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Preparation process of N,N-dimethylcyclohexylamine

A technology for the preparation of dimethylcyclohexylamine, which is applied to the preparation of amino compounds, the preparation of organic compounds, organic chemistry, etc., can solve the problems of high pressure and high production cost, and achieve low production cost, high product yield, good safety effect

Inactive Publication Date: 2010-08-11
LIAOCHENG UNIV
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  • Abstract
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Problems solved by technology

What Chinese patent (CN93110708.3; Ji Wenfu 1994.9.14) announces is to be raw material with cyclohexanone, dimethylamine and hydrogen, synthesize DMCHA under the condition of high pressure and palladium charcoal Pd / C catalysis, owing to have used hydrogen, precious metal catalyst and higher pressure, higher production costs, and production safety issues

Method used

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  • Preparation process of N,N-dimethylcyclohexylamine
  • Preparation process of N,N-dimethylcyclohexylamine

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Embodiment 1

[0013] Embodiment 1: Preparation of N, N-dimethylcyclohexylamine: In a 0.5 liter reactor equipped with an electric stirrer, reflux condensing device, and feeding funnel device, 50 grams of cyclohexylamine were added, and 135 grams of cyclohexylamine were added dropwise under stirring. 85% formic acid solution, stirred at 300 rpm for 0.5 hour, added 90 g of 36% formaldehyde solution, reacted at 90°C for 3 hours, cooled the reaction mixture, and brought it to room temperature, added an appropriate amount of sodium hydroxide solution to alkalize, water After steam distillation, the fraction at 160-163°C was collected, which was N,N-dimethylcyclohexylamine, and the yield was 82%.

[0014] Utilize FTIRNicolet-460 infrared spectrometer (liquid film method) to product analysis, draw conclusion as follows: figure 1 Shown, IR(v / cm -1 ): 2926, 2852, 2825, 2775 are antisymmetric and symmetric stretching vibration absorption of C-H; 1450, 1376 are -CH respectively 3 Antisymmetric and sy...

Embodiment 2

[0015] Embodiment 2: prepare N, N-dimethylcyclohexylamine: in the 1 liter reactor that electric stirrer, reflux condensing device, feeding funnel device are housed, add 110 grams of cyclohexylamine, add dropwise 270 grams under stirring 85% formic acid solution, stirred at 500 rpm for 1 hour, added 180 g of 36% formaldehyde solution, reacted for 4 hours at 95°C, cooled the reaction mixture, and brought it to room temperature, added an appropriate amount of sodium hydroxide solution to alkalize, water After steam distillation, the fraction at 160-163°C was collected, which was N,N-dimethylcyclohexylamine, and the yield was 84%.

Embodiment 3

[0016] Embodiment 3: prepare N, N-dimethylcyclohexylamine: in 10 liters of reactors that electric stirrer, reflux condensing device, feeding funnel device are housed, add 1100 grams of cyclohexylamines, add dropwise 2700 grams under stirring 85% formic acid solution was stirred for 1.5 hours at a speed of 500 rev / s, and 1800 g of 36% formaldehyde solution was added, and reacted for 5 hours at 98° C., and the reaction mixture was cooled to room temperature, and an appropriate amount of sodium hydroxide solution was added to make it alkaline, and water After steam distillation, the fraction at 160-163°C is collected, which is N,N-dimethylcyclohexylamine, and the yield is 86%.

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Abstract

The invention discloses a preparation process of N,N-dimethylcyclohexylamine, which comprises the steps of: adding 50-1100g of cyclohexane into a reaction kettle with capacity of 0.5-10L, wherein the reaction kettle is provided with an electric stirrer, a reflux condensing device and a charging funnel device; dropping 135-2700g of formic acid solution with mass concentration of 85-90 percent under the stirring, and stirring for 1-2h at a rotating speed of 300-600 turns / second; adding 90-1800g of formaldehyde solution with mass concentration of 35-38 percent, and reacting for 3-5h at a temperature of 90-98 DEG C; cooling a reaction mixture to room temperature, adding a defined amount of sodium hydroxide solution for alkalization, carrying out steam distillation and collecting a fraction with a temperature of 160-163 DEG C to obtain the N,N-dimethylcyclohexylamine with the yield of 82-86 percent. The invention has the characteristics of simple process, mild reaction condition, low production cost, good safety, higher yield and purity of the product, and the like.

Description

technical field [0001] The invention relates to a preparation process of N,N-dimethylcyclohexylamine. Background technique [0002] N,N-Dimethylcyclohexylamine (DMCHA) is a blowing agent mainly used in polyurethane rigid foam, semi-rigid foam and flexible foam. Because DMCHA is easy to use and operate, has good storage stability, large tolerance, easy adjustment, stable foaming, and fine and uniform foamed plastics, it is more suitable as a catalyst for the foaming of rigid foamed plastics for refrigerator insulation materials. [0003] The existing synthetic methods of DMCHA can be divided into four classes according to raw materials: N, N-dimethylaniline hydrogenation method, phenol method, cyclohexylamine method, cyclohexanone method (USP4521624, Jackisch, June 4, 1985). What Chinese patent (CN93110708.3; Ji Wenfu 1994.9.14) announces is to be raw material with cyclohexanone, dimethylamine and hydrogen, synthesize DMCHA under the condition of high pressure and palladium ...

Claims

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Application Information

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IPC IPC(8): C07C211/35C07C209/00
Inventor 牛梅菊魏新庭刘贵华王大奇
Owner LIAOCHENG UNIV
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