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Method for combining di-n-propylamine through n-propylamine disproportionated reaction and used catalyst

A technology of di-n-propylamine and catalyst, which is applied in the field of synthesis of chemical intermediate-di-n-propylamine, can solve the problem of low selectivity of di-n-propylamine, and achieve the effects of high selectivity, high yield and mild reaction conditions

Active Publication Date: 2012-08-01
ZHEJIANG JIANYE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The selectivity of di-n-propylamine is too low

Method used

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  • Method for combining di-n-propylamine through n-propylamine disproportionated reaction and used catalyst
  • Method for combining di-n-propylamine through n-propylamine disproportionated reaction and used catalyst
  • Method for combining di-n-propylamine through n-propylamine disproportionated reaction and used catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1, a kind of preparation method of the supported catalyst for synthesizing di-n-propylamine, carry out the following steps successively:

[0048] 1), initial roasting:

[0049] Gamma-alumina (γ-Al 2 O 3 ) into the muffle furnace at 430~470℃ for 3h and then at 600~650℃ for 6h; γ-Al after calcination is obtained 2 O 3 ;

[0050] The specific surface area of ​​γ-alumina after calcination is 200-220m 2 g -1 , the pore size is 13.5-14.0 nm; the particle diameter remains unchanged;

[0051] 2), γ-Al after the roasting of step 1) gained 2 O 3 Immerse in water for 36 hours, and then measure the volume reduced by water, so as to obtain γ-Al after calcination 2 O 3 The pore volume density of 0.85ml / g;

[0052] 3), the first impregnation:

[0053] 43.1g of nickel nitrate solid, 20.3g of copper nitrate solid, 2.0g of zinc nitrate solid and 5.9g of ruthenium nitrate solid (all containing no crystal water) are made up to 117ml with water (such as distilled wate...

Embodiment 2

[0062] Embodiment 2, a kind of production method of di-n-propylamine, step is as follows:

[0063] 1), the prepared supported catalyst (obtained in Example 1) is activated:

[0064] ①. The supported catalyst is preliminarily activated. The ventilation time, ventilation 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, or by using Fixed bed reactor (but need to add N 2 connecting pipes).

[0065] 2. Load the preliminarily activated supported catalyst into the 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 supported catalyst after activation was obtained.

[0066] 2), place one-n-propylamine 23.6g (0.4mol) in the raw material tank, and after the preheater (that is, the vaporization c...

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Abstract

The invention discloses a load type catalyst used for combining di-n-propylamine, which utilizes roasted gama-alumina as a carrier. An active component is loaded on the carrier and is composed of nickel, copper, zinc and ruthenium. The weight sum of the nickel, the copper, the zinc, the ruthenium and the roasted gama-alumina is the total weight. The nickel occupies 15% to 25% of the total weight, the copper occupies 5% to 12% of the total weight, the zinc occupies 0.5% to 1% of the total weight, and the ruthenium occupies 0.5% to 1% of the total weight. A preparation method of the load type catalyst for combining the di-n-propylamine and a method for preparing the di-n-propylamine by using the load type catalyst are further disclosed. N-propylamine is added in a raw material cylinder, is gasified and then passes through a fixed bed reactor containing an activated load type catalyst, catalyst disproportionated reaction is conducted under the hydrogen condition, a product is collected after condensation, and rectification is conducted to obtain the di-n-propylamine.

Description

technical field [0001] The present invention relates to a kind of synthetic method of chemical intermediate-di-n-propylamine, used catalyst and corresponding preparation method. Background technique [0002] Dipropylamine (Dipropylamine), its molecular formula is C 6 H 15 N, and its structural formula is as follows: [0003] [0004] Mono-n-propylamine (also known as n-propylamine), di-n-propylamine and tri-n-propylamine are important fine chemical intermediates for the synthesis of pesticides, medicines, dyes, petroleum additives, carbon removers, emulsifiers, etc. Among them, di-n-propylamine has a wide market demand and is mainly used for the synthesis of new herbicides such as sulfapyr, trifluralin, etc. [0005] Comprehensive literature reports, the preparation method of di-n-propylamine mainly contains following three kinds at present: [0006] 1. Acrylonitrile hydrogenation method (CN10054672): Different ratios of mono-n-propylamine, di-n-propylamine and tri-n-...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C211/06C07C209/64
Inventor 陈新志汪倩倩钱超冯烈陈云斌郑丰平
Owner ZHEJIANG JIANYE CHEM
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