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Method for synthesizing diphenyl phosphonium chloride

A technology of diphenylphosphine chloride and a synthesis method is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, chemical recovery, etc. Production and other problems, to achieve the effect of high product purity, low production cost and obvious environmental protection

Inactive Publication Date: 2013-02-27
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to overcome the technical defects of low product yield, high cost, serious environmental protection problems, and inability to produce large-scale production in the existing synthesis of diphenylphosphine chloride, the present invention provides a synthetic process route that is simple, easy to operate, and low in production cost. , little diphenylphosphine chloride synthetic method of ring pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] With [BuPy]Cl-AlCl 3 (BuPy=N-butylpyridinium cation) as an ionic liquid, the specific steps are as follows:

[0038] Step 1: Ionic liquid [BuPy]Cl-AlCl 3 Preparation of (BuPy=N-butylpyridinium cation)

[0039] Install a stirrer on the reaction kettle, add 26.67g (0.2 moles) of anhydrous AlCl under nitrogen protection 3 , Added 17.1 g (0.1 mol) of n-butylpyridine chloride in batches. 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.

[0040] The second step: the preparation of diphenylphosphine chloride

[0041] (1) Install a stirrer and a hydrogen chloride absorption system on the reaction kettle, add the ionic liquid prepared above, 234g (1 mole) of benzene, and 136.5 (1 mole) of phosphorus trichloride, heat to reflux, and keep the reflux reaction for 24 hours reaction.

[0042] (2) After the reaction, cool to room tempera...

Embodiment 2

[0047] The ionic liquid recovered in Example 1 was used instead of the catalyst used in Example 1, and the yield of diphenylphosphine chloride was 51% in terms of phosphorus trichloride, and the yield of phenylphosphine dichloride was 51%. rate 18%.

Embodiment 3

[0049] Example three with [Et 3 NH]Cl-AlCl 3 (Et 3 NH = hydrogenated triethylamine cation) ionic liquid as an example.

[0050] Step 1: Preparation of ionic liquid

[0051] 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 that the reaction is complete, and a transparent and colorless [Et 3 NH]Cl-AlCl3 ionic liquid.

[0052] The second step: the preparation of diphenylphosphine chloride

[0053] (1) Install a stirrer and a hydrogen chloride absorption system on the reactor, add the ionic liquid prepared above, 234g (1 mole) of benzene, and 136.5g (3 moles) of phosphorus trichloride, heat to reflux, and keep the reflux reaction for 24 hour response.

[0054] (2) After the reaction, cool to room temperature and let stand. The solution is divided into tw...

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Abstract

The invention discloses a method for synthesizing diphenyl phosphonium chloride. The method includes: performing reaction on raw materials of phosphorus trichloride and excessive benzene under catalyzing effect of Lewis acid ionic liquid, wherein after the reaction, the reaction liquid is divided into two layers, one layer is an ionic liquid layer, and the other layer is a mixed liquid layer. Through direct liquid separation, the ionic liquid layer is extracted, the extract liquor is mixed with the mixed liquid layer, and the mixture is respectively performed with normal pressure distillation and decompression distillation to obtain the target object diphenyl phosphonium chloride and byproduct phenyl phosphonium chloride. The ionic liquid is performed with normal pressure and decompression distillation so as to remove impurities and recover the diphenyl phosphonium chloride. Compared with the existing industrial process, the method has the advantages of being small in catalyst amount, requiring no decomplexing procedure, being easy to operate and control, not generating large amount of waste residue, being low in production cost, environment-friendly in production process and the like, and the catalyst is recoverable.

Description

technical field [0001] The invention relates to a synthesis method of organophosphorus compound diphenylphosphine chloride, which belongs to the technical field of organic chemical industry. Background technique [0002] Diphenylphosphine chloride is an important organophosphorus chemical product, which can be used in the production of photoinitiator TPO, diphenylphosphine oxide, catalyst, etc. in industry. The current industrial synthesis method is to use benzene and phosphorus trichloride as raw materials, react under the catalysis of anhydrous aluminum trichloride, and the diphenylphosphorous chloride generated is complexed with aluminum trichloride, by adding phosphorus oxychloride, dichloride Oxyhexane, crushed sodium chloride or potassium chloride react with aluminum chloride to dissociate diphenyl chloride. The disadvantage of this type of method is that the decomplexation process is troublesome, and a large amount of solid waste sensitive to water is generated. Sinc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/52
CPCY02P20/584
Inventor 王忠卫赵剑于青靳涛武清浴
Owner SHANDONG UNIV OF SCI & TECH
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