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Process for preparing mesoporous Si-Al catalysis material

A silicon-alumina material and technology for the preparation process, which are applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complex preparation process, difficult control, expensive raw materials, etc., and achieve simple operation, Easy-to-control effects

Inactive Publication Date: 2002-06-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these preparation methods with alkoxide as raw material exist bigger shortcoming, mainly contain following two points: (1) raw material is expensive, and the metal alkoxide as raw material is flammable, poisonous, difficult for preservation
(2) Different types of alkoxides have different hydrolysis rates, so the preparation process of the material is complicated and difficult to control

Method used

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  • Process for preparing mesoporous Si-Al catalysis material
  • Process for preparing mesoporous Si-Al catalysis material
  • Process for preparing mesoporous Si-Al catalysis material

Examples

Experimental program
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Embodiment 1

[0011] The specific embodiment embodiment 1 preparation of silicon-alumina catalytic material

[0012] A certain amount of water glass (SiO 2 0.39mol / L, Na 2 O0.125mol / L) solution and 0.96M Al(NO 3 ) 3 The solutions were mixed, ammonia water was added dropwise until the pH of the system was 8, stirred for one hour, filtered, and washed with water and ammonium nitrate solution for 7 times respectively. After filtering, add 200ml water and a certain amount of 0.94M HNO 3 The solution made the pH of the system = 4, and after stirring for 12 hours, a clear silica-alumina sol was obtained. Dry under vacuum conditions (vacuum degree 60 mmHg), and then bake at 550° C. for 8 hours to obtain a silicon-aluminum material.

Embodiment 2

[0014] First, use nitric acid (0.94M) to dissolve 50ml of water glass solution (SiO 2 0.78mol / L, Na 2 (00.25mol / L) pH value is adjusted to about 10, then according to the silicon-aluminum ratio of required preparation material, the aluminum sol freshly prepared is added in the water glass solution after the acidification under the condition of vigorous stirring. After adding a certain amount of nitric acid (0.94M) to dissolve the gel, a light blue silica-alumina mixed sol was prepared. When the sol automatically gels at room temperature, immediately add 70ml NH 4 NO 3 The solution (1.2M) was added to the gel for ion exchange to remove sodium ions from the gel. This process is generally repeated three times. Finally, the obtained gel sample was directly put into a muffle furnace and fired at 550°C for 10 hours to obtain the desired material. The texture data of the synthesized materials are shown in Table 1 below.

[0015] Table 1 Sample Si / Al BE...

Embodiment 4

[0016] Coulter N 4 The particle size distribution of the silica-alumina sol prepared in Example 1 was measured by a plus laser particle size analyzer. Figures A, B, C, and D in Figure (1) represent the particle size distribution diagrams of silica-alumina sol samples with different molar ratios of silicon to aluminum (the molar ratios of silicon to aluminum are 1, 4, 7, and 10, respectively). It can be seen from the figure that the particle size of the sol particles in these sol samples is generally larger. And with the increase of the molar ratio of silicon to aluminum, the particles of the sol system gradually increase, and the particle size distribution gradually widens. The above particle size distribution characterization results show that a relatively stable silica-alumina sol can be prepared by this method. Embodiment 4 TEM analysis result

[0017] figure 2 It is the TEM photo of the sol with a silicon-aluminum molar ratio of 1 and the particle size distribution o...

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Abstract

A mesoporous Si-Al catalyst is prepared from inorganic aluminium salt and water glass through adding ammonia water for deposition, washing deposit by water and ammonium nitrate solution, adding diluted nitric acid as dispergating catalyst to obtain stable and clear Si-Al sol, vacuum drying to obtain gel, and calcining at 350-650 deg.C for 1-20 hr. Its advantages include low cost, simple preparing process, high specific surface area and narrow range of mesoporous diameters.

Description

technical field [0001] The invention relates to a method for a silicon-aluminum catalytic material with concentrated mesopore distribution. In particular, it is a method for preparing mesoporous silica-alumina catalyst material without using a template. Background technique [0002] Microporous zeolite catalytic materials are widely used in petroleum processing industry due to their shape-selective catalytic performance and high reactivity. However, with the increasing depletion of petroleum resources and considering the requirements of environmental protection and other aspects, more and more attention has been paid to "eat up and squeeze out" and the deep processing of heavy oil and residual oil in petroleum processing. The existing microporous catalytic materials cannot be used for the catalytic reaction of macromolecules due to the limitation of the pores, so the synthesis of mesoporous catalytic materials has attracted more and more attention (Kresge C T, Leonowicz M E...

Claims

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Application Information

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IPC IPC(8): B01J21/00B01J21/12B01J35/10B01J37/00
Inventor 熊国兴姚楠盛世善
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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