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Process for co-production of cyclohexylamine and dicyclohexylamine and catalyst system for the process

A technology of dicyclohexylamine and catalyst, which is applied in the field of preparation of organic compounds, can solve the problems of high labor intensity, high reaction temperature and reaction pressure, low yield of cyclohexylamine, etc., so as to reduce production cost and speed up hydrogenation rate. , the effect of low content of heavy components

Active Publication Date: 2021-12-14
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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  • Process for co-production of cyclohexylamine and dicyclohexylamine and catalyst system for the process
  • Process for co-production of cyclohexylamine and dicyclohexylamine and catalyst system for the process
  • Process for co-production of cyclohexylamine and dicyclohexylamine and catalyst system for the process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0044] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 300m 2 / g) Calcined at 450°C for 4h. Use 100ml of deionized water to prepare a nitrate impregnation solution containing 3g Rh, 5g Ni, 1g Re, 0.3g Zn, heat to 80°C to form a homogeneous solution, and then add 90.7g γ-Al 2 o 3 Carrier, rotate and dip in a water bath at 80°C for 4 hours, then gradually evaporate to dryness, bake in an oven at 120°C for 12 hours; finally move to a muffle furnace, heat up to 500°C in an air atmosphere at 2-3°C / min for 6 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 element in the total mass of the catalyst.

Embodiment 2

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

[0047] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 300m 2 / g) Calcined 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°C to form a homogeneous solution, then add 86g γ-Al 2 o 3 Carrier, rotate and dip in a water bath at 80°C for 4 hours, then gradually evaporate to dryness, bake in an oven at 120°C for 12 hours; finally move to a muffle furnace, heat up to 500°C in an air atmosphere at 2-3°C / min for 6 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 element in the total mass of the catalyst.

Embodiment 3

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

[0050] Spherical silica (particle size 3mm, specific surface area 240m 2 / g) Calcined at 450°C for 4h. Use 150ml of deionized water to prepare a nitrate dipping solution containing 2g Rh, 10g Ni, 0.75g Re, and 0.5g Zn, heat to 80°C to form a homogeneous solution, then add 86.75g of silica carrier, and rotate in a water bath at 80°C After impregnating for 4 hours, gradually evaporate the water to dryness, bake in an oven at 120°C for 12 hours; finally move to a muffle furnace, heat up to 550°C in an air atmosphere at 2-3°C / min and bake for 8 hours, and the catalyst can be obtained after natural cooling . The composition of the catalyst is as follows: Rh is 2wt%, Ni is 10wt%, Re is 0.75wt%, Zn is 0.5wt%, and the rest is silicon dioxide, based on the corresponding metal elements accounting for the total mass of the catalyst.

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Abstract

The invention discloses a method for coproducing cyclohexylamine and dicyclohexylamine and a catalyst system used in the method. The method comprises the following steps: (1) passing the raw materials aniline, cyclohexanone, ammonia, and hydrogen through the first-stage reactor of the loaded Rh-Ni catalyst to obtain the first reaction solution; (2) the first reaction solution is loaded and loaded Rh-Co catalyst second section reactor, obtains the reaction solution containing cyclohexylamine and dicyclohexylamine. The invention has the advantages of cheap and easy-to-obtain raw materials, high conversion rate, good product selectivity, long catalyst life, simple process, continuous process, high degree of automation, low labor intensity, low production cost, and can obtain added value through co-production High dicyclohexylamine, and according to the market demand of the product, the composition of the product can be adjusted by changing the reaction conditions, which is suitable for industrialized large-scale production.

Description

technical field [0001] The invention relates to a method for preparing an organic compound, 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 in the organic synthesis industry. It can be used to prepare cyclohexanol, cyclohexanone, caprolactam, cellulose acetate and nylon 6, etc. Cyclohexylamine itself is a solvent and can be used in resins, paints, fats, and paraffin oils. It can also be used to prepare desulfurizer, rubber antioxidant, vulcanization accelerator, plastic and textile chemical additives, boiler feed water treatment agent, metal corrosion inhibitor, emulsifier, preservative, antistatic agent, latex coagulant, petroleum additive , fungicides, insecticides and dye intermediates. There are mainly five synthetic methods: catalytic hydrogenation of aniline, red...

Claims

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Application Information

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Patent Type & Authority Patents(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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