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Method for continuously preparing di-sec-butylamine

A technology for di-sec-butylamine and methyl ethyl ketone, which is applied in the field of continuous preparation of di-sec-butylamine, can solve the problems of unfavorable industrial popularization and application, low yield of di-sec-butylamine, harsh operating conditions, etc., and achieves low production cost. , The effect of low raw material consumption and high conversion rate

Active Publication Date: 2010-02-17
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Relevant information reports that this method is based on methyl ethyl ketone oxime as the main raw material, with Raney nickel as the catalyst under high pressure (2.5Mpa) operation in an autoclave, the operating conditions are relatively harsh, the reaction time is long (5-6h), and di-sec-butylamine The yield is relatively low, which is not conducive to industrial promotion and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: This di-sec-butylamine (C 8 h 19 N) preparation method:

[0020] γ-Al purchased in the market 2 o 3 Add a certain amount of diatomaceous earth and mix evenly, extrude, dry, and roast to obtain strips of γ-Al with a diameter of 4 mm and a length of 3 to 7 mm. 2 o 3 -Diatomaceous earth carrier, the nitrate of Ni, Cu, Cr, Mn, Zn, Fe is made into a mixed solution in proportion, for γ-Al 2 o 3 - Diatomaceous earth carrier is impregnated, after drying, it is put into muffle furnace and roasted for 24 hours, and the obtained content is 14.5% for Ni, 12.5% ​​for Cu, 6.1% for Cr, 5.3% for Mn, 5.0% for Zn, and 4.1% for Fe, The rest is γ-Al 2 o 3 and diatomaceous earth mixture Ni-Cuγ-Al 2 o 3 - diatomaceous earth catalyst.

[0021] The prepared catalyst was loaded into a stainless steel reactor with a diameter of 32×3mm and a length of 1320mm. A stainless steel temperature measuring sleeve of ∮8×1mm is installed in the reactor, the catalyst filling height...

Embodiment 2

[0024] According to the conditions and steps of Example 1, the operating conditions were changed to: temperature of 160° C., pressure (gauge pressure) of 0.6 MPa, butanone reaction conversion rate of 95%, and di-sec-butylamine selectivity of 68%.

Embodiment 3

[0026] According to the conditions and steps of Example 1, the operating conditions were changed to: temperature of 160° C., pressure (gauge pressure) of 0.8 MPa, butanone reaction conversion rate of 96%, and di-sec-butylamine selectivity of 71%.

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Abstract

The invention discloses a chemical synthesizing method, in particular a method for continuously preparing di-sec-butylamine using butanone as a raw material. In the invention, the butanone is used asthe raw material, and the butanone is pumped into a pre-heater to mix with ammonia and hydrogen to preheat and evaporate; Ni-Cu / gamma-Al2O3-diatomite is used as a catalyst, the temperature with a certain pressure is controlled, after reaction, the materials are condensed and cooled to separate gas and liquid, the gas phase enters a reactor by circulating to be used repeatedly; the liquid phase enters a rectifying tower to separate and purify the di-sec-butylamine to obtain the product; the separated ammonia, butanone and sec-butylamine return to a feeding system and enter the reactor to reactwith the supplementary hydrogen, the ammonia and the butanone. The invention has advantages of simple process, high conversion rate, good selectivity, simple process of separating, low consumption ofenergy and raw materials and low production cost.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a continuous preparation method of di-sec-butylamine using butanone as a raw material. Background technique [0002] Di-sec-butylamine is an organic chemical intermediate, mainly used in the production of herbicides (such as thiocarbazides), and can also be used in medicine, dyes, corrosion inhibitors, flotation agents, rubber vulcanization accelerators, etc. [0003] The production method of di-sec-butylamine is mainly methyl ethyl ketoxime ammonification dehydration method. Relevant information reports that this method is based on methyl ethyl ketone oxime as the main raw material, with Raney nickel as the catalyst under high pressure (2.5Mpa) operation in an autoclave, the operating conditions are relatively harsh, the reaction time is long (5-6h), and di-sec-butylamine The productive rate is relatively low, which is unfavorable for industrial promotion and application. Conten...

Claims

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Application Information

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IPC IPC(8): C07C211/07C07C209/26B01J23/889
CPCY02P20/584
Inventor 陈国建兰昭洪南巍冈伍伟伟
Owner ZHEJIANG XINHUA CHEM
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