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Zirconium dioxide loaded microsphere type silica gel superstrong acid catalyst

A technology of catalysts and small balls, applied in the direction of physical/chemical process catalysts, catalyst activation/preparation, preparation of organic compounds, etc., can solve problems such as the trouble of separating catalysts, and achieve the effects of protecting the environment, increasing the reaction temperature, and increasing the conversion rate

Inactive Publication Date: 2007-05-23
上海中远化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the existing solid superacids are all in powder form, they can only be applied in ebullating bed and tank reactors, and bring troubles in separating catalysts

Method used

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  • Zirconium dioxide loaded microsphere type silica gel superstrong acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Vacuum-dry the macroporous finished silica gel pellets and put them into a buffer solution composed of C.P grade glacial acetic acid, C.P grade ammonium acetate and pure water for hole expansion. The pH value of the buffer solution is equal to 4.9-5.1. The buffer solution and silica gel pellets The volume ratio is 2:1. Under nitrogen bubbling, keep warm at 45°C. After 72 hours, filter out the silica gel pellets and dry them in vacuum. (2) Put the dried silica gel pellets into the zirconium tetrachloride solution. The solution is prepared by mixing C.P grade concentrated hydrochloric acid and C.P grade zirconium tetrachloride, and their weight ratio is 2.0:1. Stand at normal temperature and pressure for 70 hours, stir once an hour, and filter out the pellets. (3) Put the filtered pellets into ammonia water with a concentration of 1.0-2.0% by weight, add ice cream to the ammonia water, and the volume ratio of ammonia water to pellets is 10:1. Then add concentrated ammo...

Embodiment 2

[0034] Except that the volume ratio of buffer solution and silica gel pellets in step (1) is 1.87: 1, the weight ratio of C.P grade concentrated hydrochloric acid to C.P grade zirconium tetrachloride is 1.5: 1 in step (2), and the sulfuric acid in step (4) Except that the solution concentration is 1.5N, all the other reaction steps and reaction conditions are the same as in Example 1. As a result, the small spherical solid superacid catalyst has physical and chemical indicators: the acid strength Hammett function Pka value is -15.05, and the specific surface area is 160--190m 2 / g, the pore volume is 0.546cm 3 / g, the most likely pore diameter D is equal to 112.5 Ȧ, the particle size is 4.5-5.8mm, and the internal pressure strength (average value) is ≥6kg / particle.

Embodiment 3

[0036] Except that the volume ratio of buffer solution and silica gel pellets in step (1) is 1.95: 1, the weight ratio of C.P grade concentrated hydrochloric acid and C.P grade zirconium tetrachloride in step (2) is 1.8: 1, and sulfuric acid in step (4) Except that the solution concentration is 1.5N, all the other reaction steps and reaction conditions are the same as in Example 1. As a result, the small spherical solid superacid catalyst has physical and chemical indicators: the acid strength Hammett function Pka value is -15.05, and the specific surface area is 160--190m 2 / g, the pore volume is 0.560cm 3 / g, the most likely pore diameter D is equal to 118.5 Ȧ, the particle size is 4.5-5.8mm, and the internal pressure strength (average value) ≥ 6kg / particle.

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Abstract

The invention relates to a ball silica gel solid corrosive acid catalyst which loads zirconia used in esterification and dehydration, wherein said silica gel solid corrosive acid has 1000 times protonation ability then dense sulfuric acid. And the ball silica gel solid corrosive acid uses porous ball silica gel as carrier, and absorbs zirconia and sulfuric acid in the inner hole of silica gel, with the properties of powder corrosive acid and the application in solid bed reactor, to process esterification at high pressure and temperature, to improve its transfer rate.

Description

technical field [0001] The invention relates to a superacid catalyst in chemical reactions, in particular to a small spherical silica gel solid superacid catalyst loaded with zirconium dioxide for carboxyl-hydroxyl esterification reaction or hydroxyl dehydration reaction. Background technique [0002] Since M.Hino and K, Arat, J.C successfully synthesized ZrO in 1980 2 and TiO 2 as a carrier, and loaded with H 2 SO 4 After solid superacids, solid superacids have been widely used as new types of acidic catalysts with less pollution and no corrosion. Since the existing solid superacids are all in the form of powder, they can only be applied in ebullating bed and tank reactors, and bring troubles in separating catalysts. Contents of the invention [0003] The purpose of the present invention is to address the deficiencies in the prior art, using macroporous small spherical silica gel as a carrier, and adsorbing zirconium dioxide and sulfuric acid in the inner pores of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/02B01J21/06B01J27/053B01J35/08C07C67/00
Inventor 陈唐
Owner 上海中远化工有限公司
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