A kind of preparation method of the catalyst that is used for acetone heterogeneous synthesis isophorone

A technology of isophorone and catalyst, applied in the field of catalyst preparation, can solve the problems of complex catalyst preparation process, low selectivity of isophorone, difficult regeneration, etc., achieve high catalytic activity and stability, simple preparation process, The effect of prolonging life

Active Publication Date: 2011-11-30
NINGBO QIANYAN NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, judging from the research results at this stage, the developed catalyst has disadvantages such a...

Method used

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preparation example Construction

[0014] As an example, when the magnesium salt, calcium salt, aluminum salt, and transition metal salt of the present invention are selected as nitrate, and the transition metal is selected as zirconium, the preparation method of the catalyst of the present invention includes the following steps: And zirconium nitrate dissolved in distilled water to prepare a mixed salt solution of 1-2 molar concentration. Under stirring, the alkali solution was added dropwise to the mixed salt solution until the pH value was 7-10. The precipitate is aged at a temperature of 60-100°C for 3-12 hours. After standing and cooling for 1-6 hours, it is filtered, and then the obtained filter cake is washed with deionized water to neutrality. The filter cake is dried in an oven at 80-120° C. for 12 hours, and then calcined at 350-700° C. for 2-7 hours in an air atmosphere to finally obtain a catalyst.

[0015] The mixing ratio of the magnesium nitrate, calcium nitrate, aluminum nitrate and zirconium nit...

Embodiment 1

[0020] 270 grams of magnesium nitrate hexahydrate, 250 grams of calcium nitrate tetrahydrate, 770 grams of aluminum nitrate nonahydrate and 15 grams of zirconium nitrate pentahydrate are dissolved in 2000 ml of deionized water. KOH with a mass concentration of 1% was added dropwise to pH 8.5. Constant temperature aging at 70°C for 8 hours, and standing to cool for 2 hours. Filter and wash the filter cake with deionized water until the filtrate is neutral. It was dried at 80°C for 12 hours, and calcined at 350°C for 7 hours in an air atmosphere to prepare a catalyst.

Embodiment 2

[0022] 270 grams of magnesium nitrate hexahydrate, 200 grams of calcium nitrate tetrahydrate, 500 grams of aluminum nitrate nonahydrate and 30 grams of zirconium nitrate pentahydrate are dissolved in 3000 ml of deionized water. KOH with a mass concentration of 1% was added dropwise to a pH of 7.5. Constant temperature aging at 60°C for 12 hours, and standing and cooling for 1 hour. Filter and wash the filter cake with deionized water until the filtrate is neutral. The catalyst was prepared by drying at 100°C for 12 hours and calcining at 400°C for 5 hours in an air atmosphere.

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Abstract

The invention relates to a method for preparing a catalyst used in synthesizing isophorone through an acetone multiphase method. The method provided by the invention comprises the following steps: weighing and dissolving a certain quantity of magnesium salt, calcium salt, aluminum salt and transition metal salt in distilled water to prepare a mixed salt solution; dropwise adding a precipitator-alkali solution to the mixed salt solution in the stirring course; and aging, filtering, washing, drying and roasting the precipitates to finally obtain the catalyst. Compared with the prior art, the method provided by the invention has the characteristics: (1) the preparation course of the catalyst is simple; (2) the price of the raw materials of the catalyst is low; and (3) the reaction is carriedout under gas phase conditions, and the catalyst is a magnesium-calcium-aluminum composite oxide modified by the transition metal. The catalyst provided by the invention has certain acid strength andalkali strength, thereby enabling the catalyst to have higher catalytic activity and stability. In the reaction for preparing the isophorone through acetone condensation, the conversion rate of acetone is about 34%, the selectivity of the isophorone reaches more than 90%, and the one-way running time is larger than 1000 hours.

Description

Technical field [0001] The invention relates to the field of chemical engineering, and in particular to a method for preparing a catalyst for acetone to synthesize isophorone through a heterogeneous method. Background technique [0002] Isophorone is an important fine chemical raw material with a wide range of uses. It can be used as an advanced solvent or as an organic reaction intermediate. It can dissolve nitrocellulose, acrylic esters, alkyd resins, and polyesters. It can also be used as intermediate raw materials with high polymer materials such as epoxy resin, and produce important products such as alcohol, acid, amine, ester and isocyanate through reaction. [0003] The industrialized process route for the synthesis of isophorone from acetone is mainly acetone condensation. Acetone condensation is the self-condensation of three molecules of acetone into one molecule of isophorone. The current production process is mainly the pressurized liquid phase condensation of acetone...

Claims

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Application Information

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IPC IPC(8): B01J23/02C07C49/603C07C45/74
Inventor 赵坚强张玉善李春伟
Owner NINGBO QIANYAN NEW MATERIAL TECH
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