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Mesoporous composite oxide type solid super acidic catalyst and preparation method thereof

A composite oxide, solid superacid technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve superacid deactivation, service life and repetition Problems such as poor usability, production and application, to achieve the effects of uniform grain size, excellent catalytic activity, excellent catalytic activity and reusability

Inactive Publication Date: 2011-02-23
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above related or similar background technologies use different processes to prepare a class of oxide solid superacids that also contain sulfate or sulfate. This type of sulfuric acid-promoted superacid is easy to lose sulfate as the catalytic reaction proceeds. Carbon deposits lead to rapid deactivation, so there are generally problems such as poor service life and reusability that affect and restrict actual production and application

Method used

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  • Mesoporous composite oxide type solid super acidic catalyst and preparation method thereof
  • Mesoporous composite oxide type solid super acidic catalyst and preparation method thereof
  • Mesoporous composite oxide type solid super acidic catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Weigh 3.7g and 4.5g of the two template agents P123 and Brij35, respectively, and dissolve them in 100ml of aqueous solution. When stirring until the solution is clear, first add 0.7g of phosphotungstic acid to dissolve, so that the phosphotungstic acid is completely dissolved in the above solution, then add 10ml of zirconium propoxide (70%wt) drop by drop, and stir for 12h. The samples were placed in an oven at 100°C for 24 hours. After the hydrothermal treatment, the sample was taken out, extracted with ethanol solution to remove the surfactant, and then placed in an oven at 100°C to dry the sample for 24 hours. After the sample was dried, it was placed in a muffle furnace and calcined at a high temperature of 550° C. for 5 hours to obtain a composite oxide solid acid catalyst. The mass ratio of each component in the composite oxide solid acid catalyst of this embodiment is: tungsten oxide 20%wt, zirconium oxide 80%wt. Its typical XRD diffraction pattern is as fig...

Embodiment 2

[0044] According to the preparation process of Example 1, the sample was dried and put into a muffle furnace for calcination at a high temperature of 700° C. for 3 hours. The results of the N2-adsorption-desorption analysis are shown in Table 1, and the results of the probe reaction experiment in the esterification process are shown in Table 2. It can be seen that the composite catalytic powder material is still a stable tetragonal phase nanocrystal after being calcined at 700 °C; it has a high specific surface area, and the specific surface area is greater than 90m 2 / g. The catalytic activity of the material is lower than that of the sample calcined at 550°C, and the esterification reaction effect is also relatively low. After 6 hours of reaction, the esterification conversion rate reaches 100%.

Embodiment 3

[0046] According to the preparation process of Example 1, the amount of phosphotungstic acid was changed to 0.52g, and the rest of the process flow remained unchanged. The mass ratio of each component in the composite oxide solid acid catalyst of this embodiment is: tungsten oxide 15%wt, zirconium oxide 85%wt. Its typical XRD pattern is as figure 2 As shown in 15wz-550, the results of N2-adsorption and desorption are shown in Table 2, and the results of the probe reaction experiment in the esterification process are shown in Table 3. It can be seen that the composite catalytic material sample of the present embodiment has a high specific surface area, reaching 169m 2 / g, has good catalytic activity, after 1 hour of esterification reaction, the esterification conversion rate is 69%, and after 6 hours of reaction, the esterification conversion rate reaches 100%.

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Abstract

The invention belongs to the field of catalysis of inorganic chemistry and chemical industry, and relates to a mesoporous composite oxide type solid super acidic catalyst and a preparation method thereof. The mesoporous composite oxide type solid super acidic catalyst of the invention comprises a component A and a component B, wherein the catalyst comprises 40 to 200 mass parts of component A and 5 to 80 mass parts of component B; the component A is one or two of zirconium oxide and titanium oxide; the component B is one or two of tungsten oxide, molybdenum oxide and cobalt oxide; the mesoporous composite oxide type solid super acidic catalyst has a worm-shaped mesoporous structure which consists of nanocrystallines uniformly compounded by the components; and the most probable aperture is 1 to 10nm. The catalyst prepared by the preparation method of the invention has superior catalytic activity and reusability, can be independently used as the catalyst or coated on the surface of cellular ceramic or metal carrier to serve as an integrated solid acidic catalytic material, and is a non-sulfuric acid promotion type solid super acidic catalyst.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry and chemical catalysis, and relates to a non-sulfuric acid-promoted solid superacid catalyst and a preparation method thereof, in particular to a composite oxide type high specific surface area solid superacid with excellent reusability and mesoporous structure Catalyst and method for its preparation. Background technique [0002] Superacid catalysts generally come in two forms, liquid and solid, which are called liquid superacids and solid superacids, respectively. As a catalyst for organic reactions, liquid superacids have the same drawbacks as the catalytic process of existing industrial liquid acids (such as sulfuric acid), such as severe equipment corrosion, difficulty in catalyst recovery, and easy pollution of the environment. In recent years, due to the advocacy of green chemistry , the concept of green catalysis came into being. The solid superacid has the characteristics of high activ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/30B01J23/888
Inventor 陈航榕陈崇城施剑林俞建长
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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