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Synthesis method for dichlorophenylphosphine oxide

A technology of phenylphosphine dichloride and a synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve complex unit operations, long production processes, environmental pollution, etc. problem, to achieve the effect of high product purity, low production cost and easy purification

Inactive Publication Date: 2013-06-26
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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Problems solved by technology

However, this method has a long production process, complex unit operations, more waste residues, and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Pretreatment of solid raw materials

[0026] Sodium chloride is ground finely to 160 meshes, 1.800kg (30.7mol) of sieved sodium chloride and 3.300kg (24.7mol) of aluminum trichloride are weighed, mixed evenly and added to the reactor.

[0027] (2) Synthesis of phenylphosphine dichloride

[0028] Add 8.600kg of phosphorus trichloride (62.5mol) into the reactor in (1), connect the reaction device, and stir at 50-60°C for 1 hour. Weigh 2.0kg of benzene (25mol), raise the temperature to 80°C, stir, reflux, add benzene to the reactor at a uniform speed, control for 1 hour to complete, after 5 hours of reaction, lower the temperature to 50°C, stop stirring, and stand Set aside for 0.5 hours, move the supernatant into a distiller, add 12.0 kg of phosphorus trichloride to the residue for extraction for 0.5 hours, move the supernatant into the same distiller, and extract three times in the same way. The distiller is heated, and the temperature is lower than 90° C. to disti...

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Abstract

The invention provides a synthesis method for dichlorophenylphosphine oxide, relating to a synthesis method for a catalyst for chemical industry. The synthesis method comprises the following steps of taking benzene and phosphorus trichloride as raw materials and simultaneously adding sodium chloride and alchlor as the catalyst, reacting so as to produce mixed liquor of the dichlorophenylphosphine oxide, benzene and the phosphorus trichloride and solid residue, processing the solid residue with extracting agent and mixing with the mixed liquor, thus obtaining the pure dichlorophenylphosphine oxide through distillation under normal pressure and reduced pressure. The catalyst AlCl3*XNaCl complex can be recycled. Compared with traditional method, the synthesis method has the characteristics that the operation steps are simple, the production time is short, decomplexing agent is added no more in the steps, the synthesis method is easy to operate and control, the production cost is low, and the production steps are environment-friendly, and the like.

Description

technical field [0001] The invention relates to a synthesis method of a chemical catalyst, in particular to a synthesis method of phenylphosphine dichloride. Background technique [0002] Phenylphosphine dichloride, also known as phenylphosphine dichloride, is one of the most important monomers for the synthesis of aromatic organic phosphine compounds, and is also used in the preparation of flame retardants, plasticizers, pesticides, nylon stabilizers, dyes, photosensitive Initiator intermediate. With the development of polymeric organic phosphine flame retardants, phenylphosphine dichloride, as one of the intermediates of flame retardants, has been further applied. At present, the low-temperature liquid phase method is commonly used in China. This route mainly uses phosphorus trichloride and benzene in the presence of catalyst aluminum trichloride to produce the complex of phenylphosphine dichloride and aluminum trichloride. Then use a decomplexing agent to replace the p...

Claims

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Application Information

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IPC IPC(8): C07F9/52
Inventor 范天博汤涛安贵奇刘云义
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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