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Synthetic method of N-tert-butyl diethanolamine

A technology of tert-butyldiethanolamine and synthetic method, which is applied in the direction of chemical instruments and methods, preparation of amino hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of low yield, difficult quality control, difficult operation, etc., and achieve high yield High, low cost, product quality guaranteed effect

Inactive Publication Date: 2013-10-30
SHANGHAI HUAFENG MATERIAL TECH RES INST LLP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a synthetic method of N-tert-butyldiethanolamine, to solve the technical problems existing in the existing synthetic method of N-tert-butyldiethanolamine, such as difficult operation, low yield and difficult quality control etc.

Method used

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  • Synthetic method of N-tert-butyl diethanolamine
  • Synthetic method of N-tert-butyl diethanolamine

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preparation example Construction

[0029] see figure 1 , the synthetic method of N-tert-butyldiethanolamine of the present invention, comprises the following steps:

[0030] a. Synthesis reaction: put catalyst in the reactor, replace the air in the reactor with nitrogen, vacuumize to -0.1MPa~-0.03MPa, add metered tert-butylamine, then raise the temperature in the reactor to 50-160℃, slowly Add metered ethylene oxide so that the temperature in the reactor is kept at 50-160°C, and the pressure is kept at 0-0.8MPa, until the end of the reaction to obtain a mixture containing N-tert-butyldiethanolamine;

[0031] B, post-processing: the post-processing of degassing and filtering the obtained mixture to obtain the crude product;

[0032] c. Purification: The crude product is subjected to vacuum distillation or rectification to obtain N-tert-butyldiethanolamine.

[0033] In the steps of the synthesis reaction, the feeding method of negative pressure in the reactor and a suitable catalyst are used, which have the fol...

Embodiment 1

[0037] After nitrogen replacement, 27 g of zinc acetate was added to a 3 L reactor, and the vacuum was evacuated to -0.098 MPa. Add 483 g of tert-butylamine through a metering pump, then increase the temperature in the kettle to 50° C., and slowly add 613 g of ethylene oxide in total. By controlling the addition rate of ethylene oxide and the temperature and flow of cooling water in the kettle, the temperature in the kettle is kept at 50° C., and the pressure is kept below 0.3 MPa. After all the ethylene oxide was added, when the pressure in the kettle was almost no longer reduced, the reaction was deemed to be nearly complete, and the reaction was discharged after 30 minutes. The reaction liquid is forced to flow out from the kettle through the filter by nitrogen pressure, and the filtrate is further processed. GC-MS analysis results showed that the effective content of the product in the crude product was 95%.

[0038] After the crude product is degassed, carry out rectifi...

Embodiment 2

[0040] After nitrogen replacement, 34 g of potassium hydroxide was added to a 5 L reactor, and the vacuum was evacuated to -0.07 MPa. Add 960 g of tert-butylamine through a metering pump, then increase the temperature in the kettle to 90° C., and slowly add 1226 g of ethylene oxide in total. By controlling the addition rate of ethylene oxide and the temperature and flow of cooling water in the kettle, the temperature in the kettle is kept at 90° C., and the pressure is kept below 0.4 MPa. After all the ethylene oxide was added, when the pressure in the kettle was almost no longer reduced, the reaction was deemed to be nearly complete, and the reaction was discharged after 30 minutes. The reaction liquid is forced to flow out from the kettle through the filter by nitrogen pressure, and the insoluble solids are filtered out.

[0041] After the crude product is degassed, carry out rectification and purification, the rectification pressure is -0.09MPa, and the fraction at 196-200...

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Abstract

The invention provides a synthetic method of N-tert-butyl diethanolamine. The synthetic method comprises the following steps of: a, putting a catalyst into a reactor, replacing the air in the reactor by using nitrogen, vacuumizing the reactor until the pressure is between -0.1MPa and -0.03MPa, adding metered tert-butylamine, then raising the temperature in the reactor to be 50-160 DEG C, slowly adding metered epoxyethane to ensure that the temperature in the reactor is kept between 50 DEG C and 160 DEG C, and keeping the pressure to be 0-0.8MPa until the reaction is finished to obtain a mixture containing N-tert-butyl diethanolamine; b, performing post treatment; and c, purifying to obtain the N-tert-butyl diethanolamine. Compared with the prior art, the synthetic method adopts a charging mode with negative pressure in the reactor and an appropriate catalyst, the raw material partial pressure is improved, the reaction speed can be further increased, oxidation discoloration of a product can be prevented, the reaction condition is relatively mild, the operation is more controllable, the yield is high, the product quality is more ensured, the operation is simple and the cost is low, so that the synthetic method is favorable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical product synthesis, in particular to a synthesis method of N-tert-butyldiethanolamine (TBDEA). Background technique [0002] As a fine chemical, N-tert-butyldiethanolamine can be applied to the synthesis of pharmaceutical intermediates, and can also be used as an intermediate for some auxiliary agents. [0003] At present, there are few reports on the synthetic method of N-tert-butyldiethanolamine. The existing synthetic methods are mainly based on the synthesis of tert-butylamine (TBA) and ethylene oxide (EO), and some use solvent systems, such as aqueous phase Synthesis, however, is too energy-intensive to remove water and has a high water content that is difficult to control. Japanese patent JP2011178664A discloses a method for synthesizing N-tert-butyldiethanolamine. This method requires extremely high reaction temperature, which leads to excessive pressure and affects the feeding of ethylene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/12C07C213/04
Inventor 吴淑航唐劲松项超力殷延开费长书梁红军李善军何永
Owner SHANGHAI HUAFENG MATERIAL TECH RES INST LLP
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