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Method for producing dichlorophenylphosphine

A technology for producing phenylphosphorous dichloride and phenylphosphorous dichloride, which is applied in the fields of chemical instruments and methods, organic chemistry, and compounds of Group 5/15 elements of the periodic table, and can solve the problem of phenylphosphorous dichloride Problems such as low yield, inability to carry out industrialized production, and unsuitability for industrialized production have achieved the effects of shortening the production cycle, large cost advantages and environmental protection advantages, and solving the serious problems of three wastes

Inactive Publication Date: 2016-07-06
东营美利达新型材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The yield of phenylphosphorous dichloride prepared by the metal reagent method is low, and the reaction requires relatively high reaction conditions, which is not suitable for industrial production
[0022] Phenyl chloride catalytic synthesis, BiCl3 catalytic aryl compound method, phosgene reduction method and other methods to synthesize phenyl phosphorus dichloride, although the target product can be prepared, most of the yields are too low to be industrialized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: a kind of method of producing phenyl phosphorus dichloride that the present invention mentions, its preparation method is as follows:

[0038] (1) Add 1.5mol chlorobenzene and 1.2mol phosphorus trichloride to the mixing kettle, heat up to 70°C and stir to preheat;

[0039] (2) Use high-temperature heat transfer oil to preheat the tubular reactor at 350°C;

[0040] (3) Put elemental phosphorus into the metering tank and heat up to 80°C to melt;

[0041] (4) Preheat the variable temperature and pressure device to 80°C with hot water;

[0042] (5) Steps (1) (2) (3) (4) After the temperature rises to the process temperature, use a metering pump to pump 1.0mol of the mixture of elemental phosphorus, chlorobenzene and phosphorus trichloride into the tubular reactor according to the process ratio Carry out the heat preservation cycle reaction for 6 hours, the reaction temperature is 350°C, and the pressure is 3.0MPa;

[0043] (6) After the reaction in step (5)...

Embodiment 2

[0044] Embodiment 2, a kind of method for producing phenyl phosphorus dichloride that the present invention mentions, its preparation method is as follows:

[0045] (1) Add 1.5mol chlorobenzene and 1.2mol phosphorus trichloride to the mixing kettle, heat up to 70°C and stir to preheat;

[0046] (2) Use high-temperature heat transfer oil to preheat the tubular reactor at 330°C;

[0047] (3) Put elemental phosphorus into the metering tank and heat up to 80°C to melt;

[0048] (4) Preheat the variable temperature and pressure device to 80°C with hot water;

[0049](5) Steps (1) (2) (3) (4) After the temperature rises to the process temperature, use a metering pump to pump 1.0mol of the mixture of elemental phosphorus, chlorobenzene and phosphorus trichloride into the tubular reactor according to the process ratio Carry out heat preservation cycle reaction for 6 hours, the reaction temperature is 330°C, and the pressure is 3.0MPa;

[0050] (6) After the reaction in step (5), th...

Embodiment 3

[0051] Embodiment 3, a kind of method of producing phenyl phosphorus dichloride that the present invention mentions, its preparation method is as follows:

[0052] (1) Add 1.5mol chlorobenzene and 1.2mol phosphorus trichloride to the mixing kettle, heat up to 70°C and stir to preheat;

[0053] (2) Use high-temperature heat transfer oil to preheat the tubular reactor at 350°C;

[0054] (3) Put elemental phosphorus into the metering tank and heat up to 80°C to melt;

[0055] (4) Preheat the variable temperature and pressure device to 80°C with hot water;

[0056] (5) Steps (1) (2) (3) (4) After the temperature rises to the process temperature, use a metering pump to pump 1.0mol of the mixture of elemental phosphorus, chlorobenzene and phosphorus trichloride into the tubular reactor according to the process ratio Carry out heat preservation cycle reaction for 6 hours, the reaction temperature is 350°C, and the pressure is 4.0MPa;

[0057] (6) After the reaction in step (5), th...

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Abstract

The present invention relates to a kind of method of producing phenyl phosphorus dichloride. Its technical scheme is: use chlorinated benzene, elemental phosphorus, and phosphorus trichloride as raw materials, and adopt reaction in a tubular reactor to prepare phenylphosphorus dichloride. The reaction equation is as follows: P 4 + 6C 6 h 5 Cl + 2PCl=6C 6 h 5 PCl. The beneficial effect is: since the main reaction of this method is carried out in a tubular reactor, without using a catalyst, the materials can directly reach the reaction conditions according to the ratio for rapid reaction, shorten the production cycle, and avoid the generation of a large number of by-products; at the same time It solves the potential safety hazards caused by high-temperature and high-pressure reactions in the past by using autoclaves; and there is no waste gas, waste residue, and waste water in the production process. Compared with the current process for preparing phenylphosphorus dichloride, it has greater cost advantages and environmental protection advantages.

Description

technical field [0001] The present invention relates to a kind of method of producing phenyl phosphorus dichloride. Background technique [0002] Phenylphosphine dichloride (English Dichlorophenylphosphine referred to as BPD, DCPP) is also known as dichlorophosphine benzene, phenyl dichlorophosphine, dichlorophenylphosphine, phenyl dichloride phosphine (DCPP), dichlorophenyl Phosphine is a colorless to light yellow transparent liquid at room temperature. It is an important chemical intermediate, which can be derived from many kinds of chemical products. It can be used as plasticizer, flame retardant, pesticide intermediate, paint compound, defoamer, antioxidant, photoinitiator, stabilizer, insecticide Agents, catalysts, high-pressure lubricants, and paint forming agents. The two chlorine atoms in the molecule are chemically active and can react with alcohols, phenols, aldehydes, amines, oxygen, sulfur, and halogens to prepare other organic phosphorus compounds. It can be m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/52
CPCC07F9/52
Inventor 张桂新郭庆张华
Owner 东营美利达新型材料科技有限公司
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