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Synthetic method of high-purity asymmetrical dialkyl phosphinic acid

A technology of dialkyl phosphinic acid and monoalkyl phosphinic acid is applied in the field of preparation of organophosphorus compounds, and can solve the problem that extraction and separation of rare earths are still to be studied.

Active Publication Date: 2012-09-26
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The extraction and separation performance of this product for cobalt and nickel is better than that of Cyanex272, and the performance of extraction and separation of rare earths remains to be studied (Li Linyan, Xu Shengming, Cheng Changmei, Ju Zhongjun. A synthesis method of dialkylphosphinic acid. 2009. Publication No. CN 101475588A; Li Linyan, Xu Shengming, Ju Zhongjun, Zhang Zhang, Liao Fuhui, Li Guobao. Dialkyl Phosphinic Acids: Synthesis and Applications as Extraction for Nickel and Cobalt Separation. Transactions of Nonferrous Metals Society of China. 2010(splup, 1): 205-210)

Method used

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  • Synthetic method of high-purity asymmetrical dialkyl phosphinic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Synthesis of (n-hexyl)(1-isopropyl-2,2,4,4-tetramethylpentyl)phosphinic acid

[0029] (1) Synthesis of mono(1-isopropyl-2,2,4,4-tetramethylpentyl)phosphinic acid

[0030] according to figure 1 According to the synthetic route shown, 4.05g of dry sodium hypophosphite, 4.12g of glacial acetic acid, 19.14g of triisobutylene, and 0.37g of di-tert-butyl peroxide (DTBP) were weighed sequentially in a stainless steel airtight container lined with 40ml of polytetrafluoroethylene. In the reaction kettle, start magnetic stirring, and react at 135° C. for 15 hours. Cool down to room temperature, add 0.35g of DTBP, and react at 135°C for another 15h. After cooling down to room temperature, 0.35 g of DTBP was added, and the reaction was continued at 135° C. for 15 h. Dilute the product with 50ml of anhydrous ether and transfer it to a 250ml separatory funnel, wash twice with 30ml and 20ml of deionized water, add 30ml of 4% NaOH solution to shake, let stand, the solution is divid...

Embodiment 2

[0034] Synthesis of (3,3-dimethylbutyl)(1-isopropyl-2,2,4,4-tetramethylpentyl)phosphinic acid

[0035] according to figure 1 According to the synthetic route shown, weigh 4.72g of the above-mentioned mono(1-isopropyl-2,2,4,4-tetramethylpentyl)phosphinic acid, 4.35g of 3,3-dimethyl-1-butene g, 2.57 g of propionic acid, and 0.38 g of azobisisobutyronitrile (AIBN) were placed in a stainless steel airtight reaction kettle lined with 20 ml of polytetrafluoroethylene, magnetic stirring was started, and the reaction was carried out at 90 ° C for 15 h. Cool down to room temperature, add 0.33g of AIBN, react at 90°C for another 15h, and cool down to room temperature. Add 0.38g of AIBN, react at 90°C for 15h, and cool down to room temperature. The product was diluted with 30ml n-hexane, washed twice with deionized water (20ml*2), washed twice with 4% NaOH solution (30ml*2), 10% H 2 SO 4 Acidify and wash twice (20ml*2). The n-hexane phase was washed three times with saturated brine...

Embodiment 3

[0037] Synthesis of (cyclooctyl)(1-decyl)phosphinic acid

[0038] (1) Synthesis of monocyclic octylphosphinic acid

[0039] according to figure 1 According to the synthetic route shown, 4.05g of dry sodium hypophosphite, 5ml of concentrated hydrochloric acid, 15.91g of cyclooctene, 0.22g of DTBP, and 0.11g of benzoyl peroxide (BPO) were weighed sequentially in 40ml of polytetrafluoroethylene. In a lined stainless steel airtight reaction kettle, start magnetic stirring, and react at 135°C for 15h. Cool down to room temperature, add DTBP 0.25g, BPO 0.08g, and react at 135°C for 15h. After cooling down to room temperature, 0.26 g of DTBP and 0.10 g of BPO were added, and the reaction was continued at 135° C. for 15 h. Dilute the product with 50ml of cyclohexane and transfer it to a 250ml separatory funnel, wash twice with 30ml and 20ml of deionized water, add 30ml of 4% NaOH solution for shaking, let it stand, and discard the organic phase. Then add 20ml of diethyl ether to ...

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Abstract

The invention discloses a synthetic method of high-purity asymmetrical dialkyl phosphinic acid, belonging to the technical field of synthesis of organic phosphorus compound. The synthetic method comprises the steps of carrying out addition reaction of free radials of large-steric-hindrance mono-olefine and phosphinic acid, so as to synthesize mono-alkyl phosphinic acid; and adding small steric-hindrance mono-olefine, and carrying out free radial addition reaction, so as to generate asymmetrical dialkyl phosphinic acid. The obtained product is subjected to washing by water, alkaline solution, acid solution, and saturated saline, drying and filtering, and then subjected to reduced pressure distillation or rotary evaporation so as to remove the un-reacted olefin, thereby obtaining high-purity asymmetrical dialkyl phosphinic acid. The synthetic method provided by the invention is simple in operation, mild in reaction condition, easy in implementation, and high in yield, and is suitable for mass production; and the product purification is easy, and the purity of the product is high.

Description

technical field [0001] The invention belongs to the field of preparation of organic phosphorus compounds, in particular to a method for synthesizing high-purity asymmetric dialkylphosphinic acid. Background technique [0002] Rare earth is an indispensable or alternative strategic resource for countries in the world to transform traditional industries, develop high-tech and cutting-edge defense technologies, and is known as the "vitamin of modern industry" and "treasure house of new materials". my country is a country rich in rare earth resources, with rare earth reserves accounting for 36% of the world's total, and heavy rare earth resources accounting for 90% of the world's total reserves. With the invention of sulfuric acid intensified roasting process, the establishment and application of rare earth cascade extraction theory, and the large-scale production of P507 extractant with domestic raw materials, my country has become a major producer of rare earths. Advanced tech...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 王俊莲徐盛明李晶李林艳徐刚王学军
Owner TSINGHUA UNIV
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