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Method for preparing sec-butylamine through methyl ethyl ketone catalytic ammonization hydrogenation

A technology of methyl ethyl ketone and sec-butylamine, which is applied in the field of catalytic ammonification hydrogenation of methyl ethyl ketone to prepare sec-butylamine, can solve the problems of unfavorable industrial production, high temperature of kettle reaction, and low liquid space velocity, and reduce production cost and volume The effect of high space velocity and mild reaction conditions

Inactive Publication Date: 2013-01-30
泰州石油化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deficiency of above-mentioned prior art is: kettle type reaction temperature high pressure is high, difficult to operate
In this tubular continuous reaction, the liquid space velocity is too low, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A tubular fixed-bed catalytic amination hydrogenation reactor with a length of 400 mm and an inner diameter of 12 mm was used in the test.

[0020] Catalyst preparation: 50g carrier γ-Al 2 o 3 The ball (Φ2-3mm) is immersed in the nitrate solution of Ni and Zn, the solvent is evaporated, dried at 120°C for 12 hours, and calcined at 500°C for 10 hours to obtain 10%Ni / 5%Zn / γ-Al 2 o 3 The catalyst was reductively activated by passing hydrogen at 500°C for 8 hours before the reaction.

[0021] The raw materials methyl ethyl ketone, hydrogen and ammonia are continuously input from the upper inlet of the tubular reactor. After the amination and hydrogenation reaction, the reaction products are collected after online analysis by gas chromatography, and samples are taken and analyzed at intervals of 1 hour.

[0022] Reaction conditions: The molar ratio of methyl ethyl ketone, hydrogen and ammonia is 1:6:5, and the volume space velocity of methyl ethyl ketone is 1.5h -1 , Atm...

Embodiment 2

[0024] Using the catalyst of Example 1, the reaction conditions: the molar ratio of methyl ethyl ketone, hydrogen and ammonia is 1:5:2, and the volume space velocity of methyl ethyl ketone is 1.0h -1 , Atmospheric pressure, reaction at 130°C, can continuously prepare sec-butylamine, the conversion rate of methyl ethyl ketone can reach 100%, and the selectivity of sec-butylamine is greater than 95%.

Embodiment 3-7

[0026] 15%Ni / 5%Zn / γ-Al prepared by the method of Example 1 2 o 3 Catalyst, methyl ethyl ketone, hydrogen and ammonia in a molar ratio of 1:3:2, the volume space velocity of methyl ethyl ketone is 0.3h -1 、0.4h -1 、0.5h -1 、1.0h -1 、1.5h -1 、2.0h -1 , normal pressure, 130 ° C reaction, can be continuously prepared to obtain sec-butylamine, the reaction results are shown in Table 1.

[0027] Table 1

[0028] Methyl ethyl ketone space velocity / h -1 Conversion rate of methyl ethyl ketone Selectivity of sec-butylamine Example 3 0.3 100 98.4 Example 4 0.4 100 98.6 Example 5 0.5 100 99 Example 6 1.0 100 97.3-98.8 Example 7 1.5 99-100 94.6-96.1 Example 8 2.0 96.2-98 93-94.8

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Abstract

The invention relates to a method for preparing sec-butylamine through methyl ethyl ketone catalytic ammonization hydrogenation. According to the invention, a tubular reactor is adopted; methyl ethyl ketone is adopted as a raw material; under the existence of a catalyst containing Ni and Cu or Cr or Zn or Fe, and under the condition that a methyl ethyl ketone volume space velocity is 0.3-2.5h<-1>, methyl ethyl ketone, hydrogen gas and ammonia gas are simultaneously delivered from the upper end of the reactor according to a molar ratio of 1:1-10:1-10; and a methyl ethyl ketone continuous ammonization hydrogenation reaction is carried out under a temperature of 80-160 DEG C and a normal pressure, such that sec-butylamine can be obtained by continuous preparation. According to the invention, a preparation process of the catalyst is simple, a metal load is low, and a catalytic activity is high; the reaction conditions are mild, and high-yield sec-butylamine can be obtained under normal pressure; and only trace sec-butanol and di-sec-butylamine by-products are produced. The volume space velocity of methyl ethyl ketone is high, the process is simple, and continuous production can be carried out, such that production cost is reduced, and the method is suitable for industrialization and popularization. A conversion rate of methyl ethyl ketone can reach 90-100%, and sec-butylamine selectivity is higher than 90%.

Description

technical field [0001] The invention relates to a method for preparing sec-butylamine by catalytic hydrogenation and hydrogenation of methyl ethyl ketone. Background technique [0002] Sec-butylamine is an important organic chemical intermediate, widely used in medicine, pesticide, dyestuff, chemical auxiliary, rubber and other industries. S-butylamine has the function of anti-mold and fresh-keeping. As early as 1975, the United Nations Health Organization and the Food Organization recommended S-butylamine as an excellent fresh-keeping agent with low toxicity, no teratogenicity, and no carcinogenic effects. At present, the synthesis methods of sec-butylamine mainly include: sec-butanol amination hydrogenation, butanone oxime reduction method, methyl ethyl ketone amination hydrogenation and butene amination hydrogenation. [0003] 1. S-butanol amination hydrogenation method: Chai Huanlong (Pesticides, 1983, 06: 33-42) used s-butanol as raw material to continuously prepare s-...

Claims

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Application Information

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IPC IPC(8): C07C211/07C07C209/26
Inventor 胡传清赵培庆赵志远于超英王涛陈革新金龙姚彩兰仇忠
Owner 泰州石油化工有限责任公司
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