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Catalyst used for synthesizing isophorone and preparation method thereof

A technology of isophorone and catalyst, which is applied in the field of catalyst for synthesizing isophorone and its preparation, can solve the problems of unsatisfactory activity and selectivity, unstable catalyst, complex catalyst preparation process, etc., and achieve high activity and selectivity, the preparation method is simple, and the process is green and environmentally friendly

Inactive Publication Date: 2015-12-09
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process of the above-mentioned catalyst is complex, the activity and selectivity are not satisfactory, and the catalyst is unstable and deactivated quickly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] At room temperature, dissolve 1.0 g of polyvinylpyrrolidone K30 in 30 g of absolute ethanol, and add 6.41 g of magnesium nitrate hexahydrate to the solution to prepare solution A after it is completely dissolved. Solution B was prepared by dissolving 30g of zirconium propoxide and 0.5g of acetylacetone in 80g of absolute ethanol. Solution B was added to solution A, stirred at room temperature for 1.5 h, and 1.5 g of deionized water was added dropwise to the mixed solution to obtain a viscous solution. After standing at 40°C for 48h, it turns into a gel. The gel was refluxed in 50 g of 0.2 mol / L ammonia water for 24 h. Filter, dry at 90°C for 10h, and then calcinate at 500°C for 4h to obtain the catalyst. Pack the prepared catalyst in a fixed bed reactor (φ12×600mm), and react at normal pressure, temperature 300°C, acetone mass space velocity 0.5h -1 Carry out under the condition of carrying out, result shows, acetone conversion rate is 52.8%, isophorone selectivity i...

Embodiment 2

[0021] At room temperature, dissolve 1.2g of polyvinylpyrrolidone K30 in 50g of absolute ethanol, and add 12.82g of magnesium nitrate hexahydrate to the solution to prepare solution A after it is completely dissolved. Solution B was prepared by dissolving 32g of zirconium propoxide and 0.8g of acetylacetone in 90g of absolute ethanol. Add solution B to solution A, stir at room temperature for 2 hours, add 2 g of deionized water dropwise to the mixed solution to obtain a viscous solution, which turns into a gel after standing at 60°C for 36 hours. The gel was refluxed in 60 g of 0.2 mol / L ammonia water for 24 h. Filter, dry at 100°C for 6h, and then calcinate at 450°C for 5h to obtain the catalyst. Pack the prepared catalyst in a fixed bed reactor (φ12×600mm), and react at normal pressure, temperature 300°C, acetone mass space velocity 0.5h -1 Carry out under the condition of carrying out, result shows, acetone conversion rate is 54.6%, isophorone selectivity is 86.5%, isopho...

Embodiment 3

[0023] At room temperature, dissolve 1.5g of polyvinylpyrrolidone K30 in 80g of absolute ethanol, and add 20g of magnesium nitrate hexahydrate to the solution to prepare solution A after it is completely dissolved. Solution B was prepared by dissolving 25.6g of zirconium propoxide and 1.0g of acetylacetone in 80g of absolute ethanol. Add solution B to solution A, stir at room temperature for 2 hours, add 1.8 g of deionized water dropwise to the mixed solution to obtain a viscous solution, which turns into a gel after standing at 80°C for 24 hours. The gel was refluxed in 80g0.2mol / L ammonia solution for 24h. Filter, dry at 110°C for 5h, and then calcinate at 600°C for 3.5h to obtain the catalyst. Pack the prepared catalyst in a fixed bed reactor (φ12×600mm), and react at normal pressure, temperature 300°C, acetone mass space velocity 0.5h -1 Carried out under the conditions, the results showed that the conversion rate of acetone was 51.9%, the selectivity of isophorone was 8...

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Abstract

The invention relates to isophorone, in particular to a catalyst used for synthesizing isophorone and a preparation method thereof. The catalyst used for synthesizing isophorone is prepared from components including MgO and ZrO2, wherein the mole ratio of MgO to ZrO2 is (0.1-2):1. The preparation method includes the steps that 1, polyvinylpyrrolidone K30 is dissolved in absolute ethyl alcohol, then magnesium nitrate hexahydrate is added into the solution to prepare a solution A, and zirconium propoxide and acetylacetone are added into absolute ethyl alcohol to prepare a solution B; 2, the solution B is added into the solution A to be stirred, then deionized water is added to obtain a thick solution, and the thick solution stands to be converted into gel; 3, reflux and filtration are performed on the gel in ammonia water, a filter cake is dried and then calcined, and then the catalyst used for synthesizing isophorone is obtained. The catalyst has high activity and selectivity, the conversion rate of acetone can reach 54.6%, and the overall selectivity of isophorone and mesityl oxide can reach 96.8%. The catalyst is easy to prepare and good in stability.

Description

technical field [0001] The invention relates to isophorone, in particular to a catalyst for synthesizing isophorone and a preparation method thereof. Background technique [0002] Isophorone, chemical name 3,5,5-trimethyl-2-cyclohexen-1-one, is a derivative of acetone. Isophorone has become an important ketone solvent because of its outstanding solubility, high boiling point, and low hygroscopicity. It is also an important chemical intermediate, widely used in plastics, coatings, medicine, Industrial fields such as pesticides and spices. [0003] There are two main methods for synthesizing isophorone: mesityl oxide and acetone condensation. Among them, the acetone condensation is suitable for industrialization because the raw materials are cheap and easy to obtain. The acetone condensation method can be divided into two types according to the different contact states: one is the pressurized liquid phase condensation method in alkaline solution, and the other is the gas-sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/10B01J35/10C07C49/603C07C45/74
Inventor 黎四芳卢靖
Owner XIAMEN UNIV
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