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Method for recycling triethylamine from production of propargite

A recovery method and technology for triethylamine, which are applied in the preparation of amino compounds from amines, purification/separation of amino compounds, and organic chemistry, etc., can solve the problems of not meeting the requirements of clean production, low material recovery rate, and high recovery cost. The effect of low energy consumption, low operating cost and convenient operation

Inactive Publication Date: 2011-05-04
QINGDAO HANSEN BIOLOGIC SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The material recovery rate of this method is low, about 85%, the equipment investment is large, the recovery cost is high, and there is still a large amount of triethylamine left in the waste water, which pollutes the environment and fails to meet the clean production requirements

Method used

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  • Method for recycling triethylamine from production of propargite

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Embodiment 1

[0023] (1) The recovery of triethylamine crude product: in the reactor of 1000L, add concentration and be 42% triethylamine hydrochloride waste water 700Kg, add weight purity under stirring and be 95% sodium hydroxide 105Kg; Be 65 ℃ at temperature, Atmospheric distillation for 1.5 hours gave crude triethylamine.

[0024] (2) Drying of triethylamine: in a 500L reaction kettle, add the crude product of triethylamine, and add 115Kg of sodium hydroxide with a weight purity of 95% under stirring; stir for 1 hour at a temperature of 55°C, and obtain a colorless and transparent product after being separated by a filter The triethylamine has a weight content of more than 99%, a water content of less than 0.5%, and a recovery rate of 98%. The triethylamine is directly used in the production of propargite.

[0025] (3) The residual solid in the drying kettle replaces the sodium hydroxide in (1), puts it into the distillation kettle, and recycles it for the recovery of triethylamine.

Embodiment 2

[0027] (1) The recovery of triethylamine crude product: in the reactor of 1000L, add concentration and be 42% triethylamine hydrochloride waste water 700Kg, add weight purity under stirring and be 96% sodium hydroxide 100Kg; Be 75 ℃ at temperature, Atmospheric distillation for 1.5 hours gave crude triethylamine.

[0028] (2) Drying of triethylamine: in a 500L reaction kettle, add the crude product of triethylamine, and add 110Kg of sodium hydroxide with a weight purity of 96% under stirring; stir for 1 hour at a temperature of 55°C, and obtain a colorless and transparent product after being separated by a filter The triethylamine has a weight content of more than 99%, a water content of less than 0.5%, and a recovery rate of 98%. The triethylamine is directly used in the production of propargite.

[0029] (3) The residual solid in the drying kettle replaces the sodium hydroxide in (1), puts it into the distillation kettle, and recycles it for the recovery of triethylamine.

Embodiment 3

[0031] (1) The recovery of triethylamine crude product: in the reactor of 1000L, add concentration and be 42% triethylamine hydrochloride waste water 700Kg, add residual sodium hydroxide in embodiment 2 under stirring; Be 85 ℃ at temperature, normal Pressure distillation was carried out for 1.5 hours to obtain crude triethylamine.

[0032] (2) All the other are the same as in Example 1.

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Abstract

The invention relates to a method for recycling triethylamine from production of propargite, which belongs to the technical field of pesticides. The method comprises the following steps of: reacting solid sodium hydroxide with triethylamine hydrochloride waste water in the production of propargite; distilling at the temperature of between 60 and 95 DEG C to obtain crude triethylamine; adding solid sodium hydroxide into the collected crude triethylamine; stirring and drying at the temperature of between 50 and 60 DEG C for 1 hour; and separating by using a filter so as to obtain a triethylamine product which has the weight content of over 99 percent and the water content of less than 0.5 percent and can be directly applied to the production of propargite. The method has the advantages of simple used equipment, convenience of operation, low energy consumption, high triethylamine recovery rate and low running cost and meets the requirement on pollution-free production.

Description

technical field [0001] The invention relates to a method for recovering triethylamine in the production of propargite, belonging to the technical field of agricultural production. Background technique [0002] Propargite, also known as propargite, has a chemical name of 2-(4-tert-butylphenoxy)cyclohexylprop-2-ynyl sulfite. It is a highly efficient, low-toxic, Broad-spectrum acaricide, acaricide with both contact and stomach poisoning effects, has remarkable efficacy and is not easy to produce drug resistance. It is mainly used for the control of harmful mites in various economic crops such as citrus, apple, and cotton. Propargite is one of the five new acaricides in the world. It is widely used in crops and suitable for a wide range of areas. It is marketed in Europe, America, Africa, Southeast Asia and other countries and regions. [0003] The synthesis uses p-tert-butylphenol as the starting material, reacts with epoxycyclohexane to generate aryloxycyclohexanol, and then...

Claims

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Application Information

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IPC IPC(8): C07C211/05C07C209/68C07C209/84
Inventor 李树柏刘瑞宾王德刚吴本林张金玉
Owner QINGDAO HANSEN BIOLOGIC SCI
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