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SO4<2->/ZrO2-Fe2O3-SiO2 doped mixed-crystal solid acid and preparation method thereof

A technology of zro2-fe2o3-sio2 and solid acid, which is applied in the field of preparation of solid super acid, can solve the problems of limited number of acid centers, failure to reach, low specific surface area of ​​solid acid, etc., to increase the amount of acid centers, easy to share, Good effect with repeated use

Active Publication Date: 2014-06-18
润桐(苏州)技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Solid superacid is a new type of catalyst discovered by humans. Because of its high acidity, it can activate saturated hydrocarbons that are inactive under normal conditions, and can cause various chemical reactions of saturated hydrocarbons. Moreover, because it overcomes the shortcomings of liquid acids, It is easy to separate from the reaction system, does not corrode equipment, is environmentally friendly, and can be reused. It has been paid more and more attention. In recent years, the research and development of solid superacids has become more and more extensive. However, due to the large amount of liquid acid, the acid center It has excellent fluidity, but the acid amount of solid acid is far less than that of liquid acid, mainly because the amount of acid is limited. The reason is that the specific surface area of ​​solid acid is low, which limits the number of acid centers and the combination point of carrier and sulfate Factors such as other factors affect the active acid content of solid acids. Although there are many invention patents that describe the preparation of solid acids in detail, most of them can only be prepared by ammonia hydrolysis combined with physical processing. Although these solid acids have many The strength of strong acid, because the amount of acid is limited, can not completely replace liquid acid and other defects

Method used

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  • SO4&lt;2-&gt;/ZrO2-Fe2O3-SiO2 doped mixed-crystal solid acid and preparation method thereof
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  • SO4&lt;2-&gt;/ZrO2-Fe2O3-SiO2 doped mixed-crystal solid acid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The mass parts of each component are:

[0017]

[0018] (1) ZrOCl 2 , Ammonium hexachloroiridate, cobalt acetate, and ammonium molybdate are dissolved in the non-ionized water, turn on the high-speed disperser at 1000 rpm, the temperature rises to 85 ℃, drop the ammonia into the solution, the dripping is completed in 30 minutes, immediately Add nano-iron trioxide to the mixed solution, add sodium fluorosilicate after an interval of 1 hour, continue to keep the temperature for 4 hours, then stop the high-speed disperser to stir, reduce to room temperature, stand still for 10 hours, filter the precipitate, each time Wash with 50 parts of ion-free water for 3 times to remove the chloride and fluoride ions in the precipitate, and dry it at 100°C until the water is completely evaporated;

[0019] (2) The product of the process (1) is immersed in 1.67% ammonium chloroplatinate solution for 2 hours, then calcined at 500°C for 4 hours, and then the calcined product is immersed in 5%...

Embodiment 2

[0021] The mass parts of each component are:

[0022]

[0023] (1) ZrOCl 2 , Ammonium hexachloroiridate, cobalt acetate, and ammonium molybdate are dissolved in deionized water, turn on the high-speed disperser at 1500 rpm, and the temperature rises to 95°C. Add ammonia droplets to the solution. The dripping is completed within 45 minutes, immediately Add nano-iron trioxide to the mixed solution, add sodium fluorosilicate after an interval of 1 hour, continue to keep the temperature for 3 hours, then stop the high-speed disperser to stir, reduce to room temperature, stand still for 5 hours, filter the precipitate, each time Wash 3 times with 50 parts of ion-free water to remove chloride and fluoride ions in the precipitate, and dry at 120°C until all the water evaporates;

[0024] (2) The product of the process (1) is immersed in a 2% ammonium chloroplatinate solution for 3 hours, then calcined at 650°C for 3 hours, and then the calcined product is immersed in a 10% sulfuric acid s...

Embodiment 3

[0026] The mass parts of each component are:

[0027]

[0028]

[0029] (1) ZrOCl 2 , Ammonium hexachloroiridate, cobalt acetate, and ammonium molybdate are dissolved in deionized water, and the high-speed dispersion is turned on at 1300 rpm, the temperature is increased to 90 ℃, and ammonia is added to the solution. The dripping is completed in 40 minutes. Add nano-iron trioxide to the mixed solution, add sodium fluorosilicate after an interval of 1 hour, continue to keep the temperature for 3.5 hours, then stop the high-speed disperser to stir, reduce to room temperature, stand still for 8 hours, filter the precipitate, use each time Wash with 50 parts of non-ionized water for 3 times to remove chloride and fluoride ions in the sediment, and dry at 110°C until all the water evaporates;

[0030] (C) The product of process (b) was immersed in 1% ammonium chloroplatinate solution for 2.5 hours, and then calcined at 580°C for 3.5 hours, and then the calcined product was immersed in 7...

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Abstract

The invention discloses a SO4<2-> / ZrO2-Fe2O3-SiO2 doped mixed-crystal solid acid and a preparation method thereof. The preparation method comprises the following steps: (1) dropwisely adding ammonia in an aqueous solution of ZrOCl2, ammonium hexachloroiridate, cobaltous acetate and ammonium molybdate, then adding nano ferric oxide, dispersing, after a spacing interval of 1 hour, adding sodium fluosilicate, preserving the heat, standing, filtering, collecting precipitates, washing the precipitates and drying; and (2) dipping the product obtained by the step (1) in an ammonium chloroplatinate solution, then roasting, dipping the roasted article in a sulfuric acid solution, and then roasting again to obtain the SO4<2-> / ZrO2-Fe2O3-SiO2 doped mixed-crystal solid acid. According to the invention, the strength of the acid can be significantly raised, the acid site amount is stabilized and increased, the reuse effect is good, and the solid acid disclosed herein is an ideal acid catalyst for high-molecular polymerization, addition reaction, cracking reaction, esterification reaction, etherification reaction, etc.

Description

Technical field [0001] The invention relates to a preparation method of solid super acid. Background technique [0002] Solid super acid is a new type of catalyst discovered by humans. Because of its high acidity, it can activate saturated hydrocarbons that are inactive under normal conditions, and can cause various chemical reactions of saturated hydrocarbons. It also overcomes the shortcomings of liquid acids. It has the advantages of easy separation from the reaction system, non-corrosive equipment, environmental friendliness, and reusability, etc., and has attracted more and more attention. In recent years, the research and development of solid superacids has become more and more extensive, but due to the large amount of liquid acid, the acid center It has excellent fluidity, and the amount of solid acid is far inferior to that of liquid acid. The main reason is that the amount of acid is limited. The reason is that the specific surface area of ​​solid acid is low, which limi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F290/06C08F4/26C08F4/24
Inventor 施晓旦郭和森
Owner 润桐(苏州)技术服务有限公司
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