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Method for combining tributylamine and used catalyst

A technology of tri-n-butylamine and n-butylamine, applied in the field of organic compound synthesis, can solve problems such as being unsuitable for large-scale industrial production, unable to realize continuous production, expensive catalyst, etc., and achieve good mechanical strength and stability, The effect of easy control of the reaction and suitable reaction conditions

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

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Problems solved by technology

Although the yield of this reaction is high, the catalyst is expensive, the reaction time is very long, and continuous production cannot be realized, and the solvent methanol is highly toxic, so it is not suitable for large-scale industrial production

Method used

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  • Method for combining tributylamine and used catalyst
  • Method for combining tributylamine and used catalyst
  • Method for combining tributylamine and used catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1, a kind of loaded catalyst that is used to prepare tri-n-butylamine, preparation process is as follows:

[0050] 1), initial roasting:

[0051] Gamma-alumina (γ-Al 2 o 3 ) at a temperature of 700°C to 800°C for 4 hours, and naturally cooled to room temperature to obtain the calcined γ-Al 2 o 3 ;

[0052] After testing: after roasting, the specific surface area of ​​γ-alumina is 170-180m 2 g -1 , the pore size is 16.5-17.2nm; the particle diameter remains unchanged.

[0053] 2), the roasted γ-Al obtained in step 1) 2 o 3 Immerse in water for at least 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 about 0.9ml / g;

[0054] 3), dipping:

[0055] 7.44gNi(NO 3 ) 2 ·6H 2 O, 4.54g Cu(NO 3 ) 2 ·3H 2 O, 0.72gFe(NO 3 ) 3 9H 2 O and 0.94gPt(NO 3 ) 2 Dilute the volume to 6.3ml with water (for example, distilled water) to obtain an impregnating solution, and roast...

Embodiment 2

[0059] Embodiment 2, a kind of supported catalyst for preparing tri-n-butylamine, preparation process is as follows:

[0060] Step 3) Change to the following:

[0061] 3), 8.43gNi(NO 3 ) 2 ·6H 2 O, 3.97g Cu(NO 3 ) 2 ·3H 2 O, 0.65gFe(NO 3 ) 3 9H 2 O and 1.12gPt(NO 3 ) 2 Dilute the volume to 6.3ml with water to obtain the impregnating solution, then put in 7.1g of calcined γ-alumina (specific surface area 170-180m 2 g -1 ) to fully mix and impregnate until the impregnating solution is roasted and the γ-Al 2 o 3 Absorbs completely.

[0062] Step 1), 2) and 4) are the same as in Example 1.

[0063] The supported catalyst contains Ni: 17%; Cu: 10.5%; Fe: 0.9%; Pt: 0.6%. The % is by weight.

Embodiment 3

[0064] Embodiment 3, a kind of loaded catalyst for preparing tri-n-butylamine, preparation process is as follows:

[0065] Step 3) Change to the following:

[0066] 3), 9.42gNi(NO 3 ) 2 ·6H 2 O, 3.40g Cu(NO 3 ) 2 ·3H 2 O, 0.58gFe(NO 3 ) 3 9H 2 O and 1.31gPt(NO 3 ) 2 Dilute to 6.3ml with water to obtain an impregnating solution, then add 7.1g of roasted γ-Al 2 o 3 (specific surface area 170-180m 2 g -1 ) to fully mix and impregnate until the impregnating solution is roasted and the γ-Al 2 o 3 Absorbs completely.

[0067] Step 1), 2) and 4) are the same as in Example 1.

[0068] The supported catalyst contains Ni: 19%; Cu: 9%; Fe: 0.8%; Pt: 0.7%. The % is by weight.

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Abstract

The invention discloses a load type catalyst, which utilizes roasted gama-alumina as a carrier. An active component is loaded on the carrier to obtain the load type catalyst. The active component is composed of nickel, copper, iron and platinum. The weight sum of the nickel, the copper, the iron, the platinum 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 iron occupies 0.5% to 1% of the total weight, and the platinum occupies 0.5% to 1% of the total weight. A preparation method of the load type catalyst and a method for preparing tributylamine by using the load type catalyst are further disclosed. Butylamine and dibutylamine are mixed in a mixed cylinder to obtain mixed liquid, the mixed liquid is gasified and then passes through a fixed bed reactor containing an activated load type catalyst, catalyst reaction is conducted under the hydrogen condition, and a product is collected after condensation to obtain the tributylamine.

Description

technical field [0001] The invention relates to a synthesis method of an organic compound, in particular to a synthesis method of a chemical intermediate-tri-n-butylamine, as well as a used catalyst and a preparation method. Background technique [0002] Tri-n-butylamine, whose molecular formula is C 12 h 27 N, whose structural formula is shown in S-1, has a molecular weight of 185.35, and a boiling point of 216.0-217.0°C under normal pressure. Tri-n-butylamine is a colorless or light yellow liquid at normal temperature and pressure, has a special smell, is weakly alkaline, easily soluble in ethanol, ether, etc., and slightly soluble in water. It has a wide range of industrial uses, is an important organic chemical intermediate, and is also an excellent reagent, emulsifier, extractant, insecticide and preservative. [0003] [0004] Comprehensive literature report, according to the difference of raw material and catalyzer, the preparation method of tri-n-butylamine mai...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C211/07C07C209/64
Inventor 冯烈陈云斌顾海燕骆晨希钱超陈新志
Owner ZHEJIANG JIANYE CHEM
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