Preparation method of cyclohexylamine

A technology of cyclohexylamine and catalyst, which is applied in the field of preparation of chemical product cyclohexylamine, can solve the problems of high cost and environmental pollution, and achieve the effects of long life, high yield and simple preparation process

Inactive Publication Date: 2008-04-16
HANERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process technology is mature, the raw materials are easy to obtain, and the yield is also high, but the tra...

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0009] Choose γ-Al with an average pore size of 6-8nm and a diameter of φ3mm 2 o 3 30 grams were dried and dehydrated at 250°C for 5 hours, and put into a beaker as a carrier skeleton. Weigh 8 grams of Mg(NO 3 ) 2 ·6H 2 O and 6.9 g Al(NO 3 ) 3 9H 2 O, add 34 grams of distilled water to prepare a mixed solution, pour this solution into the γ-Al 2 o 3 In a beaker, equal-volume impregnation was performed twice. Then dry at 120°C for 6 hours, bake at 1000°C for 6 hours, and cool to obtain a magnesium-aluminum spinel carrier; weigh 1.5 grams of NaHCO 3 Make 10ml solution, impregnate the carrier and dry at 120°C for 6 hours; then weigh 0.25g of PdCl 2 , add 10ml of 10% dilute hydrochloric acid to dissolve, after dissolving, impregnate with equal volume twice with the carrier prepared above, wash with distilled water until there is no chloride ion and sodium ion, then dry at 120°C for 6 hours, and then dry at 500°C Lower roasting for 8 hours.

[0010] The prepared catalys...

Embodiment 2

[0012] Catalyst preparation process is the same as embodiment 1, and the loaded palladium amount of catalyzer changes 0.2% (weight), MgO: Al 2 o 3 =1:4, MgO+Al 2 o 3 The total impregnation amount of is 10%; The phenol feed rate is 2.5 grams / hour, and other reaction conditions are constant, and the transformation rate of phenol is 94.1%, and the selectivity of cyclohexylamine is 74.5%, and the selectivity of dicyclohexylamine is 13.6%.

Embodiment 3

[0014] Choose γ-Al with an average pore size of 12.7nm 2 o 3 As the catalyst carrier skeleton, the catalyst preparation process and preparation conditions are the same as in Example 1, and the reaction conditions are also the same as in Example 1. The conversion rate of phenol is 93.1%, the selectivity of cyclohexylamine is 76.5%, and the selectivity of dicyclohexylamine is 14.7%.

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Abstract

The present invention discloses a preparation method of cyclohexylamine, in which phenol, H2, and NH3 are adopted as the raw materials, the catalyst used by the present invention adopts gamma-Al2O3 as the carrier skeleton, and magnesia-alumina spinal carrier is made through impregnating the mixed solution of nitric magnesium and nitric aluminum, then the chloride palladium hydrochloric acid solution is impregnated to obtain the hydrogenated and aminated catalyst of Pd/Al2O3-MgO/Al2O3. Then the catalyst is added into an integral reactor, firstly activated under ordinary pressure through conducting the hydrogen gas, then phenyl, hydrogen gas and ammonia gas in proportion under about 180 DEG C are conducted to produce cyclohexylamine. Compared with the aniline hydrogenation reduction generally adopted both domestically and worldwide, the present invention with simple technics has the advantages of firstly low cost, with cheaper phenol to substitute for aniline as the raw material for the preparation of cyclohexylamine; secondly the catalyst with high activity and a long life ; thirdly high yield of product with high selectivity and 4, minor pollution, with capability to meet the principle of green chemical industrial technology.

Description

Technical field: [0001] The invention belongs to the preparation technology of chemical product cyclohexylamine. Background technique: [0002] Cyclohexylamine (also known as hexahydroaniline or amino bad hexane, English name cyclohexylamine) is an important fine chemical intermediate, mainly used in the production of petroleum product additives, metal corrosion inhibitors, rubber vulcanization accelerators and anti-aging agents, food and Feed additives and other products. At present, there are four main process routes, namely hydrogenation reduction of aniline, reduction of nitrocyclohexane, catalytic amination of cyclohexanone and catalytic amination of cyclohexanol. The hydrogenation reduction method of aniline is commonly used in China. The process technology is mature, the raw material is easy to obtain, and the yield is also high, but the traditional production process of the raw material aniline can cause great pollution to the environment, and the cost is high. In...

Claims

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Application Information

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IPC IPC(8): C07C211/35C07C209/60C07C209/72B01J23/44B01J21/10
Inventor 肖钢侯晓峰
Owner HANERGY TECH
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