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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, reduced pressure, and wide source of raw materials

Active Publication Date: 2013-11-13
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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1, a kind of preparation method of the loaded catalyst that is used for synthesizing di-n-propylamine, carries out following steps successively:

[0048] 1), initial roasting:

[0049] Gamma-alumina (γ-Al 2 o 3 ) into a muffle furnace and roasted at 430-470°C for 3h, and then at 600-650°C for 6h; the roasted γ-Al 2 o 3 ;

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

[0051] 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 0.85ml / g;

[0052] 3), initial impregnation:

[0053] 43.1g nickel nitrate solid, 20.3g copper nitrate solid, 2.0g zinc nitrate solid and 5.9g ruthenium nitrate solid (all without crystal water) were fixed to 117ml with water (for example, distilled water) to obtain a ...

Embodiment 2

[0062] Embodiment 2, a kind of production method of di-n-propylamine, the steps are as follows:

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

[0064] 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).

[0065] 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.

[0066] 2), 23.6g (0.4mol) of one n-propylamine is placed in the raw material tank, after being vaporized by th...

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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 invention relates to a synthesis method of a chemical intermediate-di-n-propylamine, a catalyst used and a corresponding preparation method. Background technique [0002] Dipropylamine (Dipropylamine), its molecular formula is C 6 h 15 N, whose 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 used in 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 in the synthesis of new herbicides such as ansulfin and trifluralin. [0005] Comprehensive literature report, the preparation method of di-n-propylamine mainly contains following three kinds at present: [0006] 1. Acrylonitrile hydrogenation method (CN10054672): different catalysts can be used to produce mono-n-propylamine, di-n-propylamin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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