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Method for preparing tris(2-cyanoethyl)phosphine

A technology of acetonitrile and phosphine, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of increased equipment costs and operating costs, increased environmental treatment burden, and high production costs problems, to achieve the effect of low cost, significant economic and environmental benefits, and cost savings

Inactive Publication Date: 2009-12-30
天津市朝日科贸有限公司
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AI Technical Summary

Problems solved by technology

[0004] 1. One of the reactants, phosphine gas, is prepared from elemental phosphorus or metal phosphide, which requires a set of special phosphine generation equipment, which makes the production cost higher due to the increase in equipment costs and operating costs
[0005] 2. In the process of preparing raw material gas phosphine, some solid waste residues are produced, which increases the burden of environmental treatment

Method used

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Examples

Experimental program
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Effect test

Embodiment Construction

[0028] The following is an example of the preparation of tris(2-cyanoethyl)phosphine according to the present invention.

[0029] 1. In a 10-liter pressure reactor with stirring and jacket, add 700ml of solvent acetonitrile and 80ml of catalyst potassium hydroxide with a concentration of 10ml / L in sequence;

[0030] 2. Stir evenly and feed N 2 Purging for 20 minutes and allowing the reaction to be carried out in an oxygen-free environment throughout;

[0031] 3. Under stirring, pass in phosphine gas to make the pressure in the reactor reach about 0.6Mpa, and continue stirring for 10 minutes;

[0032] 4. Put hot water in the jacket, stop heating after the temperature of the reaction material reaches 50°C;

[0033] 5. Add 330ml of acrylonitrile (about 266g, 5.0mol) dropwise through the feeding pump, and the dropwise addition time is about 2 hours. During this process, observe the changes in the temperature and pressure of the reaction system: the temperature and pressure exper...

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PUM

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Abstract

The invention discloses a method of using industrial tail gas phosphine in a process for producing sodium hypophosphite as a raw material gas to synthesize tris(2-cyanoethyl)phosphine. The method has the advantages that: (1) the industrial tail gas phosphine is adopted as the raw material gas, has low cost and obvious value added effect, belongs to resource cyclic utilization, and has remarkable economic benefit and environmental protection benefit; and (2) equipment related to production of the raw material gas is not required so as to further save the cost for the tris(2-cyanoethyl)phosphine.

Description

1. Technical field [0001] The invention relates to a preparation method of tris(2-cyanoethyl)phosphine. 2. Background technology [0002] Tris(2-cyanoethyl)phosphine is a carrier and reducing agent in the process of protein separation, transfer and recombination, and belongs to high-tech biochemical products. At the same time, this product is also an intermediate for the production of a new generation of environmentally friendly permanent flame retardants for pure cotton fabrics, and has broad application prospects. The conventional preparation method of three (2-cyanoethyl) phosphine has been reported (for example J.Am.chem.Soc, VoL81, 1959: 1103~1107), and its preparation method is: with element phosphorus or metal phosphide (such as Aluminum phosphide) etc. react with alkali to produce phosphine gas, and then use acetonitrile as solvent to make Michael addition reaction between phosphine gas and acrylonitrile under the action of basic catalyst to obtain one (2-cyanoethyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/50
Inventor 万忠发万忠生张伟民陈翔
Owner 天津市朝日科贸有限公司
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