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Environmentally-friendly synthesis method for phenylphosphonic dichloride

A technology of phenylphosphine dichloride and phosphorus trichloride, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, chemical recovery, etc. Regeneration, inability to directly separate and other problems, to achieve obvious environmental protection, low production costs, less product by-products

Inactive Publication Date: 2010-03-17
王忠卫
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current industrial synthesis is to use benzene and PCl 3 in anhydrous AlCl 3 Reaction synthesis under catalysis, the disadvantage of this reaction is that it needs to consume excess AlCl 3 , seriously pollute the environment; on the other hand, phenylphosphine dichloride and AlCl 3 Form a complex and cannot be separated directly. The current industrial product separation method is to first add a dissociating agent to the reaction mixture to dissociate the complex of phenylphosphine dichloride and aluminum trichloride, and then extract the benzene with an organic solvent. Based phosphine dichloride, the commonly used dissociating agents are sodium chloride or sodium chloride and quaternary ammonium salt, phosphorus oxychloride, pyridine, hexane oxide, phosphorus pentoxide, etc., these separation methods have catalysts that cannot be regenerated, Disadvantages such as complicated dissociation and extraction process and heavy environmental pollution

Method used

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  • Environmentally-friendly synthesis method for phenylphosphonic dichloride
  • Environmentally-friendly synthesis method for phenylphosphonic dichloride
  • Environmentally-friendly synthesis method for phenylphosphonic dichloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Ionic liquid [BuPy]Cl-AlCl 3 Preparation of (BuPy=N-butylpyridinium cation)

[0038] Install a stirrer on the reaction kettle, add 26.67g (0.2mole) of anhydrous AlCl under the protection of nitrogen 3 , added in batches (0.1 mole) n-butylpyridine chloride. After adding the quaternary ammonium salt, keep stirring at about 60°C for 3 hours to ensure the completion of the reaction, and obtain a transparent light brown [BuPy]Cl-AlCl 3 ionic liquid.

[0039] (2) Preparation of phenylphosphine dichloride

[0040] Install a stirrer and a hydrogen chloride absorption system on the reaction kettle, add the ionic liquid prepared above, 78g (1 mole) benzene, and 411.9g (3 mole) phosphorus trichloride, heat to reflux, and keep the reflux reaction for 18 hours. After the reaction is finished, cool to room temperature and let it stand. The solution is divided into two layers. The brown liquid in the lower layer is the ionic liquid layer, and the upper layer is a colorless c...

Embodiment 2

[0043] The reclaimed ionic liquid described in Example 1 is used instead of the catalyst used in Example 1, and phenylphosphine dichloride is prepared according to the method in Example 1. The yield in terms of benzene is 64%, and product analysis shows that phosphorus trichloride is contained in the product 1.2%, phenylphosphine dichloride 98.8%, the product does not contain other impurities.

Embodiment 3

[0045] (1) Ionic liquid [trEHAm]Cl-AlCl 3 Preparation of (trEHAm = hydrogenated triethylamine cation)

[0046]Install a stirrer on the reaction kettle, add 26.67g (0.2mole) of anhydrous AlCl under the protection of nitrogen 3 , Add 13.8g (0.1mole) triethylamine hydrochloride in batches. After adding the quaternary ammonium salt, keep stirring at about 120°C for 2 hours to ensure the completion of the reaction, and obtain a transparent and colorless [trEtHAm]Cl-AlCl 3 ionic liquid.

[0047] (2) Preparation of phenylphosphine dichloride

[0048] Install a stirrer and a hydrogen chloride absorption system on the reactor, add the ionic liquid prepared above, 78g (1mole) benzene, and 411.9g (3mole) phosphorus trichloride, heat to reflux, and keep the reflux reaction for 18 hours. After the reaction, cool to room temperature and let it stand, the solution is divided into two layers, the lower layer is a colorless transparent liquid, mainly containing unreacted benzene, phosphoru...

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Abstract

The invention provides an environmentally-friendly synthesis method for phenylphosphonic dichloride. Phosphorus trichloride and benzene used as raw materials are reacted under the catalytic action ofLewis acid ionic liquid; after the reaction is finished, the reaction solution is divided into two layers, wherein one layer is an ionic liquid layer, and the other layer is a mixed solution layer ofphenylphosphonic dichloride, benzene and phosphorus trichloride; through direct solution separation, the ionic liquid layer is extracted, and the extract and the mixed solution layer are combined andthen are distilled at normal pressure and distilled at reduced pressure to obtain a phenylphosphonic dichloride target product respectively; and the ionic liquid is reclaimed after evaporation at thenormal pressure and the reduced pressure for removing imprity. Compared with the traditional industrialized process, the method has the characteristics of little using amount of a catalyst, reclaimable catalyst, easy operation and control, low production cost, environmentally-friendly production process and the like, does not need a de-complexing step, and does not produce a large amount of wasteslag.

Description

technical field [0001] The invention relates to a synthesis method of phenylphosphine dichloride, in particular to an environment-friendly synthesis method of phenylphosphine dichloride, and belongs to the technical field of chemical industry. Background technique [0002] Phenylphosphine dichloride is an important organic intermediate and an important chemical raw material in industry. It is widely used in the synthesis of flame retardants, insecticides, stabilizers, plasticizers, and antioxidants. The current industrial synthesis is to use benzene and PCl 3 in anhydrous AlCl 3 Reaction synthesis under catalysis, the disadvantage of this reaction is that it needs to consume excess AlCl 3 , seriously pollute the environment; on the other hand, phenylphosphine dichloride and AlCl 3 Form a complex and cannot be separated directly. The current industrial product separation method is to first add a dissociating agent to the reaction mixture to dissociate the complex of phenyl...

Claims

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Application Information

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IPC IPC(8): C07F9/52
CPCY02P20/584
Inventor 王忠卫刘波李艳高军曹克广
Owner 王忠卫
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