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Process for preparing compound of cyclohexdiol

A manufacturing method and technology of cyclohexanediol, applied in hydrogenation preparation, organic chemistry and other directions, can solve the problems of high cost, high temperature and high pressure hydrogenation reaction of refractory phenol, high price, etc. The effect of deep processing and utilization, reducing production cost

Inactive Publication Date: 2008-03-12
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the fact that general factories do not have high-pressure reactors, it is difficult for general factories to implement high-temperature and high-pressure hydrogenation reactions of diphenols
In addition, the method of Komachi uses expensive iodide as a reducing agent, the cost is too high, and there is no use value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: in the three-necked flask of 500 milliliters, install thermometer, stirrer, add hydroquinone (10 millimoles, 1.11 grams), Ni-Al alloy (10g), water (100 milliliters), then start stirring and heating to 90°C. A 1% aqueous sodium hydroxide solution (100 ml) was added dropwise over 1 hour. Control the reaction temperature to be 90°C-100°C. After the dropwise addition of the 1% aqueous sodium hydroxide solution was completed, stirring was continued at this temperature for 5 hours. Then it was cooled to room temperature, filtered, and the insoluble matter was removed by filtration, the aqueous solution was extracted with ethyl acetate, the organic layer was dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure. Then the concentrated product was analyzed by gas chromatography, the conversion rate of hydroquinone was 100%, and the yield rate of 1,4-cyclohexanediol was 84%.

Embodiment 2

[0015] Embodiment 2: in the three-necked flask of 500 milliliters, install thermometer, stirrer, add hydroquinone (10 millimoles, 1.11 grams), Ni-Al alloy (7g), water (100 milliliters), then start stirring and heating to 80°C. A 3% aqueous sodium hydroxide solution (100 ml) was added dropwise over 1 hour. The reaction temperature is controlled to be 80°C-100°C. After the dropwise addition of the 3% aqueous sodium hydroxide solution was completed, stirring was continued at this temperature for 7 hours. Then it was cooled to room temperature, filtered, and the insoluble matter was removed by filtration, the aqueous solution was extracted with ethyl acetate, the organic layer was dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure. Then the concentrated product was analyzed by gas chromatography, the conversion rate of hydroquinone was 100%, and the yield rate of 1,4-cyclohexanediol was 83%.

Embodiment 3

[0016] Embodiment 3: in the three-necked bottle of 500 milliliters, install thermometer, stirrer, add hydroquinone (10 millimoles, 1.11 grams), Ni-Al alloy (8g), water (100 milliliters), then start stirring and heating to 90°C. 8% cesium hydroxide aqueous solution (100 ml) was added dropwise over 1.5 hours. Control the reaction temperature to be 90°C-100°C. After the dropwise addition of the 8% cesium hydroxide aqueous solution was completed, stirring was continued at this temperature for 5 hours. Then it was cooled to room temperature, filtered, and the insoluble matter was removed by filtration, the aqueous solution was extracted with ethyl acetate, the organic layer was dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure. Then the concentrated product was analyzed by gas chromatography, the conversion rate of hydroquinone was 100%, and the yield rate of 1,4-cyclohexanediol was 82%.

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Abstract

The invention relates to a method for preparing cyclohexan diol compounding that belongs to organic compounding manufacture technology field. It directly drops buck onto dihydroxybenzene compounding, Ni-Al alloy, and water solution under the condition of whisking and heating to take reaction. Ni-Al alloy and buck would take reaction to produce hydrogen. The dihydroxybenzene would be deoxidized by hydrogen to form cyclohexan diol compounding. The invention supplies a method to take deep processing to petroleum product phenols. It has high industry application value. The invention takes reaction in water system, without any virulence harmful organic dissolvent.

Description

technical field [0001] The invention belongs to the technical field of organic compound production, in particular to a production method of cyclohexanediol compounds. Background of the invention [0002] Cyclohexanediol compounds are very important chemical intermediates, which are widely used in medicine, pesticides, household cosmetics and other industries. my country's phenol petroleum products have a large quantity and low prices. It is very important economic value to produce high value-added cyclohexanediol from phenols with cheap raw materials through hydrogenation reaction. The hydrogenation reaction of quinone generally needs to dissolve the quinone compound in an appropriate organic solvent, and then add Raney Ni or precious metal as a catalyst, such as Pt, Rh. The reaction conditions require high temperature (100-200°C) and high pressure (100-200 atm), so the catalytic hydrogenation reaction of diphenols generally needs to be carried out in special devices, such...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/19C07C35/14
Inventor 刘国斌张劫
Owner FUDAN UNIV
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