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Method for preparing 0,0-di(2-ethylhexyl)-2-ethylhexyl phosphonate

A technology of hexylphosphonate and ethylhexyl, applied in the field of 0, can solve the problems of strong corrosiveness of raw materials, cumbersome processing process, difficult process control, etc., and achieve the effects of reducing reaction temperature, reducing reaction procedures and reducing production cost.

Active Publication Date: 2015-05-20
洛阳市三诺化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantages of strong corrosiveness of raw materials (strong alkali), cumbersome treatment process, many by-products, difficult process control (blasting), etc.

Method used

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  • Method for preparing 0,0-di(2-ethylhexyl)-2-ethylhexyl phosphonate
  • Method for preparing 0,0-di(2-ethylhexyl)-2-ethylhexyl phosphonate
  • Method for preparing 0,0-di(2-ethylhexyl)-2-ethylhexyl phosphonate

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Experimental program
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Effect test

Embodiment 1

[0034] The preparation method of 0,0-two (2-ethylhexyl)-2-ethylhexylphosphonate of the present invention, it comprises the steps:

[0035] A, 77 parts by weight of toluene, 20.2 parts by weight of isooctyl alcohol, and 15.2 parts by weight of dry triethylamine are placed in the reaction vessel, then the materials in the reaction vessel are stirred, and then the materials in the reaction vessel are heated up to 50°C or 55°C or 60°C or 65°C or 70°C or 75°C or 80°C, then add 6.85 parts by weight of phosphorus trichloride dropwise to the reaction vessel, the time for the addition is 80-100min, and the addition of trichloride After phosphorus removal, keep at 40°C or 45°C or 50°C or 55°C or 60°C or 65°C or 70°C or 75°C or 80°C or 85°C or 90°C for 1.5h-2h, then cool, filter, and the mother liquor is often The toluene was distilled under pressure to obtain the crude product, and the crude product was distilled under reduced pressure to obtain triisooctyl phosphite, and the yield of t...

Embodiment 2

[0040] The preparation method of 0,0-two (2-ethylhexyl)-2-ethylhexylphosphonate of the present invention, it comprises the steps:

[0041] (1) Synthesis of triisooctyl phosphite: add 70g toluene, 20.2g (0.155mol) isooctyl alcohol, and 15.2 g (0.15 mol) of dry triethylamine. Start stirring, and after heating up to 40-90° C., slowly add 6.85 g (0.05 mol) of phosphorus trichloride dropwise from a constant pressure dropping funnel. The molar ratio of isooctyl alcohol and phosphine trichloride is 3.1:1. After the addition, continue to react at this temperature for 1.5-2h, cool, filter, distill toluene from the mother liquor under normal pressure to obtain the crude product, and distill the crude product under reduced pressure to obtain sub Tri-isooctyl phosphate, yield 96%.

[0042](2) Synthesis of 0,0-di(2-ethylhexyl)-2-ethylhexylphosphonate: 0.78g (0.005mol, 0.125eqv) of bromoisoctane, triphosphite 16.7g (0.04mol, 1eqv) of isooctyl ester and 1.48g (0.004mol, 0.1eqv) of tetrabu...

Embodiment 3

[0044] The preparation method of 0,0-two (2-ethylhexyl)-2-ethylhexylphosphonate of the present invention, it comprises the steps:

[0045] (1) Synthesis of triisooctyl phosphite: add 70g toluene, 20.2g isooctyl alcohol, and 11.9g (0.15 mol) dry pyridine. Stirring was started, and after the temperature was raised to 55° C., 6.85 g (0.05 mol) of phosphorus trichloride was slowly added dropwise from a constant pressure dropping funnel. After the addition, continue to react at this temperature for 1.5 h, cool, filter, distill toluene from the mother liquor under atmospheric pressure to obtain a crude product, and distill the crude product under reduced pressure to obtain tri-isooctyl phosphite with a yield of 96.6%.

[0046] (2) Synthesis of 0,0-bis(2-ethylhexyl)-2-ethylhexylphosphonate: 0.78g (0.005mol) of bromoisoctane and triisooctyl phosphite were placed in a 100ml three-necked flask 16.7g (0.04mol), 1.29g (0.004mol) of tetrabutylammonium bromide, reacted overnight at a temp...

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Abstract

The invention relates to a method for preparing 0,0-di(2-ethylhexyl)-2-ethylhexyl phosphonate, which aims to reduce the reaction temperature, shorten the reaction procedure and simplify the post treatment process so as to reduce the production cost and is easy to operate, high in yield and suitable for industrialized production. The method comprises the following steps of: putting 77 parts by weight of methylbenzene, 20.2 parts by weight of isooctanol and 15.2 parts by weight of dry triethylamine into a reaction container, stirring the materials in the reaction container, heating the materials in the reaction container to the temperature of between 40 and 90 DEG C, then dripping 6.85 parts by weight of phosphorus trichloride into the reaction container, keeping the temperature of between 40 and 90 DEG C for 1.5 to 2 hours, then cooling, filtering, distilling the methylbenzene from the mother solution under normal pressure to obtain a crude product, and distilling the crude product under reduced pressure, thus obtaining triisooctyl phosphite.

Description

technical field [0001] The invention belongs to the field of preparation of organic phosphorus compounds, in particular to a preparation method of 0,0-di(2-ethylhexyl)-2-ethylhexyl phosphonate. Background technique [0002] 0,0-bis(2-ethylhexyl)-2-ethylhexylphosphonate (structural formula as shown in Figure 2) is a synthetic organic phosphorus extractant 0-(2-ethylhexyl)-2-ethylhexylphosphonic acid Key intermediate of ester (trade name: P507). [0003] [0004] The above formula is the molecular structure of 0,0-bis(2-ethylhexyl)-2-ethylhexylphosphonate [0005] P507 is a highly efficient acidic organophosphorus extractant widely used at present. It is used for the separation of nickel-cobalt and the separation and purification of rare earth metals. Its structural formula is shown in Figure 3: [0006] [0007] The above formula is the molecular structure of 0-bis(2-ethylhexyl)-2-ethylhexylphosphonate. At present, the traditional method for synthesizing P507 is shown...

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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