Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid with double initiators

The technology of a trimethylpentyl group and a synthesis method is applied in the field of synthesizing bisphosphinic acid, which can solve the problem of high requirements on instruments and equipment, and achieve the effects of short reaction time, simple post-processing method, and non-toxic decomposition products.

Inactive Publication Date: 2011-12-07
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not require alkaline cleaning and acidification, which reduces the discharge of acid-base wastewater, but the reaction still needs to be completed in a high-pressure reactor, which requires high equipment.

Method used

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  • Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid with double initiators
  • Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid with double initiators
  • Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid with double initiators

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] Add 25.0g (0.28mol) sodium hypophosphite, 25.0g acetic acid and 209.5g (containing α-olefin 1.40mol) diisobutene (α-olefin content 75%), add 37.9g ​​(0.14mol) of azobisisobutylamidine hydrochloride and 15.9g (0.14mol) of 30% hydrogen peroxide, and heat to 60°C under vigorous stirring. After constant temperature reaction for 3 h, it was lowered to room temperature, allowed to stand for stratification, and the aqueous lower layer solution was separated. Wash the upper layer solution with water, add 100mL deionized water and wash 3 times. The β-olefin and a small amount of unreacted α-olefin were distilled off under reduced pressure to obtain 63.6 g of bis(2,4,4-trimethylpentyl)phosphinic acid with a yield of 78.2%. through 31 P-NMR analysis product is composed of:

[0024] Target product bis(2,4,4-trimethylpentyl)phosphinic acid 81.6%

[0025] Mono-substituted 2,4,4-trimethylpentylphosphonous acid 12.2%.

example 2

[0027] By the method of example 1, temperature of reaction is changed into 80 ℃, other methods are unchanged. Bis(2,4,4-trimethylpentyl)phosphinic acid 71.8g, yield 88.3%. through 31 P-NMR analysis product is composed of:

[0028] Target product bis(2,4,4-trimethylpentyl)phosphinic acid 91.3%

[0029] Mono-substituted 2,4,4-trimethylpentylphosphonous acid 5.9%.

example 3

[0031] By the method of example 1, temperature of reaction is changed into 100 ℃, other methods are unchanged. Bis(2,4,4-trimethylpentyl)phosphinic acid 67.6g, yield 83.1%. through 31 P-NMR analysis product is composed of:

[0032] Target product bis(2,4,4-trimethylpentyl)phosphinic acid 86.2%

[0033] Mono-substituted 2,4,4-trimethylpentylphosphonous acid 7.6%.

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Abstract

The invention relates to a method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid. The method adopts sodium hypophosphite and diisobutylene as the raw materials, and employs 2, 2'-azobis(2-methylpropionamidine) dihydrochloride and hydrogen peroxide as the radical initiators. With the steps of heating under violent stirring, a period of reaction at a constant temperature, liquid separation, organic phase washing, and vacuum distillation, the object product bis(2,4,4-trimethylpentyl) phosphinic acid can be obtained. The method provided in the invention has the advantages of short reaction time, high conversion rate, simple post-treatment method and atmospheric reaction, etc.

Description

technical field [0001] The invention relates to a method for synthesizing bis(2,4,4-trimethylpentyl)phosphinic acid. technical background [0002] Bis(2,4,4-trimethylpentyl)phosphinic acid is an extractant for acidic non-ferrous metals, which is excellent in the separation of cobalt and nickel. Its structure is as follows: [0003] [0004] There are multiple synthetic methods of two (2,4,4-trimethylpentyl) phosphinic acid, one of which is the method of adding and reoxidizing diisobutylene and phosphine free radicals reported by U.S. Patent 4,374,780 (1983) : [0005] [0006] This method is a two-step reaction, and the raw materials include toxic and flammable phosphine gas and hydrogen peroxide, a strong oxidant, which requires high equipment and personnel protection and is not conducive to large-scale industrial production. [0007] The other is the one-step method of the addition of diisobutylene and hypophosphorous acid free radicals reported by U.S. Patent 2006...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 王晓季陈振华吕常山刘东旺
Owner JIANGXI SCI & TECH NORMAL UNIV
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