Triethylamine recovery processing method in bromopyrrolecarbonitrile production process

Abstract

The invention relates to a triethylamine recovery processing method in a bromopyrrolecarbonitrile production process. The triethylamine recovery processing method comprises the following steps: 1) initial steaming: placing an acidic aqueous solution containing triethylamine hydrochloride and collected in the production process into a reaction kettle, and steaming to remove low-boiling-point substances from the solution; 2) cooling: cooling with circulating water to room temperature; 3) adjusting pH value: adding slaked lime into the solution to adjust the pH value to be 8; 4) leaving to stand: leaving to stand for 0.25-0.5 hours, then pumping the upper layer of the solution into a water-removing reaction kettle, distilling the lower layer of the solution at normal pressure, then adding the distilled lower layer of the solution into the water-removing reaction kettle to be mixed with the upper layer of the solution; 5) removing water for the first time: adding a drying agent, stirring for 2-5 hours at room temperature, leaving to stand for 0.25-0.5 hours, and pumping out the water at the lower layer; 6) removing water for the second time: adding the drying agent, stirring for 2-5 hours at room temperature, leaving to stand for 0.25-0.5 hours, pumping triethylamine at the upper layer to a receiving tank, and recycling the drying agent at the lower layer. The triethylamine recovery processing method disclosed by the invention is free of usage of caustic soda flakes, and has the advantages of being mild in operation conditions, low in production cost, simple in processing equipment, low in possibility of industrialization and the like.

Description

technical field

[0001] The invention relates to the technical field of triethylamine recovery and utilization, in particular to a method for recovery and treatment of triethylamine in the production of bromopyrrolenitrile. Background technique

[0002] Chlorfenapyr is a brand-new low-toxic and high-efficiency insecticide developed and produced by American Cyanamid Company. The main component of chlorfenapyr is a new type of pyrrole compound, which has dual effects of stomach poisoning and contact killing. Its mechanism of action is to prevent the respiratory function of mitochondria in insect cells, so that ADP cannot be converted into ATP. Without ATP, the cells will stop life Function.

[0003] Bromopyrrolecarbil is a precursor intermediate for the synthesis of chlorfenapyr, and the acid-binding agent triethylamine is used in the synthesis process. Triethylamine does not participate in the synthesis, and exists in the bromopyrrole nitrile post-treatment washing solution ...

Examples

Embodiment 1

[0031] A kind of triethylamine recovery processing method in the bromopyrrole nitrile production, comprises the following steps:

[0032] 1) Initial steaming: Put 3000L of the acidic aqueous solution containing triethylamine hydrochloride collected in production into a 5000L enamel reaction kettle, control the pressure in the reaction kettle to -0.05MPa, and the temperature to 65-70℃, and evaporate the solution Medium low boilers;

[0033] 2) Cooling: After the initial steaming, the reactor is cooled to room temperature by circulating cooling water;

[0034] 3) Adjust the pH value: Add 450Kg of slaked lime to the solution to adjust the pH value to 8;

[0035] 4) Stand still: After adjusting the pH value, the solution is left to stand for 0.25-0.5h, the upper layer solution (628Kg) is pumped into the dehydration reaction kettle, and the lower layer solution (77Kg) is added to the dehydration reaction kettle and the upper layer solution after atmospheric pressure distillati...

Embodiment 2

[0041] A kind of triethylamine recovery processing method in the bromopyrrole nitrile production, comprises the following steps:

[0042] 1) Initial steaming: Put 3000L of the acidic aqueous solution containing triethylamine hydrochloride collected in production into a 5000L enamel reaction kettle, control the pressure in the reaction kettle to -0.06MPa, and the temperature to 55-60℃, and evaporate the solution Medium low boilers;

[0043] 2) Cooling: After the initial steaming, the reactor is cooled to room temperature by circulating cooling water;

[0044] 3) Adjust the pH value: Add 450Kg of slaked lime to the solution to adjust the pH value to 8;

[0045] 4) Stand still: After adjusting the pH value, the solution is left to stand for 0.25-0.5h, the upper layer solution (623Kg) is pumped into the dehydration reaction kettle, and the lower layer solution is distilled under normal pressure (80Kg) into the dehydration reaction kettle and the upper layer solution mix;

...

Embodiment 3

[0049] A kind of triethylamine recovery processing method in the bromopyrrole nitrile production, comprises the following steps:

[0050] 1) Initial steaming: put 3000L of the acidic aqueous solution containing triethylamine hydrochloride collected in production into a 5000L enamel reaction kettle, control the pressure in the reaction kettle to -0.07MPa, and the temperature to 45-50℃, and evaporate the solution Medium low boilers;

[0051] 2) Cooling: After the initial steaming, the reactor is cooled to room temperature by circulating cooling water;

[0052] 3) Adjust the pH value: Add 450Kg of slaked lime to the solution to adjust the pH value to 8;

[0053] 4) Stand still: After adjusting the pH value, the solution is left to stand for 0.25-0.5h, the upper layer solution (634Kg) is pumped into the dehydration reaction kettle, and the lower layer solution is distilled under normal pressure (72Kg) into the dehydration reaction kettle and the upper layer solution mix;

[0...

technical field

[0001] The invention relates to the technical field of triethylamine recovery and utilization, in particular to a method for recovery and treatment of triethylamine in the production of bromopyrrolenitrile. Background technique

[0002] Chlorfenapyr is a brand-new low-toxic and high-efficiency insecticide developed and produced by American Cyanamid Company. The main component of chlorfenapyr is a new type of pyrrole compound, which has dual effects of stomach poisoning and contact killing. Its mechanism of action is to prevent the respiratory function of mitochondria in insect cells, so that ADP cannot be converted into ATP. Without ATP, the cells will stop life Function.

[0003] Bromopyrrolecarbil is a precursor intermediate for the synthesis of chlorfenapyr, and the acid-binding agent triethylamine is used in the synthesis process. Triethylamine does not participate in the synthesis, and exists in the bromopyrrole nitrile post-treatment washing solution ...

Examples

Embodiment 1

[0031] A kind of triethylamine recovery processing method in the bromopyrrole nitrile production, comprises the following steps:

[0032] 1) Initial steaming: Put 3000L of the acidic aqueous solution containing triethylamine hydrochloride collected in production into a 5000L enamel reaction kettle, control the pressure in the reaction kettle to -0.05MPa, and the temperature to 65-70℃, and evaporate the solution Medium low boilers;

[0033] 2) Cooling: After the initial steaming, the reactor is cooled to room temperature by circulating cooling water;

[0034] 3) Adjust the pH value: Add 450Kg of slaked lime to the solution to adjust the pH value to 8;

[0035] 4) Stand still: After adjusting the pH value, the solution is left to stand for 0.25-0.5h, the upper layer solution (628Kg) is pumped into the dehydration reaction kettle, and the lower layer solution (77Kg) is added to the dehydration reaction kettle and the upper layer solution after atmospheric pressure distillati...

Embodiment 2

[0041] A kind of triethylamine recovery processing method in the bromopyrrole nitrile production, comprises the following steps:

[0042] 1) Initial steaming: Put 3000L of the acidic aqueous solution containing triethylamine hydrochloride collected in production into a 5000L enamel reaction kettle, control the pressure in the reaction kettle to -0.06MPa, and the temperature to 55-60℃, and evaporate the solution Medium low boilers;

[0043] 2) Cooling: After the initial steaming, the reactor is cooled to room temperature by circulating cooling water;

[0044] 3) Adjust the pH value: Add 450Kg of slaked lime to the solution to adjust the pH value to 8;

[0045] 4) Stand still: After adjusting the pH value, the solution is left to stand for 0.25-0.5h, the upper layer solution (623Kg) is pumped into the dehydration reaction kettle, and the lower layer solution is distilled under normal pressure (80Kg) into the dehydration reaction kettle and the upper layer solution mix;

...

Embodiment 3

[0049] A kind of triethylamine recovery processing method in the bromopyrrole nitrile production, comprises the following steps:

[0050] 1) Initial steaming: put 3000L of the acidic aqueous solution containing triethylamine hydrochloride collected in production into a 5000L enamel reaction kettle, control the pressure in the reaction kettle to -0.07MPa, and the temperature to 45-50℃, and evaporate the solution Medium low boilers;

[0051] 2) Cooling: After the initial steaming, the reactor is cooled to room temperature by circulating cooling water;

[0052] 3) Adjust the pH value: Add 450Kg of slaked lime to the solution to adjust the pH value to 8;

[0053] 4) Stand still: After adjusting the pH value, the solution is left to stand for 0.25-0.5h, the upper layer solution (634Kg) is pumped into the dehydration reaction kettle, and the lower layer solution is distilled under normal pressure (72Kg) into the dehydration reaction kettle and the upper layer solution mix;

[0...

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