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Preparation method of tributyl phosphate

A technology of tributyl phosphate and n-butanol, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of low product yield recovery, environmental pollution, low reaction temperature and other issues, to achieve the effects of cheap price, safe storage, improved yield and purity

Inactive Publication Date: 2017-12-29
ZHANGJIAGANG SANLIAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Hydrogen chloride gas will be generated during the esterification reaction, and hydrogen chloride gas will pollute the environment. In order to inhibit the reaction of hydrogen chloride with phosphoric acid ester and alcohol, a higher vacuum degree and a very low reaction temperature are generally controlled, which will lead to product yield and alcohol recovery rate is low

Method used

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  • Preparation method of tributyl phosphate

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Embodiment 1

[0020] A kind of preparation method of tributyl phosphate described in the present embodiment, comprises the following steps:

[0021] (1) Add n-butanol, sodium metal and toluene to the reaction device in sequence, then stir and heat up to reflux to generate a mixed solution containing sodium butoxide; wherein, the hydrogen generated by the reaction is removed from the solvent toluene by the separator in the reaction device After separation, the reaction temperature is controlled at 28°C, and the stirring speed is 50r / min, and the reaction time is controlled at 2.3 hours; the molar mass ratio of n-butanol and sodium metal is 1.1: 1, and 100g solvent is added for every 1mol sodium metal;

[0022] (2) Cool the mixed solution containing sodium butoxide to 15°C, add phosphorus oxychloride dropwise to the reaction device within 30 minutes to carry out esterification reaction, and generate a mixed solution containing tributyl phosphate; the esterification reaction temperature Contro...

Embodiment 2

[0027] A kind of preparation method of tributyl phosphate described in the present embodiment, comprises the following steps:

[0028] (1) Add n-butanol, sodium metal and toluene to the reaction device in sequence, then stir and heat up to reflux to generate a mixed solution containing sodium butoxide; wherein, the hydrogen generated by the reaction is removed from the solvent toluene by the separator in the reaction device After separation, the reaction temperature is controlled at 30°C, and the stirring speed is 60r / min, and the reaction time is controlled at 2 hours; the molar mass ratio of n-butanol and sodium metal is 1.4: 0.8, and 97g solvent is added for every 1mol sodium metal;

[0029] (2) Cool the mixed solution containing sodium butoxide to 12°C, add phosphorus oxychloride dropwise to the reaction device within 30 minutes to carry out esterification reaction, and generate a mixed solution containing tributyl phosphate; the esterification reaction temperature Control...

Embodiment 3

[0033] A kind of preparation method of tributyl phosphate described in the present embodiment, comprises the following steps:

[0034] (1) Add n-butanol, sodium metal and toluene to the reaction device in sequence, then stir and heat up to reflux to generate a mixed solution containing sodium butoxide; wherein, the hydrogen generated by the reaction is removed from the solvent toluene by the separator in the reaction device After separation, the reaction temperature is controlled at 32°C, the stirring speed is 55r / min, and the reaction time is controlled at 1.8 hours; the molar mass ratio of n-butanol and sodium metal is 0.8: 1.2, and 103g solvent is added for every 1mol sodium metal;

[0035] (2) Cool the mixed solution containing sodium butoxide to 18°C, add phosphorus oxychloride dropwise to the reaction device within 30 minutes to carry out esterification reaction, and generate a mixed solution containing tributyl phosphate; the esterification reaction temperature Control ...

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Abstract

The invention discloses a preparation method of tributyl phosphate. The preparation method of tributyl phosphate comprises steps as follows: (1), n-butyl alcohol, metallic sodium and a solvent are added to a reaction device in sequence and are stirred and heated until reflux occurs, and a mixed solution containing sodium butoxide is produced; hydrogen produced in the reaction is separated out by a separator in the reaction device; (2), the mixed solution containing sodium butoxide is cooled to 15 DEG C plus or minus 3 DEG C, phosphorus oxychloride is dropwise added to the reaction device for an esterification reaction, and a mixed solution containing tributyl phosphate is produced; (3), the mixed solution containing tributyl phosphate is heated to 80 DEG C plus or minus 6 DEG C, subjected to thermal insulation for 1 h plus or minus 0.3 h and then cooled to 20 DEG C plus or minus 5 DEG C, filtering, pressure reducing, secondary washing and distillation for alcohol and solvent removal are performed, and tributyl phosphate is obtained. According to the preparation method, hydrogen chloride gas cannot be produced in the reaction process, the working environment is greatly improved, and besides, yield and purity of tributyl phosphate are effectively increased.

Description

technical field [0001] The invention relates to the technical field of chemical product production, in particular to a preparation method of tributyl phosphate. Background technique [0002] Tributyl phosphate is mainly used as lubricant, flotation agent, defoamer, emulsifier, stabilizer or extractant, for the separation of ferrous metals, the grouping and purification of rare earth elements, and the separation of rare earth and non-rare earth elements , Treatment of phenolic wastewater, etc. The current preparation method for preparing tributyl phosphate is the direct esterification synthesis of alcohol and phosphorus oxychloride under the catalysis of metal chloride, such as aluminum trichloride. Hydrogen chloride gas will be generated during the esterification reaction, and hydrogen chloride gas will pollute the environment. In order to inhibit the reaction of hydrogen chloride with phosphoric acid ester and alcohol, a higher vacuum degree and a very low reaction tempera...

Claims

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Application Information

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IPC IPC(8): C07F9/11
CPCC07F9/11
Inventor 程经顺倪建彬
Owner ZHANGJIAGANG SANLIAN CHEM TECH
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