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Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid under normal pressure

A technique for synthesizing trimethylpentyl under normal pressure, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve harsh reaction conditions, high equipment requirements, and long reaction time problems such as mild reaction conditions, shortened reaction time, and simple process

Inactive Publication Date: 2011-04-20
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis method and preparation process described in the literature and published patents are all required to be carried out in an autoclave, and the reaction time is long, the reaction conditions are harsh (pressure, inert environment, high temperature, etc.), and the equipment requirements are very high

Method used

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  • Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid under normal pressure
  • Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid under normal pressure
  • Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid under normal pressure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 50.0g (471mmol) of sodium hypophosphite, 50.0g (833mmol) of acetic acid and 211.40g (1413mmol) of diisobutylene (75%) in a 1000mL four-necked flask equipped with a mechanical stirrer, a thermometer, a condenser and a dropping funnel. , stirred, and dropwise added 3.09g (18.84mmol) of benzene solution of azobisisobutyronitrile from the dropping funnel at room temperature. The benzene solution of g (9.42mmol) azobisisobutyronitrile was added with an initiator every 2 hours. After reacting for 10 hours, the temperature was lowered to 50° C., washed with alkali, acidified, dried and vacuum rotary evaporated to obtain the product di(2,4,4-trimethylpentyl)phosphinic acid. The composition of the product is as follows:

[0023] 31 P-NMR analysis:

[0024] Target product di(2,4,4-trimethylpentyl)phosphinic acid 78%

[0025] Mono-substituted 2,4,4-trimethylpentylphosphonous acid 13.8%

[0026] Other components 8.2%.

Embodiment 2

[0028] According to the method of Example 1, the time interval for adding the initiator was changed to 1 hour, and the other methods were unchanged. The composition of the product is as follows:

[0029] 31 P-NMR analysis:

[0030] Target product bis(2,4,4-trimethylpentyl)phosphinic acid 88.9%

[0031] Mono-substituted 2,4,4-trimethylpentylphosphonous acid 6.4%

[0032] Other components 4.7%.

Embodiment 3

[0034] According to the method of Example 1, the time interval for adding the initiator was changed to 3 hours, and the other methods were unchanged. The composition of the product is as follows:

[0035] 31 P-NMR analysis:

[0036] Target product di(2,4,4-trimethylpentyl)phosphinic acid 71.4%

[0037] Mono-substituted 2,4,4-trimethylpentylphosphonous acid 17.5%

[0038] Other components 11.1%.

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Abstract

The invention discloses a method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid under normal pressure, which comprises: dissolving sodium hypophosphite in acetic acid; adding diisobutylene; dripping azodiisobutyronitrile into the solution under normal pressure and at room temperature; after the dripping is finished, heating till refluxing; reacting for 2 hours under a refluxing condition; dripping azodiisobutyronitrile once, and then dripping azodiisobutyronitrile every 1 to 3 hours; and finally, washing with alkali, acidifying, dewatering and performing vacuum evaporation by spinning to obtain the target product, namely bis(2,4,4-trimethylpentyl) phosphinic acid. Compared with the conventional method, the method has the advantages that: the reaction can be performed smoothly under normal temperature; the reaction time is reduced greatly; the reaction condition is mild; the bis(2,4,4-trimethylpentyl) phosphinic acid yield is high; the technical process is simple; and the like. In the method, the synthesis can be accomplished by one step, so the raw material waste and energy consumption, which are caused by synthesis by multiple steps, are reduced, and cost is reduced.

Description

technical field [0001] The invention relates to a method for synthesizing di(2,4,4-trimethylpentyl)phosphinic acid under normal pressure. technical background [0002] Bis(2,4,4-trimethylpentyl)phosphinic acid is a new type of extraction agent for acidic rare metals. It has excellent performance in the extraction of cobalt and nickel, and is an important chemical product. The structure is as follows: [0003] [0004] The method for the synthesis of two (2,4,4-trimethylpentyl) phosphinic acid of existing literature report mainly contains: 1. RORBERTSON A J. The patent No. of "is US4374780, and the patent application date is 1983 / 02 / 03. In the patent, diisobutene, phosphine and hydrogen peroxide are used as raw materials, and two steps of free radical addition and oxidation are carried out under catalyst and pressure conditions. Reaction method for synthesizing two (2,4,4-trimethylpentyl) phosphinic acid. [0005] In addition, Shiming Wo and Floryan De Campo in the titl...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 王晓季
Owner JIANGXI SCI & TECH NORMAL UNIV
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