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Method for preparing magnetic SO42-/ZrO2/Fe3O4/attapulgite solid acid catalyst

A solid acid catalyst, attapulgite technology, applied in the preparation of organic compounds, physical/chemical process catalysts, preparation of carboxylic acid esters, etc., to achieve the effects of low production cost, easy availability of raw materials, and high catalytic activity

Inactive Publication Date: 2010-12-01
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Magnetic materials can also be loaded on attapulgite crystals by chemical precipitation or impregnation, calcination, and reduction methods to prepare magnetic attapulgite composite materials (Applied Surface Science, 2008, 255(5), 2020-2025), CN101537356 , CN101618349), there is no report on preparing magnetic composite solid acid catalyst on attapulgite with magnetic materials and solid acid active components loaded

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1g attapulgite, 0.66g zirconium oxychloride, 1.17g FeCl 3 , 5.78gFeSO 4 ·8H 2 O was added to 40mlH 2 In O, stir mechanically for 30min to form a mixed slurry, in which Fe 2+ , Fe 3+ The molar concentrations of zirconium oxychloride and zirconium oxychloride are 0.52, 0.18, and 0.05 mol / L respectively; then the mixed slurry is heated to 40°C, and 0.1 mol / L NaOH solution is slowly added dropwise to make the pH to 10, and the stirring is continued for 3 hours at a constant temperature. Then filter with suction, wash with water until neutral, dry at 110°C for 12 hours, and grind to a size below 200 mesh to obtain a mixed powder; use 0.5mol / LH for the mixed powder 2 SO 4 The solution was soaked for 24 hours, then suction filtered, dried at 110°C for 12 hours, ground to below 200 mesh, and then calcined at 400°C for 3 hours to obtain magnetic SO 4 2- / ZrO 2 / Fe 3 o 4 / Attapulgite solid acid catalyst.

[0015] Add glacial acetic acid (0.5mol), n-butanol (0.55mol) a...

Embodiment 2

[0017] 1g attapulgite, 1.31g zirconium oxychloride, 1.85gFe 2 (SO 4 ) 3 9H 2 O, 3.82gFeCl 2 4H 2 O was added to 40mlH 2 In O, stir mechanically for 30min to form a mixed slurry, in which Fe 2+ , Fe 3+ The molar concentrations of zirconium oxychloride and zirconium oxychloride are 0.48, 0.165, and 0.1mol / L respectively; then the mixed slurry is heated to 50°C, and 0.5mol / L NaOH solution is slowly added dropwise to make the pH to 11, and the stirring is continued for 2.5h at constant temperature , followed by suction filtration, washed with water until neutral, dried at 110°C for 12 hours, and ground to below 200 mesh to obtain a mixed powder; the mixed powder was mixed with 0.6mol / LH 2 SO 4 The solution was soaked for 20 hours, then suction filtered, dried at 110°C for 12 hours, ground to below 200 mesh, and then calcined at 450°C for 2.5 hours to obtain magnetic SO 4 2- / ZrO 2 / Fe 3 o 4 / Attapulgite solid acid catalyst.

[0018] The above catalyst was applied to...

Embodiment 3

[0020] 1g attapulgite, 2.56g zirconium oxychloride, 0.87g FeCl 3 , 4.34gFeSO 4 ·8H 2 O was added to 40mlH 2 In O, stir mechanically for 30min to form a mixed slurry, in which Fe 2+ , Fe 3+ The molar concentrations of zirconium oxychloride and zirconium oxychloride are 0.39, 0.134, and 0.2mol / L respectively; then the mixed slurry is heated to 55°C, and 1mol / L NaOH solution is slowly added dropwise to make the pH 12, and the stirring is continued for 2 hours at a constant temperature, and then Suction filter, wash with water until neutral, dry at 110°C for 12 hours, and grind to below 200 mesh to obtain mixed powder; use 0.7mol / LH for mixed powder 2 SO 4 The solution was soaked for 16 hours, then suction filtered, dried at 110°C for 18 hours, ground to below 200 mesh, and then calcined at 500°C for 2 hours to obtain magnetic SO 4 2- / ZrO 2 / Fe 3 o 4 / Attapulgite solid acid catalyst.

[0021] The above catalyst was applied to the reaction system of Example 1. Under th...

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PUM

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Abstract

The invention discloses a method for preparing a magnetic SO42- / ZrO2 / Fe3O4 / attapulgite solid acid catalyst, which comprises the steps of: firstly, dissolving attapulgite clay, zirconium oxychloride, ferric salt and ferrous salt in water to form mixed size; then slowly dripping alkali liquor into the mixed size under mechanical stirring to form black precipitates; aging, filtering, washing, drying and grinding the black precipitates to obtain mixed powder; and finally, acidifying the mixed powder with sulfuric acid, leaching, drying, pulverizing and calcining to prepare the magnetic SO42- / ZrO2 / Fe3O4 / attapulgite solid acid catalyst. By taking low-cost attapulgite clay as raw materials and loading magnetic materials and solid acid, the method is simple and has available raw materials and low production cost, and the prepared catalyst has high catalytic activity and magnetism and is easy to separate from products.

Description

technical field [0001] The present invention relates to a kind of preparation method of magnetic attapulgite solid acid catalyst, specifically a kind of attapulgite clay is used as carrier, loads Fe 3 o 4 and ZrO 2 , A method for preparing a magnetic solid acid catalyst through acidification and calcination. Background technique [0002] Traditional inorganic acids are cheap and have high catalytic activity, and are widely used in acid-catalyzed reactions such as esterification, alkylation, and isomerization. However, it is difficult to separate the inorganic acid catalyst from the product, and it is highly corrosive to equipment. It is difficult to recycle, and it also has great pollution to the environment. Compared with inorganic acids, solid acid catalysts have the advantages of high catalytic activity, non-corrosiveness, continuous production, and easy separation of products and catalysts. They have attracted widespread attention and have gradually replaced inorganic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C69/14C07C67/08
Inventor 蒋金龙固旭冯良东程晓春谷亚昕
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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