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Catalyst, preparation method thereof, and n-hexylamine production process using catalyst

A production process and catalyst technology, which is applied in the field of n-hexylamine production, can solve the problems of poor selectivity, low conversion rate and high reaction conditions, and achieve the effects of high conversion rate, corrosion avoidance and mild reaction conditions

Inactive Publication Date: 2019-10-08
山东达民化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing production process has relatively high reaction conditions, low conversion rate and poor selectivity.

Method used

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  • Catalyst, preparation method thereof, and n-hexylamine production process using catalyst
  • Catalyst, preparation method thereof, and n-hexylamine production process using catalyst
  • Catalyst, preparation method thereof, and n-hexylamine production process using catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of catalyst, described catalyst is Co-Zn / Al 2 o 3 , including the following components by weight: Co is 10.0%, Zn is 20.0%, and the rest is Al 2 o 3 .

[0020] A preparation method of catalyst, comprising the steps of: Al(OH) 3 Prepare a sodium metaaluminate solution with 40% NaOH, neutralize the precipitate with nitric acid, age, filter, wash, and roll into balls, dry, and roast to obtain spherical Al with a diameter of 1-3mm. 2 o 3 Carrier, the nitrate of Co and Zn is made into a mixed solution in proportion, for Al 2 o 3 The carrier is impregnated, dried and placed in a muffle furnace for calcination at 490°C for 6 hours. After cooling, it is impregnated with a mixed solution of Co and Zn nitrates again, and the catalyst is calcined under the same conditions. The bulk density of the catalyst was 0.90 g / ml. The catalyst number is A-1.

Embodiment 2

[0022] A kind of catalyst, described catalyst is Co-Zn / Al 2 o 3 , including the following components by weight: Co is 15.0%, Zn is 20.0%, and the rest is Al 2 o 3 .

[0023] A preparation method of catalyst, comprising the steps of: Al(OH) 3 Prepare a sodium metaaluminate solution with 40% NaOH, neutralize the precipitate with nitric acid, age, filter, wash, and roll into balls, dry, and roast to obtain spherical Al with a diameter of 1-3mm. 2 o 3 Carrier, the nitrate of Co and Zn is made into a mixed solution in proportion, for Al 2 o 3 The carrier is impregnated, dried and placed in a muffle furnace for calcination at 490°C for 6 hours. After cooling, it is impregnated with a mixed solution of Co and Zn nitrates again, and the catalyst is calcined under the same conditions. The bulk density of the catalyst was 0.90 g / ml. The catalyst number is A-2.

Embodiment 3

[0025] A kind of catalyst, described catalyst is Co-Zn / Al 2 o 3 , including the following components by weight: Co is 15.0%, Zn is 15.0%, and the rest is Al 2 o 3 .

[0026] A preparation method of catalyst, comprising the steps of: Al(OH) 3 Prepare a sodium metaaluminate solution with 40% NaOH, neutralize the precipitate with nitric acid, age, filter, wash, and roll into balls, dry, and roast to obtain spherical Al with a diameter of 1-3mm. 2 o 3 Carrier, the nitrate of Co and Zn is made into a mixed solution in proportion, for Al 2 o 3 The carrier is impregnated, dried and placed in a muffle furnace for calcination at 490°C for 6 hours. After cooling, it is impregnated with a mixed solution of Co and Zn nitrates again, and the catalyst is calcined under the same conditions. The bulk density of the catalyst was 0.90 g / ml. The catalyst number is A-3.

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Abstract

The invention discloses a catalyst, a preparation method thereof, and an n-hexylamine production process using the catalyst, and relates to the technical field of n-hexylamine production. The preparation method comprises the following steps: step 1, putting a prepared catalyst into a reactor, and carrying out reacting with pure hydrogen at pressure of 0.05MPa, at a temperature of 460 DEG C and ata space velocity of 1000 h<-1> for 24 hours, wherein the reaction is carried out in a gas phase, and a continuous process is adopted under set reaction conditions; and step 2, pumping n-hexane into avaporization preheater through a flow meter, mixing and pre-heating the n-hexane with ammonia gas and hydrogen, gasifying the mixture, feeding the gasified mixture into a fixed bed reactor for reacting, cooling the material obtained after the reaction by a condenser, carrying out gas-liquid separation, feeding the liquid phase into an azeotropic rectification tower for separation and purification,and carrying out vacuum rectification on the liquid phase product to obtain a normal hexane series mixed product. The reaction conditions of the process are mild, and a gas-solid reaction is adopted,so that corrosion of the liquid-phase materials to reaction equipment under a high-temperature high-pressure condition is avoided. Requirements on equipment materials are low, and fully continuous production can be realized.

Description

technical field [0001] The invention relates to the technical field of n-hexylamine production, in particular to a catalyst, a preparation method thereof and a n-hexylamine production process using the catalyst. Background technique [0002] N-hexylamine is a fine chemical raw material, mainly used in organic synthesis; used in intermediates of dyes, pigments, surfactants, and pharmaceutical synthesis; used in organic synthesis intermediates and biochemical reagents; Electronic chemicals such as etching solution formulations for OLED displays. The current preparation method of n-hexylamine: it is obtained by treating methyl n-hexyl ketone oxime with phosphorus pentachloride. Methyl n-hexyl ketone oxime was treated with phosphorus pentachloride in ether, then added water and stirred evenly, and the layers were separated. The N-acetyl n-ethylamine produced by the rearrangement was dissolved in ether, and the ether layer was separated. Ether was recovered by distillation, an...

Claims

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Application Information

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IPC IPC(8): B01J23/80C07C211/07C07C209/16
CPCB01J23/80C07C209/16C07C211/07
Inventor 陈国华郭文杰
Owner 山东达民化工股份有限公司
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