl phosphorus dichloride at 450-600°C, but the reaction temperature is still high, and the conversion rate of phosphorus trichloride is relatively low, and Most of the halogenated hydrocarbon catalysts have a certain degree of toxicity, and the separation operation from the raw materials is relatively cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: A method for synthesizing methyl phosphorus dichloride based on carbon microsphere-supported iron-nickel-cerium catalyst

[0029] Include the following steps:

[0030] 1. Preparation of dipping solution

[0031] Weigh 500 grams of three salts of iron sulfate, nickel chloride and cerium sulfate according to the atomic molar ratio of iron, nickel and cerium of 12:7:1, and add deionized water while stirring to completely dissolve the three salts, and the solution is in a clear and transparent state. , to obtain an impregnation solution with a total mass concentration of three salts of 31%.

[0032] 2. Preparation of carbon microsphere-supported iron-nickel-cerium catalyst

[0033] Add carbon microspheres accounting for 30% of the total mass of the impregnation solution into the impregnation solution, impregnate for 36 hours at a stirring rate of 6000 rpm, filter out the carbon microspheres, rinse with deionized water for 3 times, and then put them in a vacuum ...

Embodiment 2

[0041] 1. Preparation of dipping solution

[0042] Weigh 500 grams of three salts of iron sulfate, nickel chloride and cerium sulfate according to the atomic molar ratio of iron, nickel and cerium of 25:24:1, and add deionized water while stirring to completely dissolve the three salts, and the solution is in a clear and transparent state. , to obtain an impregnation solution with a total mass concentration of three salts of 34%.

[0043] 2. Preparation of carbon microsphere-supported iron-nickel-cerium catalyst

[0044]Add carbon microspheres accounting for 20% of the total mass of the impregnating liquid into the impregnating liquid, impregnate for 26 hours at a stirring rate of 3000 rpm, filter out the carbon microspheres, rinse with deionized water for 3 times, and put them in a vacuum drying oven at 80°C Dry for 3 hours;

[0045] The carbon microspheres have a particle size of 100 microns, an internal pore size distribution of 5 to 15 nanometers, and a specific surface ...

Embodiment 3

[0052] 1. Preparation of dipping solution

[0053] Weigh 500 grams of iron sulfate, nickel chloride and cerium sulfate three salts according to the atomic molar ratio of iron, nickel and cerium of 65:27:8, and add deionized water while stirring, so that the three salts are completely dissolved, and the solution is in a clear and transparent state. , to obtain an impregnation solution with a total mass concentration of three salts of 32%.

[0054] 2. Preparation of carbon microsphere-supported iron-nickel-cerium catalyst

[0055] Add carbon microspheres accounting for 40% of the total mass of the impregnating liquid into the impregnating liquid, impregnate for 48 hours at a stirring rate of 7000 rpm, filter out the carbon microspheres, rinse with deionized water for 3 times, and put them in a vacuum drying oven at 80°C Dry for 3 hours;

[0056] The carbon microspheres have a particle size of 300 microns, an internal pore size distribution of 30-40 nanometers, and a specific s...

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Abstract

A method for synthesizing methyl phosphorus dichloride based on a carbon microsphere-supported iron-nickel-cerium catalyst, comprising preparation of an impregnation solution, preparation of a carbon microsphere-supported iron-nickel-cerium catalyst, and synthesis of methyl phosphorus dichloride; the synthesis method uses carbon Microsphere-supported iron-nickel-cerium catalyst, the three-element loading of iron-nickel-cerium accounts for 0.2~1% of the total mass of the carbon microsphere carrier, and the atomic molar ratio of iron-nickel-cerium loaded into the carbon microsphere is 49~62:29~48: 3~9. The reaction temperature of this method is low, 300~400℃, the conversion rate of phosphorus trichloride is 20.4~30.1%, the yield of methyl phosphorus dichloride is 94.6~97.5%, and the catalyst is solid, non-toxic and easy to separate from the reaction system. The service life is 2800~3400 hours, and each gram of carbon microsphere-supported iron nickel cerium catalyst can produce 3.6~6.5 kg of methyl phosphorus dichloride.

Description

technical field [0001] The invention relates to a method for synthesizing methyl phosphorus dichloride based on a carbon microsphere-supported iron-nickel-cerium catalyst, which belongs to the field of organic synthesis. Background technique [0002] Methyl phosphorus dichloride is one of the most basic compounds of organophosphorus chemical industry. It is widely used in the synthesis of pesticides, medicines, flame retardants and other chemicals. Especially in recent years, with the rapid market demand for the new high-efficiency herbicide glufosinate Growth, methyl phosphorus dichloride, as the most critical intermediate in the synthesis of glufosinate-ammonium, has a very broad market prospect. The pure product of methyl phosphorus dichloride is a colorless transparent liquid with a strong pungent smell. Its chemical properties are extremely active and it is easy to absorb water. When it interacts with water, it will exotherm violently and even burn. The cost of storage ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/52B01J23/83B01J37/02B01J37/18
CPCC07F9/52B01J23/83B01J37/0213B01J37/18
Inventor 赵焱槐波马骏张清堂郭贵臣
Owner 潍坊新绿化工有限公司