Method for preparing 1,3-cyclohexanedimethanamine

A technology for the reaction of cyclohexyldimethylamine and m-xylylenediamine, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of high cost, achieve easy rectification, simple process operation, The effect of high yield

Inactive Publication Date: 2018-06-26
QINGDAO XIANGZHI ELECTRONICS TECH CO LTD
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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

[0019] Put 60g of m-xylylenediamine, 120g of dioxane, 5.62g of 50% sodium hydroxide solution and 8g of Raney nickel catalyst in the autoclave successively, close the kettle, replace it with H2 for three times, feed H2 to 5MPa, and start stirring Heat to 60°C, then inflate to 6MPa, wait for the reaction to absorb hydrogen, and when the pressure drops to 5MPa, inflate to 6MPa, repeat this operation until no more 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.

[0020] Drop into a certain amount of above-mentioned MXDA reaction liquid and the ruthenium carbon catalyst of 4g5% successively in autoclave, close still, use

[0021] After replacing H2 three times, feed H2 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, repe...

Embodiment 2

[0023] In the autoclave, drop into 37.5g m-xylylenediamine, 150g dioxane, 5.7g50% sodium hydroxide solution and 8g Raney nickel catalyst successively, close the autoclave, replace with H2 after three times, pass into H2 to 5MPa, open Stir and heat to 70°C, then inflate to 6MPa, react to absorb hydrogen, when the pressure drops to 5MPa, inflate to 6MPa, repeat this operation until no more hydrogen is absorbed, and then react for about 60 minutes. Cool to room temperature, vent and open the kettle, pour out the supernatant (MXDA reaction solution), and use the lower layer catalyst.

[0024] Put a certain amount of the above-mentioned MXDA reaction solution and 4g of 5% ruthenium carbon catalyst in the autoclave in turn, close the autoclave, replace it with H2 three times, feed H2 to 6MPa, start stirring and heat to 100°C, then inflate to 7MPa, and wait for the reaction Absorb hydrogen, when the pressure drops to 6MPa, inflate to 7MPa, repeat the operation until no more hydrogen ...

Embodiment 3

[0026] In the autoclave, drop into 37.5g m-xylylenediamine, 150g dioxane, 5.7g50% sodium hydroxide solution and 8g Raney nickel catalyst successively, close the autoclave, replace with H2 after three times, pass into H2 to 5MPa, open Stir and heat to 70°C, then inflate to 6MPa, wait for the reaction to absorb hydrogen, and when the pressure drops to 5MPa, inflate to 6MPa, repeat the 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. Put a certain amount of the above MXDA reaction solution and 5g of 5% ruthenium carbon catalyst in the autoclave in turn, close the autoclave, replace it with H2 three times, feed H2 to 6MPa, start stirring and heat to 100°C, then inflate to 7MPa, and wait for the reaction Absorb hydrogen, when the pressure drops to 6MPa, inflate to 7MPa, repeat the operation until no...

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PUM

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Abstract

The invention relates to a method for preparing 1,3-cyclohexanedimethanamine. The method comprises the following steps: two-stage hydrogenation is performed in a same solvent, in first-stage hydrogenation, Raney nickel is used as a catalyst, one or more of methanol, methylamine and 1,4-dioxane are used as solvents, an organic amine, liquid ammonia, water or sodium hydroxide is used as an auxiliaryagent, under the conditions of the reaction temperature of 40-80 DEG C and the reaction pressure of 5-8MPa, isophthalonitrile reacts with a hydrogen gas, wherein the reaction time is 1-5h, so that anm-xylylenediamine reaction solution is obtained; and in second-stage hydrogenation, ruthenium supported activated carbon is used as a catalyst, under the conditions of the reaction temperature of 80-130 DEG C and the reaction pressure of 5-8MPa, the m-xylylenediamine reaction solution and a hydrogen gas continue to react, wherein the reaction time is 1-6h, and therefore the 1,3-cyclohexanedimethanamine is prepared, wherein the total yield of the 1,3-cyclohexanedimethanamine can be up to 90%. The method provided by the invention has simple operation and a high yield, the prepared 1,3-cyclohexanedimethanamine is easy to be rectified, and the method can be directly improved based on a current MXDA production process, and is easy to industrialize.

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), the molecular formula is C8H18N2, 1,3-BAC is a colorless transparent liquid with a slight ammonia smell, the boiling point is 220°C, the freezing point is below -70°C, the flash point is 113°C (Cleveland open cup type), the specific gravity ( 20°C) 0.942, viscosity 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. [0003] Nowadays, Mitsubishi Gas, BASF and other manufacturers mainly produce 1,3-BAC ab...

Claims

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Application Information

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IPC IPC(8): C07C209/48C07C211/18
CPCC07C209/48C07C211/18
Inventor 不公告发明人
Owner QINGDAO XIANGZHI ELECTRONICS TECH CO LTD
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