Joint production method for cyclohexylamine and dicyclohexylamine and catalyst system applied to method

A dicyclohexylamine and catalyst technology, applied in the field of organic compound preparation, can solve the problems of increasing the difficulty of industrialization, high labor intensity, and low purity of dicyclohexylamine rectification, so as to improve operation safety and reduce equipment cost. investment, the effect of reducing production costs

Active Publication Date: 2019-03-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction pressure of the present invention is low, and the material requirement of equipment is low, but the shortcoming of the present invention is that the yield of cyclohexylamine is low, only about 93%, and the present invention does not illustrate the dicyclohexylamine with higher added value simultaneously. The yield of amine
The disadvantages of the present invention are that the raw material cyclohexanone oxime is not easy to obtain, and industrialization is difficult; the total yield of cyclohexylamine and dicyclohexylamine is low, and the rectification purity of dicyclohexylamine is low, which cannot meet the requirements of the high-end market. need
The disadvantage of the present invention is that the conversion rate of phenol is on the low side, and phenol needs to be recycled, which increases the difficulty of industrialization
The disadvantage of the present invention is that cyclohexylamine and dicyclohexylamine are prepared by one-step hydrogenation method, and there will be many impurities in the reaction solution, which will increase the difficulty of product separation and purification. In addition, the batch process is adopted, which has high labor intensity and safety factor. Low
The disadvantages of the present invention mainly contain three: one is that the catalyst adopts oxide extrusion molding, and the utilization rate of active components in the catalyst is relatively low; the other is that the reaction temperature and reaction pressure of the present invention are relatively high, and the reaction temperature is 160-230°C , easy to produce heavy components, affecting the separation and purification of dicyclohexylamine; the reaction pressure is 10-30MPa, which requires high pressure resistance of the reactor, which is a major hazard; the third is to improve the selectivity of dicyclohexylamine. The invention is mainly achieved by increasing the reaction temperature, but this will lead to a significant decrease in the life of the catalyst

Method used

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  • Joint production method for cyclohexylamine and dicyclohexylamine and catalyst system applied to method
  • Joint production method for cyclohexylamine and dicyclohexylamine and catalyst system applied to method
  • Joint production method for cyclohexylamine and dicyclohexylamine and catalyst system applied to method

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Experimental program
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Effect test

Embodiment 1

[0043] 1# Preparation of supported Rh-Ni catalyst:

[0044] The spherical γ-Al 2 O 3 (Particle size 3mm, specific surface area 300m 2 / g) Calcination at 450°C for 4h. Use 100ml deionized water to prepare a nitrate impregnation solution containing 3g Rh, 5g Ni, 1g Re, 0.3g Zn, heat to 80℃ to form a homogeneous solution, and then add 90.7g γ-Al 2 O 3 The carrier is rotated and immersed in a water bath at 80°C for 4 hours, and then the water is gradually evaporated to dryness, and then baked in an oven at 120°C for 12 hours; finally moved to a muffle furnace, heated at 2-3°C / min to 500°C in an air atmosphere, and baked 6 After hours, the catalyst can be obtained after natural cooling. The composition of the catalyst is: Rh is 3wt%, Ni is 5wt%, Re is 1wt%, Zn is 0.3wt%, and the rest is γ-Al 2 O 3 , Based on the corresponding metal elements in the total mass of the catalyst.

Embodiment 2

[0046] 2# Preparation of supported Rh-Co catalyst:

[0047] The spherical γ-Al 2 O 3 (Particle size 3mm, specific surface area 300m 2 / g) Calcination at 450°C for 4h. Use 150ml deionized water to prepare a nitrate impregnation solution containing 3g Rh, 10g Co, 0.5g Re, 0.5g Mo, heat to 80℃ to form a homogeneous solution, and then add 86g γ-Al 2 O 3 The carrier is rotated and immersed in a water bath at 80°C for 4 hours, and then the water is gradually evaporated to dryness, and then baked in an oven at 120°C for 12 hours; finally moved to a muffle furnace, heated at 2-3°C / min to 500°C in an air atmosphere, and baked 6 After hours, the catalyst can be obtained after natural cooling. The composition of the catalyst is: Rh is 3wt%, Co is 10wt%, Re is 0.5wt%, Mo is 0.5wt%, and the rest is γ-Al 2 O 3 , Based on the corresponding metal elements in the total mass of the catalyst.

Embodiment 3

[0049] 3# Preparation of supported Rh-Ni catalyst:

[0050] The spherical silica (particle size 3mm, specific surface area 240m 2 / g) Calcination at 450°C for 4h. Prepare a nitrate impregnation solution containing 2g Rh, 10g Ni, 0.75g Re, 0.5g Zn with 150ml deionized water, heat to 80℃ to form a homogeneous solution, then add 86.75g silica carrier and rotate in a water bath at 80℃ After being immersed for 4 hours, the water is gradually evaporated and dried in an oven at 120°C for 12 hours; finally moved to a muffle furnace, heated at 2-3°C / min to 550°C for 8 hours in an air atmosphere, and the catalyst can be obtained after natural cooling . The composition of the catalyst is: Rh is 2wt%, Ni is 10wt%, Re is 0.75wt%, Zn is 0.5wt%, and the rest is silica, based on the corresponding metal elements in the total mass of the catalyst.

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Abstract

The invention discloses a joint production method for cyclohexylamine and dicyclohexylamine and a catalyst system applied to the method. The method comprises the following steps: (1) enabling the rawmaterials of phenylamine, cyclohexanone, ammonia and hydrogen to pass through a first section of a reactor which an Rh-Ni catalyst is filled into and loaded on to obtain first reaction liquid; (2) enabling the first reaction liquid pass through a second section of the reactor which an Rh-Co catalyst is filled into and loaded on to obtain reaction liquid containing the cyclohexylamine and the dicyclohexylamine. The combined production method disclosed by the invention has the advantages that the raw materials are cheap and easy to obtain, the conversion rate is high, product selectivity is good, service life of catalysts is long, technological processes are simple, a continuous technology is utilized, an automation degree is high, labor intensity is low, production cost is low, and the dicyclohexylamine with a high added value can be jointly produced; furthermore, product composition can be adjusted by changing reaction conditions according to the market need situation of the products;thus, the joint production method is suitable for industrial mass production.

Description

Technical field [0001] The invention relates to a method for preparing organic compounds, and more specifically to a method for co-producing cyclohexylamine and dicyclohexylamine and a catalyst system used in the method. Background technique [0002] Cyclohexylamine is an important fine chemical intermediate and an extremely versatile raw material for the organic synthesis industry. It can be used to prepare cyclohexanol, cyclohexanone, caprolactam, cellulose acetate, nylon 6, etc. Cyclohexylamine itself is a solvent and can be used in resins, coatings, fats, and paraffin oils. It can also be used to prepare desulfurizers, rubber antioxidants, vulcanization accelerators, chemical additives for plastics and textiles, boiler feedwater treatment agents, metal corrosion inhibitors, emulsifiers, preservatives, antistatic agents, latex coagulants, petroleum additives , Fungicides, insecticides and dye intermediates. There are five main synthesis methods: aniline catalytic hydrogenati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/72C07C209/26C07C209/52C07C209/22C07C211/35B01J23/89
CPCC07C209/22C07C209/26C07C209/52C07C209/72B01J23/002B01J23/8986B01J23/8993C07C2601/14B01J2523/00C07C211/35B01J2523/27B01J2523/31B01J2523/74B01J2523/822B01J2523/847B01J2523/68B01J2523/73B01J2523/845B01J2523/41
Inventor 刘振国张聪颖李鑫张兵周亚文魏运恒
Owner WANHUA CHEM GRP CO LTD
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