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Method for preparing 1,3-cyclohexyl dimethylamine

The technology of cyclohexyldimethylamine and solvent is applied in the field of preparation of pesticide intermediates, which can solve the problem of high cost and achieve the effects of easy rectification, simple process operation and high yield.

Inactive Publication Date: 2013-02-06
SHANGHAI CAC CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since MXDA is obtained by hydrogenation of IPN, the cost of preparing 1,3-BAC from MXDA is too high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Drop into 60g m-xylylenediamine successively in the autoclave, 120g dioxane, 5.62g50% sodium hydroxide solution and 8g Raney nickel catalyst, close the still, use H 2 After three replacements, H 2 To 5MPa, stir and heat to 60°C, then inflate to 6MPa, wait for the reaction to absorb hydrogen, when the pressure drops to 5MPa, inflate to 6MPa, repeat the operation until no hydrogen is absorbed, and the reaction is about 80 minutes at this time. Cool to room temperature, vent the hydrogen, open the kettle, pour out the supernatant liquid (MXDA reaction liquid), and use the catalyst in the lower layer.

[0021] Drop into a certain amount of above-mentioned MXDA reaction solution and the ruthenium carbon catalyst of 4g5% successively in autoclave, close still, use H 2 After three replacements, H 2 To 6MPa, stir and heat to 90°C, then inflate to 7MPa, react to absorb hydrogen, when the pressure drops to 6MPa, inflate to 7MPa, repeat this operation until no more hydrogen is a...

Embodiment 2

[0023] In the autoclave, drop into 37.5g m-xylylenediamine successively, 150g dioxane, 5.7g50% sodium hydroxide solution and 8g Raney nickel catalyst, close the still, use H 2 After three replacements, H 2 To 5MPa, stir and heat to 70°C, then inflate to 6MPa, react to absorb hydrogen, when the pressure drops to 5MPa, inflate to 6MPa, repeat the operation until no more hydrogen is absorbed, and the reaction is about 60 minutes at this time. Cool to room temperature, vent and open the kettle, pour out the supernatant (MXDA reaction solution), and use the lower layer catalyst.

[0024] Drop into a certain amount of above-mentioned MXDA reaction solution and the ruthenium carbon catalyst of 4g5% successively in autoclave, close still, use H 2 After three replacements, H 2 To 6MPa, stir and heat to 100°C, then inflate to 7MPa, wait for the reaction to absorb hydrogen, when the pressure drops to 6MPa, inflate to 7MPa, repeat this operation until no more hydrogen is absorbed, and t...

Embodiment 3

[0026] In the autoclave, drop into 37.5g m-xylylenediamine successively, 150g dioxane, 5.7g50% sodium hydroxide solution and 8g Raney nickel catalyst, close the still, use H 2 After three replacements, H 2 To 5MPa, stir and heat to 70°C, then inflate to 6MPa, wait for the reaction to absorb hydrogen, when the pressure drops to 5MPa, inflate to 6MPa, repeat this operation until no more hydrogen is absorbed, and the reaction is about 100 minutes at this time. Cool to room temperature, vent and open the kettle, pour out the supernatant (MXDA reaction solution), and use the lower layer catalyst.

[0027] Drop into a certain amount of above-mentioned MXDA reaction liquid and the ruthenium carbon catalyst of 5g5% successively in autoclave, close still, use H 2 After three replacements, H 2 To 6MPa, stir and heat to 100°C, then inflate to 7MPa, wait for the reaction to absorb hydrogen, when the pressure drops to 6MPa, inflate to 7MPa, repeat the operation until no hydrogen is absor...

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PUM

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Abstract

The invention relates to a method for preparing 1,3-cyclohexyl dimethylamine. Two steps of hydrogenation are carried out under the same solvent, the first step of hydrogenation uses raney nickel as a catalyst, one or more of methanol, methylamine or 1,4-dioxane is or are used as the solvent, and organic amine, liquid ammonia, water or sodium hydroxide are used as an addition agent. Under the condition of 40-80 DEG C of reaction temperature and 5-8 MPa of reaction pressure, isophthalonitrile and hydrogen are reacted, the reaction time is 1-5 hours, and an isophthalonitrile reaction solution is obtained. The second step of hydrogenation uses ruthenium-supported activated carbon as the catalyst. Under the condition of 80-130 DEG C of reaction temperature and 5-8 MPa of reaction pressure, the isophthalonitrile reaction solution and hydrogen are reacted, the reaction time is 1-6 hours, and 1,3-cyclohexyl dimethylamine is obtained. The total yield of the method can reach 90 percent. The method has the advantages of simplicity in process operation, high yield and easiness in rectification, can be directly improved on the current MXDA production process, and is easy for industrialization.

Description

technical field [0001] The invention relates to a method for preparing a pesticide intermediate, in particular to a method for preparing 1,3-cyclohexyldimethylamine. Background technique [0002] 1,3-BAC, the Chinese name is 1,3-cyclohexyldimethylamine or 1,3-diaminomethylcyclohexane, the English name is 1,3-Bis(aminomethyl)Cyclohexane or 1,3-Cyclohexanedimethanamine( CA name), [0003] Molecular formula is C 8 h 18 N 2 , 1,3-BAC is a colorless, transparent liquid with a slight ammonia smell, with a boiling point of 220°C, a freezing point below -70°C, a flash point of 113°C (Cleveland open cup), a specific gravity (20°C) of 0.942, and a viscosity of 9.06 ( cp, 20°C), vapor pressure 14mmHg (120°C). Soluble in water, alcohol, ether, n-hexane, cyclohexane, benzene and other solvents. It is mainly used as curing agent for epoxy resin, polyurethane intermediate and anti-corrosion and anti-rust agent. [0004] Nowadays, Mitsubishi Gas, BASF and other manufacturers mainly p...

Claims

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Application Information

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IPC IPC(8): C07C211/36C07C209/72
Inventor 王海波潘逢亮黄志文
Owner SHANGHAI CAC CHEM