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Synthetic method for secondary butylamine

A synthesis method, sec-butylamine technology, applied in chemical instruments and methods, Raney-type catalysts, organic chemistry, etc., can solve problems such as high cost and difficult operation, and achieve low production cost, simple equipment, and high product purity Effect

Active Publication Date: 2008-04-30
ZHEJIANG JIANYE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Difficult to operate and high cost, thus limiting its further industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: a kind of synthetic method of sec-butylamine, carry out following steps successively:

[0013] 1, prepare fresh Raney nickel (Raney Ni) catalyst (this is prior art): 2g Ni-Al alloy is dissolved in batches in the 100mL sodium hydroxide aqueous solution that contains 10g sodium hydroxide, keep stirring, until no longer Bubbles are produced. Pour off the upper aqueous solution, wash with fresh distilled water several times, until the final wash is neutral.

[0014] 2. Into a 500mL autoclave, add all Raney Ni and butanone oxime 188.6mL (174.2g / 2.0mol) prepared above in sequence. First replace the autoclave with hydrogen three times, and then fill it with hydrogen to 2.5 MPa; then add 17 g (1.0 mol) of ammonia into the autoclave. Heat the above-mentioned substances in the autoclave to 85°C to carry out the reduction reaction. During the reaction, the pressure drops, and hydrogen needs to be continuously replenished, and the hydrogenation is carried out under ...

Embodiment 2

[0017] Embodiment 2: a kind of synthetic method of sec-butylamine, carry out following steps successively:

[0018] 1, prepare fresh Raney Ni catalyst: with embodiment 1.

[0019] 2. In a 500mL autoclave, add water 100mL (100g / 5.56mol), Raney Ni catalyst 3.0g (by fresh Raney Ni catalyst 1.0g and the Raney Ni catalyst (i.e. filter cake) 2.0g recycled in Example 1 composition) and butanone oxime 95mL (87.78g / 1.01mol). Replace the autoclave twice with hydrogen, then fill it up to 1.0MPa, heat the above mixture in the autoclave to 150°C for reduction reaction, the pressure drops during the reaction, hydrogen needs to be continuously replenished, and hydrogenation is carried out under the condition of maintaining the pressure at 1.0MPa ; Until the hydrogen is no longer absorbed, the pressure is kept constant at this time, and the reaction time is 20h in total.

[0020] 3. It is equal to embodiment 1. The resulting sec-butylamine yield is 68.3%. The total yield of the obtained s...

Embodiment 3

[0021] Embodiment 3: a kind of synthetic method of sec-butylamine, carry out following steps successively:

[0022] 1, prepare fresh Raney Ni catalyst: with embodiment 1.

[0023] 2. Add methanol 100mL (79.2g / 2.47mol), fresh Raney Ni catalyst 8.7g and butanone oxime 94mL (87.2g / 1.0mol) sequentially into a 500mL autoclave. Firstly, the autoclave was replaced twice with hydrogen, and then filled to 6.0 MPa; and 34 g (2.0 mol) of ammonia was added into the autoclave. Heat the above-mentioned mixture in the autoclave to 65°C for reduction reaction. During the reaction, the pressure drops, and hydrogen needs to be continuously replenished. Keep the pressure at 6.0MPa and hydrogenate; until no more hydrogen is absorbed, the pressure is kept constant at this time, and the reaction time is It is 5.5h.

[0024] 3. It is equal to embodiment 1. The resulting sec-butylamine yield reaches 92.5%. The total yield of the obtained sec-butylamine and di-sec-butylamine is 96.3%.

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Abstract

The process of synthesizing secondary butylamine includes the reduction reaction of butanone oxime and hydrogen under the action of ammonia at pressure of 1-6 MPa and temperature of 20-150 deg.c in the presence of Raney Ni catalyst; and the dewatering and rectification of the reaction product. The Raney Ni catalyst amount is 0.28-10 wt% of butanone oxime, and the weight ratio between ammonia and butanone oxime is 0-2 to 1. The secondary butylamine synthesizing process has low cost and high yield.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing a chemical intermediate - sec-butylamine. Background technique [0002] Sec-butylamine is an important organic chemical intermediate, and its synthesis methods mainly include: [0003] (1) Document Canadian Journal of Chemistry, 1981, 59(20): 3007-11, using lithium aluminum hydride to reduce butanone oxime to obtain the target product. Because the reaction needs to use the reducing agent lithium aluminum hydride, which is expensive and difficult to operate, the production cost is too high and it is not suitable for industrial production. [0004] (2), the document Journal of Molecular Catalysis A: Chemical, 1999, 146 (1-2): 129-138, using butanone as raw material, using palladium loaded on modified activated carbon as catalyst, and benzylamine at a hydrogen pressure of 60bar Under the conditions of reaction, chiral sec-butanol was obtained...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/03C07C209/24B01J25/02
Inventor 陈新志刘金强
Owner ZHEJIANG JIANYE CHEM
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