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A method for removing dibutylamine in tetrabutylurea

A technology of tetrabutylurea and dibutylamine, applied in chemical instruments and methods, preparation of urea derivatives, preparation of organic compounds, etc., can solve the problem of affecting the flow rate of working fluid and device capacity, high dibutylamine content, affecting the device Safe and stable operation and other issues

Active Publication Date: 2021-02-09
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Based on the new hydrogen peroxide production process containing tetrabutylurea three-solvent working fluid, the existing hydrogen peroxide production equipment often has abnormal phenomena such as accumulation of working fluid under the sieve plate of the extraction tower during operation, which not only affects the flow rate of the working fluid and The production capacity of the device also affects the safe and stable operation of the device. The high content of dibutylamine in tetrabutylurea is the main reason for the above abnormal phenomenon
The existing production technology of tetrabutyl urea can only reduce the content of dibutylamine in tetrabutyl urea to about 1000mg / L through distillation and other processes, and it is difficult to solve the problem of abnormal operation of the extraction tower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Measure 100mL of tetrabutylurea into a 500mL flask, wherein the content of dibutylamine is 1032.6mg / L. Add 0.05g of 27.5% hydrogen peroxide, stir evenly, keep the temperature at 10-20°C, then add 5g of 1% phosphoric acid aqueous solution, after the addition is completed, continue to react for 0.2h, after the reaction is completed, let stand for 10min to separate layers and separate Go out organic phase, wash organic phase with the water of 1 / 5 organic phase volume at every turn, wash with water 3 times, pH value is 5, wash once with 10ml 1% sodium hydroxide aqueous solution again, then wash to neutrality, detect and handle four The content of dibutylamine in butylurea is 83.6mg / L.

Embodiment 2

[0015] Measure 100mL of tetrabutylurea into a 500mL flask, wherein the content of dibutylamine is 1032.6mg / L. Add 0.1g of 27.5% hydrogen peroxide, stir evenly, keep the temperature at 30-40°C, then add 10g of 3% dilute sulfuric acid, continue the reaction for 2h, then let stand for 10min to separate layers. Separate the organic phase, wash the organic phase with water of 1 / 5 of the volume of the organic phase each time, sink in water three times, and the pH value is 7. After testing, the content of dibutylamine in tetrabutylurea is 73.4 mg / L.

Embodiment 3

[0017] Measure 100mL of tetrabutylurea into a 500mL flask, wherein the content of dibutylamine is 827.6mg / L. Add 0.15g of 27.5% hydrogen peroxide, stir evenly, keep the temperature at 35-45°C, then add 20g of 1% dilute nitric acid, after the addition is complete, continue the reaction for 5h, after the reaction, let stand for 10min to separate layers. After layering, the organic phase was washed three times with water, the pH value was 5, washed once with 3% aqueous sodium hydroxide solution, and then washed to neutrality. The content of dibutylamine in tetrabutylurea after detection was 78.0mg / L.

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Abstract

The invention discloses a method for removing dibutylamine from tetrabutylurea, which comprises the following steps: (1) adding industrial-grade tetrabutylurea into a reaction vessel, adding hydrogen peroxide, and stirring evenly at 10-60°C; (2) Add an aqueous solution of inorganic acid or organic acid to the reactor in step (1), react at room temperature for 0.2 to 5 hours, and let it stand for 10 minutes; (3) Wash the organic phase with 1 / 5 of the volume of the organic phase each time, and wash it with water for 3 times , if the pH value of the organic phase is > 6, continue to wash with water until neutral; if the pH value of the organic phase is ≤ 6, neutralize with alkali, and then wash with water until neutral. The method can reduce the dibutylamine content in the technical grade tetrabutylurea to below 100mg / L.

Description

technical field [0001] The invention relates to a method for removing dibutylamine in tetrabutylurea. Background technique [0002] Tetrabutylurea (1,1,3,3-Tetrabutylurea, referred to as TBU), is a colorless to light yellow, odorless liquid at normal temperature and pressure, and is a widely used organic synthesis intermediate or Solvent, which can be used to prepare pesticides, medicines, dyes, plasticizers and stabilizers for plastics, catalysts and solvents for phosgenation reactions, and lubricating oils; it can also replace highly toxic phosphoric acid amides for the preparation of aminoplast additives. The important use is to replace trioctyl phosphate (TOP) as a solvent for alkylanthraquinone and alkylanthrahydroquinone in the process of synthesizing hydrogen peroxide by anthraquinone method. By partially or completely replacing TOP with TBU, the solubility of alkylanthraquinones and alkylanthrahydroquinones in the working fluid can be increased, the hydrogenation ef...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C273/18C07C275/06
CPCC07C273/189C07C275/06
Inventor 马会强赵晓东沈冲柴春玲冯彬
Owner LIMING RES INST OF CHEM IND