Magnetic solid acid catalyst and preparation method and application thereof

A magnetic solid acid and catalyst technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of non-magnetism, easy loss of acidic sites, and small specific surface area of ​​solid acidic substances. High specific saturation magnetization, stable physical and chemical properties, and good magnetic response performance

Active Publication Date: 2009-09-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN1453067A provides a kind of magnetic solid superacid catalyst Zr(SO 4 ) 2 / Fe 3 o 4 and preparation method thereof, the purpose of which is to solve the difficult problem of fine particle catalyst recovery and separation
[0008] In summary, most of the magnetic solid acid catalysts are obtained by coating the solid acidic substance directly on the outside of the magnetic core by the co-precipitation method, and the specific surface area of ​​the solid acidic substance is small, and it is easy to decompose, so the catalytic performance of the prepared catalyst Poor activity, easy to lose acidic sites
In addition, the porosity of the solid acidic substance makes the magnetic core vulnerable to the external environment and is easily transformed into a non-magnetic substance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 0.5mol / L FeCl 2 Solution 240ml with 0.5mol / L FeCl 3 Mix 40ml of the solution, add 0.1mol / L NaOH solution under strong stirring until 103 o 4 .

[0050] the above Fe 3 o 4 Dilute to 10g / L with absolute ethanol, add tetraethoxysilane (0.001mol / gFe 3 o 4 ), to which 18% NH was added under stirring 3 .H 2 O (the molar ratio of ammonia to tetraethoxysilane is 25), stirred for 6 hours, magnetically separated, washed with absolute ethanol, and finally dried at 80° C. for 2 hours to obtain the magnetic powder coated for the first time.

[0051] Dilute the coated magnetic powder for the first time to 20g / L with distilled water, disperse it ultrasonically for 5min, adjust the pH of the suspension to 8~10 with 0.1mol / L NaOH solution, and raise the temperature of the suspension to 80°C, and then add it to At the same time slowly add 0.05mol / L of SiO 2 Solution (sodium silicate modulus is 1, the addition amount is 0.001molSiO 2 / g magnetic powder) and 0.1mol / L HCl solution...

Embodiment 2

[0056] In the process of preparing magnetic alumina, other conditions of Example 1 are kept constant, and the difference is that in the peptization process, magnetic powder, pseudo-boehmite (the mass content of alumina is 75%), H 3 PO 4 The mass ratio of the solution (mass concentration is 5%) mixed by the three is 1:12:100, and the obtained magnetic γ-Al 2 o 3 The weight ratio of each component is Fe 3 o 4 :SiO2 2 :Al 2 o 3 =9:1:90.

[0057] 2.3g NiSO 4 .6H 2 Dissolve O in deionized water to make a solution of 8ml, then impregnate 10g of the above-mentioned 150-250um carrier with the same volume of this impregnating solution, dry at 100°C for 4h, and then roast at 550°C for 6h to obtain a magnetic solid acid catalyst NiSO 4 / γ-Al 2 o 3 . The specific surface area of ​​the product measured by the static low temperature nitrogen adsorption capacity method is 179m 2 / g, the specific saturation magnetization of the product measured by the vibrating sample magnetomet...

Embodiment 3

[0060] In the process of preparing magnetic alumina, keep the other conditions of Example 1 unchanged, the difference is that the second coating of SiO 2 The amount of sodium silicate added in the process is 0.003molSiO 2 / g magnetic powder, and bake the dried product at 550°C for 2 hours to obtain magnetic alumina. The weight ratio of each component of the product obtained is Fe 3 o 4 :SiO2 2 :Al 2 o 3 = 24:6:70.

[0061] 5.9g Zr(SO 4 ) 2 .4H 2 Dissolve O in deionized water to make a solution of 8ml, then impregnate 10g of the above-mentioned 150-250um carrier with the same volume of this impregnation solution, dry at 150°C for 4h, and then roast at 650°C for 6h to obtain a magnetic solid acid catalyst ZrSO 4 / γ-Al 2 o 3 . The specific surface area of ​​the product measured by the static low-temperature nitrogen adsorption capacity method is 152m 2 / g, the specific saturation magnetization of the product measured by the vibrating sample magnetometer is 14.7emu / g...

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Abstract

The invention relates to a magnetic solid acid catalyst which comprises magnetic aluminum oxide and transitional metal loaded on the magnetic aluminum oxide, wherein the weight proportion of the magnetic aluminum oxide and the transitional metal is 1.5-99:1 on the basis of transitional metal sulphate, and the transitional metal is one or more selected from IB, IIB, IVB and VIII groups; the magnetic aluminum oxide comprises Gamma-Al2O3 and magnetic particles embedded in the Gamma-Al2O3, and the weight proportion of the Gamma-Al2O3 and the magnetic particles is 1-9:1; the magnetic particles comprise SiO2 and magnetic kernels embedded in the SiO2, and the weight proportion of the SiO2 and the magnetic kernels is 0.1-1:1; the magnetic kernel is one or more selected from magnetic metals, magnetic alloys and magnetic metal oxides. The magnetic solid acid catalyst has the characteristics of large specific surface area, good magnetic property, stable physicochemical property, and the like, can be applied to processes of fluidized bed and magnetic stabilization bed and is specially suitable for integrating with a magnetic stabilization bed reactor for acid catalyzed reaction in the filed of oil processing.

Description

technical field [0001] The invention relates to a magnetic solid acid catalyst and its preparation method and application. Background technique [0002] Acid-catalyzed reactions are fundamental to petroleum processing and the chemical industry. Most hydrocarbon conversion reactions in petroleum processing are acid-catalyzed reactions, such as cracking, alkylation, superposition, isomerization, and methanol conversion. In the chemical industry, acid-catalyzed reactions are not only used in the synthesis of basic chemicals, but also in the synthesis of specialty chemicals, such as drugs, plastics, pesticides, flavors, and fragrances. [0003] The early acid-catalyzed reactions were mostly homogeneous catalytic reactions based on inorganic acids or salts as catalysts. Inorganic acids or salts have high catalytic activity, but there are many reaction by-products, and it is difficult to separate catalysts from products, making continuous production difficult. In addition, inorg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C10G50/00C07C2/16C07C2/58B01J37/02
Inventor 彭颖宗保宁孟祥堃
Owner CHINA PETROLEUM & CHEM CORP
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