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Method for preparing alpha-isophorone

A technology of isophorone and acetone, which is applied in the field of preparation of α-isophorone, can solve the problem that the end point is not easy to control, and achieve the effect of easy control of the reaction

Inactive Publication Date: 2014-03-26
LANZHOU UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to solve the existing shortcoming that the reaction multi-step condensation makes the end point difficult to control when preparing α-isophorone by condensation of acetone, and to provide a method for preparing α-isophorone with easy controllable reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 450g of acetone, 100g of deionized water, 3.4090g of KOH and 135g of xylene into the autoclave in turn, and heat up under stirring conditions, from room temperature to 218°C. At this time, the pressure is 48bar, start timing, and after 2.0 hours of reaction, the temperature 221°C, pressure 47.5bar, sampling from the sampling port of the reactor, analyzed by gas chromatography, the conversion rate of acetone is 39.7%, the selectivity of α-isophorone is 69.61%, the total selectivity of mesityl oxide and isopropanol is 1.49% , basically no tetramolecular polymerization products. After the reaction solution is cooled, separate the water and xylene phases, recover the acetone and xylene by rectifying the xylene phase under normal pressure, and then separate α-isophorone by rectifying under reduced pressure. The number of boards is 20 pieces.

Embodiment 2

[0027] Add 600g of acetone, 133g of deionized water, 4.5460g of KOH and 180g of xylene into the autoclave in sequence, heat up under stirring conditions, from room temperature to 218°C, at this time the pressure is 50bar, start timing, react for 2.0h, and the temperature is 220°C ℃, pressure 49bar, sampling by gas chromatography analysis, acetone conversion rate 45.26%, α-isophorone selectivity 72.05%, mesityl oxide and isopropanol total selectivity 1.00%, basically no tetramolecular polymerization products.

Embodiment 3

[0029] Add 450g of acetone, 100g of deionized water, 3.4090g of KOH, and 135g of acetone into the autoclave in sequence, heat up to 217°C with a pressure of 48bar under stirring, start timing, and take a sample from the sampling port of the autoclave until the reaction reaches 2.0 hours. According to gas chromatography analysis, the conversion rate of acetone is 39.70%, the selectivity of α-isophorone is 69.61%, the total selectivity of mesityl oxide and isopropanol is 1.49%, and the reaction lasts for 2.5 hours. At this time, the temperature is 221°C and the pressure is 47bar. Sampling from the sampling port of the reaction kettle, the sampling condensate was analyzed by gas chromatography, the conversion rate of acetone was 47.31%, the selectivity of α-isophorone was 66.51%, the total selectivity of mesityl oxide and isopropanol was 1.67%, basically no four Molecular Polymerization Product.

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PUM

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Abstract

The invention discloses a method for preparing alpha-isophorone. The method comprises the step of generating the condensation reaction by acetone under the alkaline catalysis to obtain the alpha-isophorone. The method is characterized in that the condensation reaction is performed in a water and dimethylbenzene mixed solvent system. According to the method, the condensation reaction is performed in the water and dimethylbenzene mixed solvent system; after the condensation reaction is performed for certain time, the selectivity of the alpha-isophorone is basically stabilized; even if the condensation reaction continues to be performed, the influence on the selectivity of the alpha-isophorone, mesityl oxide and isopropyl-ketol is very small; the phenomenon that a reaction endpoint is required to be controlled by the conventional synthesis method is avoided, and the method disclosed by the invention is suitable for industrial production. According to the method disclosed by the invention, the acetone conversion rate is 25-55 percent; the selectivity of the alpha-isophorone is 65-80 percent, and the total selectivity of the mesityl oxide and the isopropyl-ketol is 0.5-10 percent.

Description

technical field [0001] The present invention relates to a method for preparing α-isophorone. Background technique [0002] α-Isophorone has a wide range of uses, and it is the raw material for plastics, adhesives, medicines, spices, epoxy resin curing agents, and paints. The synthesis of α-isophorone mainly adopts the liquid-phase condensation method, which is obtained by the alkali-catalyzed condensation of acetone. The existing methods mainly contain the following: [0003] In 1944, S.A. Ballard reported that using 20% ​​NaOH as a catalyst, reacting at 150°C for 3 hours, the conversion rate of acetone was 17%, and the selectivity of α-isophorone was 39%. In 1946, Ballard studied the concentration of different catalysts, the reaction The influence of time and feeding speed on the conversion rate of acetone and the selectivity of α-isophorone is obtained. The optimal condition is that acetone is reacted under 28% KOH aqueous solution for 40 minutes at 170 ° C, the conversio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/603C07C45/67
CPCC07C45/67C07C45/73C07C45/74C07C2601/16C07C49/603C07C49/203C07C49/17
Inventor 许鹏飞张磊梁立新胡秀琴李晓明毛志红张义新
Owner LANZHOU UNIVERSITY
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