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A kind of preparation method of dimethyl heptyl methylphosphonate

A technology of dimethyl heptyl methyl phosphonate and diphenyl methyl phosphonate, which is applied in the field of organophosphorus fine chemicals, can solve the problems of route A, such as dangerous operation, high raw material price, and slow reaction speed, and achieve easy purification , short reaction time, less side effects

Active Publication Date: 2019-01-18
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Among them, the A route has the disadvantages of dangerous operation and high raw material price; the B route has the disadvantages of slow reaction speed and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1. Add 310.0g of diphenyl methylphosphonate and 292.5g of 2-octanol into a reactor with a volume of 500mL according to a molar ratio of 1:2.25, and then add 1g of sodium hydroxide to the reactor. After uniform stirring, 500 mL of reaction liquid was obtained; the amount of the catalyst added was 0.3% of the mass of the diphenyl methylphosphonate.

[0026] Step 2, feed nitrogen into the reactor in which the reaction solution is housed in step 1, start vacuuming until the pressure in the reactor is 7.5kPa after the nitrogen is full, repeat nitrogen filling and vacuuming 3 times, Raise the temperature of the reaction solution to 125°C at a heating rate of 0.5°C / min, and then react for 5 hours. During the reaction, vacuum was continuously applied to remove the phenol generated by the reaction;

[0027] Step 3, after the reaction described in step 2 ends, the product is cooled to room temperature, then washed to neutrality, and then distilled under reduced pressure to o...

Embodiment 2

[0029] Step 1. Add 155g of diphenyl methylphosphonate and 130g of 2-octanol into the reactor according to the molar ratio of 1:2, then add 0.15g of potassium hydroxide to the reactor, and stir evenly to obtain Reaction solution; the addition amount of the catalyst is 0.1% of the mass of the diphenyl methylphosphonate.

[0030] Step 2, feed nitrogen into the reactor in which the reaction solution is housed in step 1, and start vacuuming until the pressure in the reactor is 5kPa after the nitrogen is full, repeat nitrogen filling and vacuumizing 3 times, with Raise the temperature of the reaction solution to 50°C at a heating rate of 0.5°C / min, and then react for 6 hours. During the reaction, keep vacuuming to remove the phenol generated by the reaction;

[0031] Step 3, after the reaction described in step 2 ends, the product is cooled to room temperature, then washed to neutrality, and then distilled under reduced pressure to obtain dimethylheptyl methylphosphonate; the pressu...

Embodiment 3

[0033] Step 1. Add 620g of diphenyl methylphosphonate and 650g of 2-octanol into the reactor according to the molar ratio of 1:2.5, then add 18.6g of sodium carbonate to the reactor, and stir evenly to obtain the reaction liquid; the addition of the sodium carbonate is 3% of the quality of the diphenyl methyl phosphonate;

[0034] Step 2, feed helium into the reactor in which the reaction liquid is housed in step 1, and start vacuuming until the pressure in the reactor is 10kPa after the helium is full, after repeatedly filling nitrogen and vacuumizing 3 times , the temperature of the reaction solution was raised to 200°C at a heating rate of 0.5°C / min, and then reacted for 5 hours. During the reaction, vacuum was continued to remove the phenol generated by the reaction;

[0035] Step 3, after the reaction described in step 2 ends, the product is cooled to room temperature, then washed to neutrality, and then distilled under reduced pressure to obtain dimethylheptyl methylphos...

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Abstract

The invention discloses a preparation method of di-methyl-heptyl methyl phosphonate. The method comprises the steps of (1) adding diphenyl methyl phosphonate and 2-octanol to a reactor according to the molar ratio of 1:(2 to 2.5), then adding catalysts to the reactor, and uniformly stirring, so that reaction liquid is obtained; (2) leading inert gas to the reactor, vacuumizing after the reactor is filled with the inert gas, heating the reaction liquid to 50 DEG C to 200 DEG C for reaction for 4 h to 6 h at the same time, and continuously vacuumizing during reaction so as to remove phenol which is generated during reaction; (3) cooling products to room temperature after the reaction is finished, then washing with water to be neutral, then reducing pressure and distilling, so that the di-methyl-heptyl methyl phosphonate is obtained. The preparation method has the advantages of simple synthetic route, mild reaction conditions, short reaction time, less side reaction, high reaction yield and no discharge of etchant gas and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organophosphorus fine chemicals, and in particular relates to a preparation method of dimethylheptyl methylphosphonate. Background technique [0002] Dimethylheptyl methylphosphonate, chemical formula C 17 h 37 o 3 P, molecular weight 320.3, trade name P350, dimethylheptyl methylphosphonate is a neutral phosphorus extractant, light yellow transparent liquid, boiling point 120℃~122℃(26.66Pa), specific gravity 0.9148(25℃), Refractive index 1.4360, slightly soluble in water, easily soluble in kerosene, carbon tetrachloride, benzene and other organic solvents. Because the methyl group in the P350 molecule is directly connected to the phosphorus atom, the electron-pushing effect of the methyl group increases the electron cloud density of the P=0 bond, so it has a greater complexing ability than other organic phosphine extractants; It has good chemical stability and radiation performance. P350 has been wid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40
CPCC07F9/4075
Inventor 刘卫涛李文李潇李小安雷东卫王宪沛张立龙闫俊
Owner XIAN ORIGIN CHEM TECH
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