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Synthesis method of dimethylheptyl 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 measurement, achieve low equipment investment, high yield, and reduce equipment investment Effect

Active Publication Date: 2012-11-28
洛阳市三诺化工有限公司
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  • 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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  • Synthesis method of dimethylheptyl methylphosphonate
  • Synthesis method of dimethylheptyl methylphosphonate

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Embodiment 1

[0023] The synthetic method of methylheptyl phosphonate of the present invention may further comprise the steps:

[0024] A, the acyl chloride reagent is joined in the reaction vessel, and the acyl chloride reagent is a kind of in thionyl chloride, phosphorus pentachloride, triphosgene, and dimethyl methyl phosphonate (DMMP) is added dropwise to at room temperature In the acid chloride reagent, taking mol as the unit of measurement, the consumption of the acid chloride 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 heterocycle or N-substituted N-containing aromatic heterocycle or tertiary amine, stir evenly at room temperature, and then raise the temperature of the material in the reaction vessel to 60 ℃ or 150℃, keep warm for 1.5h or 2.5h or 2.5h, then distill under reduced pressure...

Embodiment 2

[0029] The synthetic method of methylheptyl phosphonate of the present invention may further comprise the steps:

[0030] (1) Acyl chloride reaction: Add a mixture of 124.08 g (1 mol) of dimethyl methylphosphonate and 0.8 g of pyridine (0.01 mol) dropwise to 520.6 g of PCl at 20°C 5 (2.5mol), keep stirring at room temperature for 1h, heat up to 80°C, keep warm for 2h, and collect the substance with a boiling point of 56-57°C / 14mmHg by distillation under reduced pressure to obtain methylphosphonodichloride with a yield of 94.2% and a purity of 98.1%.

[0031] (2) Esterification reaction: under stirring, slowly add 14.9g of methylphosphonic dichloride (0.1mol) into 65.1g of secondary octanol (0.5mol), the generated HCl gas is absorbed with lye, and the generated Chloromethane collection. First react at room temperature (about 30°C) for 45min, then react at 55°C for 1.5h, and finally react at 85°C for 2h.

[0032] (3) Post-treatment: the reaction solution was cooled to room tem...

Embodiment 3

[0036] The synthetic method of methylheptyl phosphonate of the present invention may further comprise the steps:

[0037](1) Acid chlorination reaction: Slowly add a mixture of 124.08g dimethyl methylphosphonate (1mol) and 0.73gDMF (0.01mol) dropwise to 297.5g thionyl chloride (2.5mol), and heat to reflux, After 4 hours of heat preservation, the reaction solution was cooled, and the substance with a boiling point of 56-57° C. / 14 mmHg was collected by distillation under reduced pressure to obtain methylphosphonic dichloride with a yield of 96.4% and a purity of 98.5%.

[0038] (2) Esterification: under stirring, slowly add 14.9g of methylphosphonic dichloride (0.1mol) into 78.1g of 2-octanol (0.6mol), the generated HCl gas is absorbed with lye, and the generated Chloromethane collection. First react at room temperature (about 30°C) for 45min, then react at 55°C for 1.5h, and finally react at 85°C for 2h.

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

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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 preparation of organic phosphorus compounds, in particular to a method for synthesizing dimethylheptyl methylphosphonate. Background technique [0002] Dimethylheptyl methylphosphonate (trade name: P350) is a highly efficient neutral organic phosphorus extractant widely used at present. It is used for the extraction and separation of rare earths, uranium-thorium, cobalt-nickel and scandium. Its structural formula is as follows: [0003] [0004] At present, the general synthetic method of dimethylheptyl methylphosphonate is to generate a methyl complex by reacting methyl chloride, phosphorus trichloride, and aluminum trichloride in an autoclave, and then carry out the compound by secondary octanol 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 ...

Claims

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Application Information

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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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