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 unreachable, limited number of acid centers, low specific surface area of ​​solid acid, etc., to achieve easy sharing, increase the amount of acid centers, Good effect with repeated use

Active Publication Date: 2013-01-30
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 were dissolved in ion-free water, and the high-speed disperser was turned on at 1000 rpm, the temperature rose to 85°C, and ammonia water was added dropwise to the solution, and the dropwise addition was completed in 30 minutes, and immediately Add nano-ferric oxide into the mixture, add sodium fluorosilicate after an interval of 1 hour, continue to keep warm for 4 hours, then stop stirring the high-speed disperser, drop to normal temperature, and filter the precipitate after standing still for 10 hours. Wash 3 times with 50 parts of deionized water to remove chloride ions and fluoride ions in the precipitate, and dry at 100°C until all the water evaporates;

[0019] (2) Immerse the product of (1) in 1.67% ammonium chloroplatinate solution for 2 hours, then bake it at 500°C for 4 hours, and then put the roasted product in 5% sulfur...

Embodiment 2

[0021] The mass parts of each component are:

[0022]

[0023] (1) ZrOCl 2 , ammonium hexachloroiridate, cobalt acetate, and ammonium molybdate were dissolved in ion-free water, and the high-speed disperser was turned on at 1500 rpm, the temperature rose to 95°C, and ammonia water was added dropwise to the solution, and the dropwise addition was completed in 45 minutes, and immediately Add nano-ferric oxide into the mixture, add sodium fluorosilicate after an interval of 1 hour, continue to keep warm for 3 hours, then stop stirring the high-speed disperser, drop to normal temperature, and filter the precipitate after standing still for 5 hours. Wash 3 times with 50 parts of deionized water to remove chloride ions and fluoride ions in the precipitate, and dry at 120°C until all the water evaporates;

[0024] (2) Immerse the product of (1) in 2% ammonium chloroplatinate solution for 3 hours, then bake it at 650°C for 3 hours, and then put the roasted product in 10% sulfuric ...

Embodiment 3

[0026] The mass parts of each component are:

[0027]

[0028]

[0029] (1) ZrOCl 2 , ammonium hexachloroiridate, cobalt acetate, and ammonium molybdate were dissolved in ion-free water, and the high-speed dispersion was turned on at 1300 rpm. The temperature rose to 90°C, and ammonia water was added dropwise to the solution. After 40 minutes, the dropwise addition was completed, and immediately Add nano-ferric oxide into the mixture, add sodium fluorosilicate after an interval of 1 hour, continue to keep warm for 3.5 hours, then stop stirring the high-speed disperser, drop to normal temperature, and filter the precipitate after standing still for 8 hours. Wash 3 times with 50 parts of deionized water to remove chloride and fluoride ions in the precipitate, and dry at 110°C until all the water evaporates;

[0030] (c) Immerse the product of (b) in 1% ammonium chloroplatinate solution for 2.5 hours, then roast at 580°C for 3.5 hours, then put the roasted product in 7.5% ...

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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 superacid. Background technique [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 t...

Claims

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Application Information

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Patent Type & Authority Applications(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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