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Heterogeneous catalyst for preparing isophorone, preparation and applications thereof

A heterogeneous catalyst and isophorone technology, applied in the direction of physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, carbon-based compound preparation, etc., can solve problems such as decline and low conversion rate, Achieve the effects of simple preparation method, high activity and selectivity, and low price

Active Publication Date: 2019-06-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the surface area of ​​the catalyst is too small, acetone cannot fully contact with the catalyst surface, resulting in low conversion rate
On the other hand, if the generated isophorone cannot diffuse from the surface of the catalyst as soon as possible, the isophorone will further undergo aldol condensation with acetone to generate high-boiling point by-products, resulting in a decrease in selectivity

Method used

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  • Heterogeneous catalyst for preparing isophorone, preparation and applications thereof
  • Heterogeneous catalyst for preparing isophorone, preparation and applications thereof
  • Heterogeneous catalyst for preparing isophorone, preparation and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The nitrate is prepared in a mixed salt solution according to the molar ratio Mg:Al:Ce=20:10:0.16. Weigh 25g magnesium nitrate hexahydrate, 18.29g aluminum nitrate nonahydrate, 0.43g cerium ammonium nitrate, and dissolve them in 100ml distilled water , Add 1 gram of hexamethylene tetramine and 1 gram of amantadine as the template agent; at the same time configure lye: add 9.35 grams of NaOH and 6.36 grams of Na 2 CO 3 Dissolve in 50ml of water to obtain a precipitate. At 80°C, drop the precipitant into the mixed salt solution, the pH of the mixed solution is 8-9, continue to stir for 5 hours and then stand for 12 hours. The mixed solution was filtered, washed with water three times, and the filter cake was dried at 120°C for 12 hours and calcined at 550°C for 5 hours. The above catalyst is used in the reaction of acetone condensation to prepare isophorone, a fixed bed reactor is used, and 3 grams of catalyst are loaded. Under normal pressure, pump acetone into the syste...

Embodiment 2

[0040] The nitrate is prepared according to the molar ratio of Mg:Al:Ce:Cu=20:10:0.16:0.1 to prepare a mixed salt solution, weigh 25g magnesium nitrate hexahydrate, 18.29g aluminum nitrate nonahydrate, 0.43g cerium ammonium nitrate, 0.2g nitric acid Copper, dissolve it in 100ml of distilled water, add 1g of stencil agent hexamethylenetetramine and 1g of octadecyltrimethylammonium chloride; at the same time, configure lye: add 9.35g of NaOH and 6.36g of Na 2 CO 3 Dissolve in 50ml of water to obtain a precipitate. At 80°C, drop the precipitant into the mixed salt solution, the pH of the mixed solution is 8-9, continue to stir for 5 hours and then stand for 12 hours. The mixed solution was filtered, washed with water three times, and the filter cake was dried at 120°C for 12 hours and calcined at 600°C for 5 hours. The above catalyst is used in the reaction of acetone condensation to prepare isophorone, a fixed bed reactor is used, and 3 grams of catalyst are loaded. Under normal...

Embodiment 3

[0042] Prepare the mixed salt solution according to the molar ratio of Mg:Al:Ce:Cu=20:10:1:0.1 for nitrate, weigh 25g magnesium nitrate hexahydrate, 18.29g aluminum nitrate nonahydrate, 2.67g cerium ammonium nitrate, 0.2g nitric acid Dissolve copper in 100ml of distilled water, add 1g of stencil agent hexamethylenetetramine and 1g of tetraethylammonium hydroxide; also configure lye: add 8.88g NaOH and 6.04g Na 2 CO 3 Dissolve in 50ml of water to obtain a precipitate. At 80°C, drop the precipitating agent into the mixed salt solution, the pH of the mixed solution is 7-8, continue to stir for 5 hours and then stand for 12 hours. The mixed solution was filtered, washed with water three times, and the filter cake was dried at 120°C for 12 hours and calcined at 650°C for 5 hours. The above catalyst is used in the reaction of acetone condensation to prepare isophorone, a fixed bed reactor is used, and 3 grams of catalyst are loaded. Under normal pressure, pump acetone into the syste...

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Abstract

The present invention provides a method for preparing a heterogeneous catalyst in the presence of a templating agent, wherein the heterogeneous catalyst is used for preparing isophorone through acetone condensation, and is a modified composite oxide (MgO-Al2O3-M<x+>Ox / 2) based on a magnesium aluminum oxide. The preparation method comprises: weighing a certain amount of a mixed salt, dissolving ina certain amount of water, adding a certain amount of a templating agent, adding a certain amount of a precipitating agent to the mixed salt solution in a dropwise manner at a certain temperature, aging, filtering, washing, drying, and calcining to obtain the catalyst. Compared with the catalyst in the prior art, the catalyst of the present invention has advantages of simple preparation method, low price, low bulk density, high activity, high selectivity and good stability. According to the present invention, in the reaction for preparing isophorone through acetone condensation, the reaction temperature is 250-300 DEG C, the mass space velocity of acetone is 1-8 h<-1> under normal pressure, the conversion rate of acetone is up to 45%, the isophorone selectivity is 75%, the mesityl oxide and isophorone selectivity is 90%, and the technology is suitable for the industrial production of isophorone.

Description

Technical field [0001] The invention provides a method for preparing a composite heterogeneous catalyst in the presence of a stencil agent for preparing isophorone by condensation of acetone. The technical field of the invention belongs to the field of catalytic chemistry and fine chemicals. Background technique [0002] Isophorone (IP) is obtained by acetone Aldol condensation and Michael addition cyclization. It is a high-boiling solvent with strong solubility; in addition, because of its conjugated unsaturated ketone structure, it can be further reacted to obtain alcohol , Acids, amines, esters and isocyanates are important organic intermediates in fine chemicals. [0003] The process route for preparing isophorone from acetone via heterogeneous catalysis has the advantages of environmental protection, high conversion rate, and easy amplification. However, the current problems are the same as the liquid phase method, the product is complex, and the selectivity of isophorone is...

Claims

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Application Information

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IPC IPC(8): B01J23/10B01J23/83B01J23/02B01J23/72B01J23/755B01J23/75B01J21/10B01J23/06B01J23/34C07C45/74C07C49/603
Inventor 郑卓孙亮徐雪峰梁鑫淼薛兴亚林小鹏窦荣坦陈苏昌
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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