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Method for effectively inhibiting thermal decomposition of phosphorus trichloride in preparation process of monoalkyl phosphine dichloride

A technology of monoalkylphosphine dichloride and phosphorus trichloride, which is applied in the field of preparation of new monoalkylphosphine dichloride, and can solve the problems of thermal decomposition of phosphorus trichloride, flammability and explosion of elemental phosphorus, safety hazards, etc. problems, to achieve efficient inhibition of decomposition, suitable for large-scale industrial production, and excellent results

Inactive Publication Date: 2021-07-13
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the decomposition of phosphorus trichloride to produce toxic elemental phosphorus and chlorine gas, elemental phosphorus is flammable and explosive, and there is a great potential safety hazard
Basically all there is the problem of phosphorus trichloride thermal decomposition in the method of prior art

Method used

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  • Method for effectively inhibiting thermal decomposition of phosphorus trichloride in preparation process of monoalkyl phosphine dichloride
  • Method for effectively inhibiting thermal decomposition of phosphorus trichloride in preparation process of monoalkyl phosphine dichloride
  • Method for effectively inhibiting thermal decomposition of phosphorus trichloride in preparation process of monoalkyl phosphine dichloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The reaction was evaluated with a tubular reactor with a diameter of 3 cm and a length of 50 cm. The specific experimental process was as follows: phosphorus trichloride and monochlorobenzene were directly mixed, and injected into a 150 ° C vaporizer at a certain flow rate through a liquid feeding device. The gas, methane and air pass through the high-temperature heating reaction zone and then pass through a tubular cooler with a temperature between 130-160°C. The auxiliary agent is cooled and collected as a liquid. The separation yield exceeds 90%. The gaseous product is further separated by cyclone. The liquid mixture containing the product is obtained after treatment in the cooling section and the final distillation separation to obtain the target product. The liquid material was collected for analysis, and the reaction conditions and results are listed in Table 1 below.

Embodiment 2 to 8

[0033] The experiment was carried out in the same manner as in Example 1 except that the reaction was adjusted according to the reaction conditions in Table 1, and the results are shown in Table 1 below.

Embodiment 9 to 14

[0035] For comparison, the test was carried out in the same manner as in Example 1 except that the reaction was adjusted according to the reaction conditions in Table 1 (without adding chlorobenzene), and the results are shown in Table 1 below.

[0036] Table 1

[0037]

[0038] In addition, experiments have confirmed that the addition of air will significantly aggravate the decomposition of phosphorus trichloride. Comparative Examples 6 and 12 prove that in the presence of air, monochlorobenzene can also well inhibit the decomposition of phosphorus trichloride. Decomposition, indicating that under aerobic or anaerobic conditions, monochlorobenzene can play a good role in inhibiting the decomposition of phosphorus trichloride.

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Abstract

The invention discloses a method for effectively inhibiting thermal decomposition of phosphorus trichloride in the preparation process of monoalkyl phosphine dichloride. The method comprises the following steps: adding an auxiliary agent together with phosphorus trichloride in the preparation process of monoalkyl phosphine dichloride, wherein the auxiliary agent is a chlorobenzene aromatic compound, and the mass ratio of the auxiliary agent to phosphorus trichloride is 20: 1-0.1: 1. The method is simple and effective, and decomposition of phosphorus trichloride can be efficiently inhibited by adding a small amount of auxiliaries, so that the utilization rate and conversion rate of phosphorus trichloride are improved. Meanwhile, after the reaction is finished, thorough separation of the auxiliary agent can be realized by simply controlling the temperature of a reaction mixture. According to the method, the effect is excellent, the production cost is not greatly increased, and meanwhile, the addition of the auxiliary agent does not cause side reaction, so that the method is suitable for large-scale industrial production requirements.

Description

technical field [0001] The invention belongs to the field of industrial chemical synthesis, and in particular relates to a method for inhibiting the thermal decomposition of phosphorus trichloride in the preparation process of monoalkylphosphine dichloride, and a novel monoalkyl dichloride obtained therefrom. Preparation method of phosphine. Background technique [0002] Monoalkyl phosphine dichloride, especially methyl phosphine dichloride, is an important intermediate in the synthesis of organophosphorus compounds, which can be used to synthesize flame retardants, low-toxicity herbicides, etc. [0003] The relatively mature route for synthesizing monoalkylphosphine dichloride at this stage is to use methane and phosphorus trichloride to carry out gas-phase reaction at high temperature to generate monoalkylphosphine dichloride in one step. For example, Chinese patent CN106117267A discloses a green synthesis method of methyl phosphine dichloride, which uses phosphorus penta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/52
CPCC07F9/52
Inventor 安增建郑可
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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