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The synthetic method of dimethyl heptyl methylphosphonate

A technology of dimethyl heptyl methyl phosphonate and dimethyl methyl phosphonate, which is applied in the field of preparation of organophosphorus compounds, can solve problems such as difficulty in raw material metering, achieve reduction of various side reactions, high yield, and reduce equipment The effect of investment

Active Publication Date: 2017-01-25
洛阳市三诺化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In order to solve the above technical problems, the present invention provides a method that can solve the difficult problem of raw material measurement in the current process and the safety problems caused by the use of high-pressure reactors, thereby reducing production costs, and the operation process is simple, the output and yield are high, and it is suitable for industrialization. The synthetic method of the methylheptyl methylphosphonate produced

Method used

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  • The synthetic method of dimethyl heptyl methylphosphonate
  • The synthetic method of dimethyl heptyl methylphosphonate

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Embodiment 1

[0023] The method for synthesizing dimethylheptyl methylphosphonate of the present invention includes the following steps:

[0024] A. Add the acyl chlorination reagent to the reaction vessel. The acyl chlorination reagent is one of thionyl chloride, phosphorus pentachloride, and triphosgene. Add dimethyl methylphosphonate (DMMP) dropwise to the reaction vessel at room temperature. In the acyl chlorination reagent, with mol as the unit of measurement, the dosage of the acyl chlorination reagent is 2 times or 2.5 times or 3 times or 3.5 times or 4 times or 4.5 times or 5 times that of dimethyl methylphosphonate (DMMP), and Add a catalytic amount of catalyst, the catalyst is N,N-disubstituted formamide or N-containing aromatic heterocyclic ring or N-substituted N-containing aromatic heterocyclic ring or tertiary amine. Stir uniformly at room temperature, and then raise the temperature in the reaction vessel to 60 ℃ or 150℃, heat preservation and reaction for 1.5h or 2.5h or 2.5h, t...

Embodiment 2

[0029] The method for synthesizing dimethylheptyl methylphosphonate of the present invention includes the following steps:

[0030] (1) Acid chlorination reaction: Add a mixture of 124.08g (1mol) of dimethyl methylphosphonate and 0.8g of pyridine (0.01mol) to 520.6gPCl at 20°C. 5 (2.5mol), keep at room temperature and stir for 1 hour, warm to 80°C, keep reaction for 2 hours, collect the substance with boiling point 56-57°C / 14mmHg by vacuum distillation to obtain methylphosphonic dichloride, yield 94.2%, purity 98.1%.

[0031] (2) Esterification reaction: Under stirring, 14.9g methylphosphonic dichloride (0.1mol) was slowly added to 65.1g secondary octanol (0.5mol), the generated HCl gas was absorbed by lye, and the generated The methyl chloride is collected. React at room temperature (about 30°C) for 45 minutes, then at 55°C for 1.5 hours, and finally at 85°C for 2 hours.

[0032] (3) Post-treatment: the reaction solution was cooled to room temperature, washed with water to neutrali...

Embodiment 3

[0036] The method for synthesizing dimethylheptyl methylphosphonate of the present invention includes the following steps:

[0037] (1) Chlorination reaction: Add a mixture of 124.08g of dimethyl methylphosphonate (1mol) and 0.73g of DMF (0.01mol) slowly dropwise to 297.5g of thionyl chloride (2.5mol), and heat to reflux, After keeping the temperature for 4 hours and cooling the reaction liquid, the substance with the boiling point of 56-57° C. / 14mmHg is collected by vacuum distillation to obtain methylphosphonic dichloride with a yield of 96.4% and a purity of 98.5%.

[0038] (2) Esterification reaction: Under stirring, 14.9g methylphosphonic dichloride (0.1mol) is slowly added to 78.1g secondary octanol (0.6mol), the generated HCl gas is absorbed by lye, and the generated The methyl chloride is collected. React at room temperature (about 30°C) for 45 minutes, then at 55°C for 1.5 hours, and finally at 85°C for 2 hours.

[0039] (3) Post-treatment: the reaction solution was cooled...

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Abstract

The invention relates to a synthesis method of dimethylheptyl methylphosphonate, and aims to solve the difficulty in raw material measurement and the safety problem caused by the use of the high-pressure reaction kettle in the existing technique, thereby lowering the production cost. The invention has the advantages of simple operating procedure, high output and high yield, and is suitable for industrial production. The method comprises the following steps: adding an acyl-chlorination reagent into a reaction vessel, wherein the acyl-chlorination reagent is thionyl chloride, phosphorous pentachloride or triphosgene; dropwisely adding dimethyl methyl phosphonate (DMMP) into the acyl-chlorination reagent at room temperature and adding catalytic amount of catalyst, wherein the consumption of the acyl-chlorination reagent is 2-5 times of the DMMP (0.6-1.5 times for triphosgene) on mol basis, and the catalyst is N,N-di-substituted-formamide or N-containing aromatic heterocyclic ring or N-substituted N-containing aromatic heterocyclic ring or tertiary amine; and uniformly stirring at room temperature.

Description

Technical field [0001] The invention belongs to the field of organophosphorus compound preparation, and specifically relates to a method for synthesizing dimethyl heptyl methylphosphonate. Background technique [0002] Dimethylheptyl methylphosphonate (trade name: P350) is a widely used high-efficiency neutral organic phosphorus extractant for the extraction and separation of rare earth, uranium-thorium, cobalt-nickel and scandium. Its structural formula is as follows: [0003] [0004] At present, the general synthetic method for dimethylheptyl methylphosphonate is to react methyl chloride, phosphorus trichloride, and aluminum trichloride in an autoclave to form a methyl compound, and then sec Obtained by alcoholysis, the synthetic route is shown below. [0005] CH 3 Cl+PCl 3 +AlCl 3 →[CH 3 PCl 3 ] + [AlCl 4 ] - [0006] [CH 3 PCl 3 ] + [AlCl 4 ] - +3ROH→CH 3 P(O)(OR) 2 [0007] R=C 6 H 13 CH(CH 3 )- [0008] The key to this route is the synthesis of the intermediate methyl compound. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40
Inventor 王亚涛杨晓亮刘麦女王丽娟李亚利
Owner 洛阳市三诺化工有限公司
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