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Method for synthesizing mesityl oxide and isophorone

A technology of composite oxides and composite catalysts, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve problems such as difficult processing, high production cost, low conversion rate of acetone, etc., to improve selectivity Effect

Pending Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The liquid-phase condensation method is the pressurized liquid-phase condensation of acetone in an alkaline solution. It is an industrial method mainly used abroad at present. This method has the advantages of simple catalyst and convenient operation. The disadvantage is that the reaction kettle is a high-pressure equipment and its internal structure is relatively complicated. , the conversion rate of acetone is not high, the production cost is high, the waste liquid contains a large amount of potassium hydroxide, it is difficult to handle, and the operation process of the distillation tower is not easy to control, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 40g of magnesium aluminum hydrotalcite and 12g of 30% alkaline silica sol, mix them evenly, extrude into a strip, let stand in the air for 8 hours to obtain mixture I, dry in an oven at 150°C for 4h, and then roast at 450°C for 6h to obtain compound II, Compound II was hydrothermally treated at 180°C for 48 hours to obtain Compound III. After compound III was dried, it was calcined again at 450°C for 6 hours to obtain magnesium-aluminum composite oxide IV, which is the desired catalyst. The catalyst performance evaluation test was carried out on a fixed-bed tubular reactor (Ф25×500mm stainless steel), with a catalyst loading of 10ml, evaluation conditions: temperature 300°C, normal pressure, space velocity 0.5h -1 . Gas chromatographic analysis: selectivity of mesityl oxide is 35%, selectivity of isophorone is 36%, total effective selectivity is 71%.

Embodiment 2

[0029] Weigh 40g of magnesium aluminum hydrotalcite, 20g of 30% alkaline silica sol, mix them evenly, extrude into a strip, let stand in the air for 8 hours to obtain mixture I, dry in an oven at 150°C for 4h, and then roast at 450°C for 6h to obtain compound II, Compound II was hydrothermally treated at 180°C for 48 hours to obtain Compound III. After compound III was dried, it was calcined again at 450°C for 6 hours to obtain magnesium-aluminum composite oxide IV, which is the desired catalyst. The catalyst performance evaluation test was carried out on a fixed-bed tubular reactor (Ф25×500mm stainless steel), with a catalyst loading of 10ml, evaluation conditions: temperature 310°C, normal pressure, space velocity 1h -1 . Gas chromatography analysis: mesityl oxide selectivity 38%, isophorone selectivity 34%, total effective selectivity 72%.

Embodiment 3

[0031] Weigh 40g of magnesium aluminum hydrotalcite and 40g of 30% alkaline silica sol, mix them uniformly, extrude into a strip, let stand in the air for 8 hours to obtain mixture I, dry in an oven at 150°C for 6h, and then roast at 450°C for 8h to obtain compound II. Compound II was hydrothermally treated at 180°C for 48 hours to obtain Compound III, which was dried and calcined again at 450°C for 8 hours to obtain magnesium-aluminum composite oxide IV, which is the desired catalyst. The catalyst performance evaluation test was carried out on a fixed-bed tubular reactor (Ф25×500mm stainless steel), with a catalyst loading of 10ml, evaluation conditions: temperature 310°C, normal pressure, space velocity 0.5h -1 . Gas chromatographic analysis: the selectivity of mesityl oxide is 40%, the selectivity of isophorone is 33%, and the total effective selectivity is 73%.

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Abstract

The invention relates to a method for synthesizing mesityl oxide and isophorone by an acetone one-step method. The method comprises the following steps: adopting a fixed bed reactor, adopting acetoneas a reaction raw material, filling a magnesium-aluminum composite oxide catalyst prepared by adding silica sol into the reactor, and carrying out condensation reaction on acetone to generate synthesis mesityl oxide and isophorone.

Description

technical field [0001] The invention relates to a method for synthesizing mesityl oxide and isophorone. Background technique [0002] The self-condensation reaction of acetone is a series of reactions, the dimerization product is mainly mesityl oxide, and the trimerization product is mainly isophorone. [0003] Mesityl oxide is an important intermediate in organic synthesis, mainly used in medicines, fine chemicals and pesticides, etc. It can be used as a medium boiling point solvent, nitrocellulose and various resins, especially vinyl resins and spray paints, etc. solvent. [0004] The chemical name of isophorone is 3,5,5-trimethyl-2-cyclohexen-1-one, which is a colorless and low-volatility liquid with a high boiling point, low hygroscopicity, and small evaporation An important ketone solvent with excellent properties of speed and outstanding solvency. At the same time, it is also an important organic chemical raw material. Its derivative isophorone diisocyanate (IPDI) i...

Claims

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Application Information

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IPC IPC(8): B01J21/10B01J37/08B01J37/10C07C45/74C07C49/603C07C49/04
CPCB01J21/10B01J23/002B01J37/082B01J37/10C07C45/74C07C2601/16C07C49/603C07C49/04
Inventor 马夏坪金照生吕建刚周海春孙兰萍金萍刘波黄祖娟赵帅许烽
Owner CHINA PETROLEUM & CHEM CORP
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