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A kind of heterogeneous catalyst for preparing isophorone and its preparation and application

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 the problems of low conversion rate and decline

Active Publication Date: 2021-08-17
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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  • A kind of heterogeneous catalyst for preparing isophorone and its preparation and application
  • A kind of heterogeneous catalyst for preparing isophorone and its preparation and application
  • A kind of heterogeneous catalyst for preparing isophorone and its preparation and application

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Embodiment 1

[0038] The nitrate is configured as a mixed salt solution according to the molar ratio Mg:Al:Ce=20:10:0.16, weigh 25g of magnesium nitrate hexahydrate, 18.29g of aluminum nitrate nonahydrate, and 0.43g of ammonium cerium nitrate, and dissolve them in 100ml of distilled water , add 1 gram of template agent hexamethylenetetramine, 1 gram of amantadine; prepare lye at the same time: mix 9.35 grams of NaOH and 6.36 grams of NaOH2 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 8-9, continue stirring for 5 hours and then let stand for 12 hours. The mixed solution was filtered, washed three times with water, the filter cake was dried at 120°C for 12h, and baked at 550°C for 5h. The above catalyst was used for the reaction of acetone condensation to prepare isophorone, using a fixed-bed reactor filled with 3 grams of catalyst. Under normal pressure, pump acetone into the syst...

Embodiment 2

[0040] Nitrate is configured mixed salt solution according to molar ratio Mg:Al:Ce:Cu=20:10:0.16:0.1, weighs 25g magnesium nitrate hexahydrate, 18.29g aluminum nitrate nonahydrate, 0.43g ammonium cerium nitrate, 0.2 gram nitric acid Copper, dissolve it in 100ml distilled water, add 1 gram of template agent hexamethylenetetramine, 1 gram of octadecyltrimethylammonium chloride; prepare lye at the same time: mix 9.35 grams of NaOH and 6.36 grams of NaOH 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 8-9, continue stirring for 5 hours and then let stand for 12 hours. The mixed solution was filtered, washed three times with water, the filter cake was dried at 120°C for 12h, and calcined at 600°C for 5h. The above catalyst was used for the reaction of acetone condensation to prepare isophorone, using a fixed-bed reactor filled with 3 grams of catalyst. Under normal press...

Embodiment 3

[0042] Nitrate is configured mixed salt solution according to molar ratio Mg:Al:Ce:Cu=20:10:1:0.1, weighs 25g magnesium nitrate hexahydrate, 18.29g aluminum nitrate nonahydrate, 2.67g ammonium cerium nitrate, 0.2 gram nitric acid Dissolve copper in 100ml of distilled water, add 1 gram of template agent hexamethylenetetramine, 1 gram of tetraethylammonium hydroxide; prepare lye at the same time: mix 8.88 grams of NaOH and 6.04 grams of NaOH 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 stirring for 5 hours and then let it stand for 12 hours. The mixed solution was filtered, washed three times with water, the filter cake was dried at 120°C for 12h, and then calcined at 650°C for 5h. The above catalyst was used for the reaction of acetone condensation to prepare isophorone, using a fixed-bed reactor filled with 3 grams of catalyst. Under normal pressure...

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Abstract

The invention provides a method for preparing a heterogeneous catalyst in the presence of a template agent for preparing isophorone through condensation of acetone. The catalyst is a modified composite oxide based on magnesium aluminum oxide: MgO‑Al 2 o 3 -M x+ o x / 2 . The preparation method comprises the following steps: weighing a certain amount of mixed salt and dissolving it in a certain amount of water, adding a certain amount of template agent, and dropping a certain amount of precipitating agent into the mixed salt solution at a certain temperature. The catalyst is obtained after aging, filtering, washing, drying and roasting. Compared with the prior art, the preparation method of the catalyst is simple and convenient, the price is low, the bulk density is small, the activity and selectivity are high, and the stability is good. In the reaction of acetone condensation to prepare isophorone, the reaction temperature is 250℃~300℃, under normal pressure, the mass space velocity of acetone is 1~8h ‑1 , the highest conversion rate of acetone is 45%, the selectivity of isophorone is 75%, and the selectivity of mesityl oxide and isophorone is 90%. This technology is suitable for industrial production of isophorone.

Description

technical field [0001] The invention provides a composite heterogeneous catalyst and method for preparing isophorone by condensation of acetone in the presence of a template agent. The technical field of the invention belongs to the field of catalytic chemistry and fine chemical industry. 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 alcohols. , acids, amines, esters and isocyanates, etc., are important organic intermediates in fine chemicals. [0003] The process route of preparing isophorone from acetone via heterogeneous catalysis has the advantages of environmental protection, high conversion rate and easy scale-up. However, the current problems are the same as the liquid phase method, the product is complex, and the selectivity of isophor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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