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Method and used catalytic agent for synthesizing N-butylethylamine

A technology of ethyl n-butylamine and catalyst, which is applied in the field of synthesis of chemical intermediate-N-ethyl n-butylamine, can solve problems such as heavy burden and reduced catalyst activity, achieve cost reduction, reduce the burden of separation, and reduce the price cheap effect

Active Publication Date: 2013-08-14
ZHEJIANG JIANYE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The presence of water, on the one hand, will reduce the activity of the catalyst, on the other hand, it will form azeotrope and bring a great burden to the separation

Method used

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  • Method and used catalytic agent for synthesizing N-butylethylamine
  • Method and used catalytic agent for synthesizing N-butylethylamine
  • Method and used catalytic agent for synthesizing N-butylethylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1, the preparation method of supported catalyst, carry out following steps successively:

[0047] 1), initial roasting:

[0048] Gamma-alumina (γ-Al 2 o 3 ) at 430-470°C for 3 hours, and then at 600-650°C for 6 hours; 2 o 3 .

[0049] After testing: the specific surface area of ​​the γ-alumina after roasting is 200-220m 2 g -1 , the pore diameter is 13.5-14.0nm, and the particle diameter remains unchanged.

[0050] 2), the roasted γ-Al obtained in step 1)2 o 3 Immerse in water for 36 hours, and then measure the volume of water reduction, so as to obtain the γ-Al after calcination 2 o 3 The pore volume density is 0.83ml / g.

[0051] 3), initial impregnation:

[0052] 47.4g of copper nitrate trihydrate and 63.3g of solid nickel nitrate hexahydrate (the molar ratio of copper and nickel elements is 0.9:1) were adjusted to 118mL with water (for example, distilled water) to obtain a mixed solution;

[0053] After step 1) the obtained γ-Al after roasting ...

Embodiment 2

[0061] Embodiment 2, a kind of synthetic method of N-ethyl n-butylamine, carry out following steps successively:

[0062] 1), the prepared supported catalyst (gained in Example 1) is activated:

[0063] ①. Initially activate the supported catalyst first. During the initial activation, the aeration time, aeration flow rate and heating temperature in different activation time periods are shown in Table 1 above; this step can be carried out outside the fixed bed reactor, and can also be used Fixed bed reactor (but need to add N 2 connecting pipes).

[0064] ②. Load the initially activated supported catalyst into a fixed-bed reactor, and reactivate it at 160-250°C (for example, 240°C) under the action of hydrogen until the activation is completed (that is, there is no condensed water in the lower part of the fixed-bed reactor) produced); the activated supported catalyst was obtained.

[0065] 2), 730g (16.2mol) of ethylamine and 580g (7.95mol) of n-butylamine are mixed and then...

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Abstract

The invention discloses a loading-type catalytic agent for synthesizing N-butylethylamine. Gamma-alumina after roasting serves as a carrier, active components composed of Cu and Ni are loaded on the carrier, sum of weight of the Cu, the Ni and the gamma-AI2O3 after roasting is total weight, sum of weight of the Cu and the Ni occupies 25%-38% of the total weight, and ratio of amount of substance of the Cu and the Ni is 0.9-1.5 / 1. The invention further provides a preparation method of the loading-type catalytic agent. A method for synthesizing the N-butylethylamine by using the loading-type catalytic agent is further provided, ethylamine and the n-butylamine are mixed in a mixing tank to obtain mixed liquor which passes through a fixed bed reactor containing activated loading-type catalyticagent after being vaporized, an amine disproportionated reaction is carried out in a hydrogenation condition, products are collected after condensation, and rectification is carried out to obtain theN-butylethylamine.

Description

technical field [0001] The invention relates to a synthesis method of a chemical intermediate-N-ethyl n-butylamine, a used catalyst and a preparation method. Background technique [0002] N-ethyl-n-butylamine (N-ethyl-n-butylamine), its molecular formula is C 6 h 15 N, whose structural formula is as follows: [0003] [0004] N-ethyl n-butylamine is an important pesticide and pharmaceutical intermediate, which can be used in the synthesis of herbicides such as clofenac and flurafen; it can also be used in the synthesis of milnacipran derivatives (nervous system drugs) and CRF receptor inhibitors, etc. In addition, due to the electron-rich nature of amines, they can also interact with CS 2 etc. as ligands for metals such as Gd, In, and Zn. [0005] The synthesis method of N-ethyl n-butylamine can be roughly divided into substitution amination and catalytic amination at present. For the synthesis of N-ethyl n-butylamine, it can be realized by the N-ethylation of n-but...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755C07C211/08C07C209/64
Inventor 陈新志黄佳民钱超冯烈陈云斌曹伟富
Owner ZHEJIANG JIANYE CHEM
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