Synthesis method for continuously producing N,N-dimethyl cyclohexyl amine

A technology of dimethylcyclohexylamine and a synthesis method, which is applied in the field of continuous production of N, can solve the problems of low utilization rate of raw materials and catalysts, difficult closed-circuit circulation, large energy consumption, etc. Good, low consumption of raw materials

Active Publication Date: 2010-01-06
ZHEJIANG XINHUA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The characteristics of the batch reactor reaction production process determine that the production process is difficult to achieve closed-circuit circulation in the system, the energy consumption is large, the utilization rate of raw materials and catalysts is relatively low, there are many three wastes, and the pressure on environmental protection is high.

Method used

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  • Synthesis method for continuously producing N,N-dimethyl cyclohexyl amine
  • Synthesis method for continuously producing N,N-dimethyl cyclohexyl amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The synthetic method of this N,N-dimethylcyclohexylamine:

[0019] First prepare the catalyst:

[0020] Industrial Co / Al 2 o 3 The catalyst is a catalyst, numbered A1, and the composition (weight ratio) of the catalyst is: Cu is 5.0%, Co is 25.0%, Ti is 0.1%, Mn is 0.2%, Cr is 0.1%, and the rest is Al 2 o 3 .

[0021] Industrial Co / Al 2 o 3 The catalyst is a catalyst, coded as A2, and the composition (weight ratio) of the catalyst is: Cu is 5.0%, Co is 20.0%, Ti is 1.0%, Mn is 3.0%, Cr is 1.0%, and the rest is diatomaceous earth.

[0022] Industrial Co / Al 2 o 3 Catalyst is catalyst, numbering is A3, and the composition (weight ratio) of catalyst is: Cu is 5.0%, Co is 25.0%, and the rest is Al 2 o 3 .

[0023] 1), with cyclohexanol and dimethylamine as raw materials, with the Co / Al prepared above 2 o 3 A catalyst is a catalyst.

[0024] 2), the reaction is carried out in the vapor phase in the presence of hydrogen, using a continuous process.

[0025] 3) C...

Embodiment 2--- Embodiment 6

[0026] Embodiment 2 --- Embodiment 6: the catalyst in embodiment 1 is charged into a stainless steel reactor with an inner diameter of 25 mm and a length of 1500 mm. The catalyst loading height is 1200mm, and the catalyst loading volume is 600ml. The reaction raw materials are top-in and bottom-out. The material flowing out from the bottom of the reactor enters the separator after being condensed and cooled. The gas phase ammonia and hydrogen are discharged from the top of the separator. The mol ratio of a kind of mixed gas is 20%, and embodiment 5---6, the mol ratio that hydrogen accounts for three kinds of mixed gases is 30%. The composition was analyzed by gas chromatography, and the specific reaction conditions and results are listed in the table below.

[0027] Reaction conditions and results

[0028]

[0029] From the data in the above table, it can be seen that the content of Co in the catalyst is the main content, followed by the content of Cu, and a small amount ...

Embodiment 7

[0030] Example 7...Example 11: According to the device, process and catalyst described in Examples 2-6, the loading amount of the catalyst is 600ml, and a 240-hour stable operation test is carried out. Reaction pressure 1.0MPa, temperature 160°C, alcohol liquid space velocity 0.5h -1 , the amine-alcohol molar ratio is 1, and the molar ratio of hydrogen to the three mixed gases is 25%. The composition was analyzed by gas chromatography, and the specific reaction conditions and results are listed in the table below.

[0031] 240-hour stability operation test

[0032]

[0033] It can be seen from the data in the above table that under the process conditions, the conversion rate of the reaction is higher than 70%, the selectivity is higher than 80%, and the catalyst has better stability.

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Abstract

The invention discloses a chemical synthesis method, in particular a synthesis method for continuously producing N,N-dimethyl cyclohexyl amine, taking cyclohexanol and dimethylamine as raw materials and carrying out closed loop circulation in the whole process. In the chemical synthesis method, the reaction is performed by taking Co / Al2O3 as a catalyst, and controlling the pressure, the temperature, the mol ratio of the cyclohexanol to the dimethylamine and the consumption of the catalyst to 0.01-3.5m3 / (hr*m3 catalyst); condensing and the cooling, gas-liquid separation and gas phrase recycling are carried out on the reacted materials; and liquid phrase enters a rectification tower for separating and purifying the N, N-dimethyl cyclohexyl amine to obtain the finished product. The synthetic method has the advantages of simple flow, easy operation, high conversion rate of raw materials, good selectivity of products, few byproducts, simple separation flow, low consumption of the raw materials, obvious environment-friendly effect, low production cost of the products and convenience for industrial large-scale production.

Description

technical field [0001] The present invention relates to a chemical synthesis method, in particular to a method for continuously producing N,N-dimethylcyclohexylamine using cyclohexanol and dimethylamine as raw materials, using a fixed-bed reactor, and carrying out closed-circuit circulation in the whole process . Background technique [0002] N,N-Dimethylcyclohexylamine is a fine chemical product, which is widely used as a foaming catalyst for flexible polyurethane foam, semi-rigid foam and rigid foam, and is also used in the synthesis of cationic surfactants , intermediates of rubber accelerators and fabric treatment agents. Its physical characteristics are: Molecular formula C 8 h 17 N, molecular weight 127.23, boiling point 159°C, melting point <-77°C, density 0.849g / ml; CAS number: 98-94-2; colorless and transparent liquid, slightly soluble in water, miscible in alcohol, benzene, acetone, English name n, n-dimethylcyclohexylamine. [0003] N, N-dimethylcyclohexyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/35C07C209/16B01J23/889
Inventor 谢自强刘训军王爱民劳丽全兰昭洪
Owner ZHEJIANG XINHUA CHEM
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