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Method for preparing N,N-dimethylcyclohexylamine and N-methyl-dicyclohexylamine

A technology of methyldicyclohexylamine and dimethylcyclohexylamine, which is applied in the field of preparing polyurethane catalysts, can solve problems such as poor selectivity, low product yield, and harmful environment, and achieve low production cost, high product yield, High conversion effect

Active Publication Date: 2015-09-09
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this patent is that the raw material uses foul-smelling dimethylamine aqueous solution, which not only causes harm to the environment, but also increases the difficulty and cost of post-processing, and in addition cannot realize continuous production
The weak point of this invention is that the single-pass conversion rate of cyclohexanol is low, and the selectivity of N,N-dimethylcyclohexylamine is poor. Under optimal conditions, the conversion rate of cyclohexanol is only 89.12%. N,N - The selectivity of dimethylcyclohexylamine is 93.75%, in addition dimethylamine is very harmful to the environment
[0009] (1) High value-added N-methyldicyclohexylamine cannot be produced during the preparation of N,N-dimethylcyclohexylamine, and the reaction time is long, the operation process is complicated, the product yield is low or the conversion rate of continuous raw materials Low
[0010] (2) The raw materials of the reaction have high requirements on materials or are harmful to the environment

Method used

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  • Method for preparing N,N-dimethylcyclohexylamine and N-methyl-dicyclohexylamine
  • Method for preparing N,N-dimethylcyclohexylamine and N-methyl-dicyclohexylamine
  • Method for preparing N,N-dimethylcyclohexylamine and N-methyl-dicyclohexylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparation of 1# nickel-based catalyst:

[0042] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 250m 2 / g, pore volume 0.45cc / g) was calcined at 450°C for 4h. Dissolve 123.88g of nickel nitrate hexahydrate, 19.23g of chromium nitrate nonahydrate, and 1.91g of copper nitrate trihydrate in 500ml of deionized water, heat to 80°C to form a homogeneous solution, and then add 472g of 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: Ni is 5wt%, Cr is 0.5wt%, Cu is 0.1wt%, and the rest is γ-Al 2 o 3 , based on the corresponding metal element in the total mass of the catalyst.

Embodiment 2

[0044] Preparation of 2# cobalt catalyst:

[0045] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 250m 2 / g, pore volume 0.45cc / g) was calcined at 450°C for 4h. Dissolve 123.47g of cobalt nitrate hexahydrate, 6.47g of potassium nitrate, and 0.92g of ammonium heptamolybdate tetrahydrate in 500ml of deionized water, heat to 80°C to form a homogeneous solution, and then add 472.0g of 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: Co is 5.0wt%, K is 0.5wt%, Mo is 0.1wt%, and the rest is γ-Al 2 o 3 , based on the corresponding metal element in the total mass of the catalyst.

Embodiment 3

[0047] Preparation of 3# nickel-based catalyst:

[0048] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 250m 2 / g, pore volume 0.45cc / g) was calcined at 450°C for 4h. Dissolve 247.75g of nickel nitrate hexahydrate, 19.23g of chromium nitrate nonahydrate, and 22.75g of zinc nitrate hexahydrate in 800ml of deionized water, heat to 80°C to form a homogeneous solution, and then add 442.5g of γ-Al 2 o 3 Carriers were rotated and dipped in a water bath at 80°C for 4 hours, then evaporated to dryness gradually, and baked in an oven at 120°C for 12 hours; finally moved to a muffle furnace, and were heated to 500°C in an air atmosphere at 2-3°C / min for 8 Hours, the catalyst can be obtained after natural cooling. The composition of the catalyst is: Ni is 10wt%, Cr is 0.5wt%, Zn is 1wt%, and the rest is γ-Al 2 o 3 , based on the corresponding metal element in the total mass of the catalyst.

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Abstract

The invention discloses a method for preparing N,N-dimethylcyclohexylamine and N-methyl-dicyclohexylamine, which comprise the following steps: under certain reaction temperature and pressure condition, cyclohexanone, ammonia, hydrogen and formaldehyde pass through a two-stage reactor to obtain the N,N-dimethylcyclohexylamine and N-methyl-dicyclohexylamine. The method has the advantages of easily available raw material with low cost, high conversion rate, good product selectivity, little by-product, simple flow, and low production cost, N-methyl-dicyclohexylamine with high added value can be obtained through combined production, product composition can be adjusted by changing the reaction condition according to the market demand condition of the product, and the method is suitable for industrial large scale production.

Description

technical field [0001] The invention relates to a method for preparing a polyurethane catalyst, in particular to a method for co-producing N,N-dimethylcyclohexylamine and N-methyldicyclohexylamine. Background technique [0002] N-methyldicyclohexylamine is a gel co-catalyst for polyurethane molded foam and polyurethane rigid foam, which can promote skin curing and increase the hardness of polyether polyurethane block foam. It can be used as a catalyst for low-density soft foam, molded soft foam, packaging foam and as an auxiliary catalyst for rigid foam. It can be used with N,N-dimethylcyclohexylamine and used for high resilience molded foam, semi-rigid foam, polyurethane Self-crusting foam. The current production of N-methyldicyclohexylamine is mainly obtained by the reaction of dicyclohexylamine and formaldehyde. [0003] N,N-Dimethylcyclohexylamine is a low-viscosity, moderately active amine catalyst that can catalyze both gelation and foaming, and can provide a relativ...

Claims

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Application Information

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IPC IPC(8): C07C211/35C07C209/26
Inventor 刘振国张聪颖李鑫刘志鹏唐磊高占宇吴健王丛任树杰曹善健陈浩李文滨黎源
Owner WANHUA CHEM GRP CO LTD
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