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Monolithic titanium oxide-aluminum oxide material and preparation method thereof

A technology of alumina and titanium oxide, which is applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems that the product does not have a three-dimensional macroporous structure, and the environmental pollution of the discharge is serious, so as to eliminate Non-uniform pore size, increased specific surface area, and energy-saving effects

Active Publication Date: 2020-03-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] CN99113284.X has prepared titanium-containing aluminum hydroxide, but because the titanium salt solution contains chloride ions and sulfate radical plasma, which will corrode the equipment, the discharge produced during roasting will pollute the environment seriously, and the resulting product does not have a three-dimensional macroporous structure

Method used

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  • Monolithic titanium oxide-aluminum oxide material and preparation method thereof
  • Monolithic titanium oxide-aluminum oxide material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Preparation of titanium-containing aluminum sol: Boehmite powder, titanium dioxide ultrafine particles (average particle size 10nm) are mixed with distilled water to form a suspension, and hydrochloric acid is added dropwise under continuous stirring conditions to meet the acid / aluminum molar ratio of 0.07 After the dropwise addition, the temperature was raised to 85°C and refluxed for 5 hours to form a stable aluminum sol, and then a paste was formed by rotary evaporation (temperature 40°C, vacuum degree 100Pa).

[0041] (2) Mix water, absolute ethanol, aluminum chloride, polyethylene glycol, paste, and acetamide evenly at room temperature, and then add pyridine. The contents of each component of the mixture are by weight: water 22wt%, Ethanol 20wt%, aluminum chloride 22wt%, polyethylene glycol (viscosity average molecular weight 1 million) 1.0wt%, paste 5wt% (containing 20wt% titanium dioxide), acetamide 2wt%, pyridine 28%. After mixing evenly, cast it into the se...

Embodiment 2

[0044] Step (1) is the same as in Example 1.

[0045] (2) Mix water, absolute ethanol, aluminum chloride, polyethylene glycol, paste, and formamide at room temperature, and then add pyridine. The contents of each component of the mixture are by weight: water 24wt%, Ethanol 20wt%, aluminum chloride 22wt%, polyethylene glycol (viscosity average molecular weight 2 million) 1.0wt%, paste 3wt% (containing 25wt% titanium dioxide), formamide 3wt%, pyridine 27%. After mixing evenly, cast it into a plastic anti-honeycomb mold, continue to age at 70°C for 48 hours after gelation, soak the aged mixture in ethanol for 48 hours after demoulding, after soaking and remove the liquid phase, bake at 60°C Dry until the product no longer loses weight significantly, and then calcined at 650° C. for 6 hours to obtain a cylindrical monolithic titanium oxide-alumina composite oxide material.

[0046] The obtained monolithic alumina material has a total porosity of 74% and a specific surface area of...

Embodiment 3

[0048] Step (1) is the same as in Example 1, except that the particle size of the ultrafine titanium dioxide used is 15 nm.

[0049] (2) Mix water, absolute ethanol, aluminum chloride, polyethylene glycol, paste, N,N-dimethylformamide evenly at room temperature, and then add pyridine. The components of the mixture are by weight, and the content They are: water 22wt%, ethanol 20wt%, aluminum chloride 21wt%, polyethylene glycol (viscosity average molecular weight 2 million) 1.0wt%, paste 8wt% (containing 20wt% titanium dioxide), N, N-two Methylformamide 2wt%, pyridine 26%. After mixing evenly, cast it into a plastic anti-honeycomb mold, continue to age at 70°C for 48 hours after gelation, soak the aged mixture in ethanol for 48 hours after demoulding, after soaking and remove the liquid phase, bake at 60°C Dry until the product no longer loses weight significantly, and then calcined at 700° C. for 6 hours to obtain a cylindrical monolithic titanium oxide-alumina composite oxide...

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Abstract

The invention discloses a monolithic titanium oxide-aluminum oxide material and a preparation method thereof, wherein the monolithic titanium oxide-aluminum oxide material has a honeycomb structure, the distribution number of the honeycomb holes in the cross section is 1-50 / cm<2>, microcosmic macropores are formed in the walls of the honeycomb holes, the diameter of the macropores is 100-1000 nm,and the macropores are evenly distributed and communicated in a three-dimensional mode. The preparation method comprises the following steps: (1) slowly adding a gel solvent into a boehmite powder turbid liquid, and carrying out heating aging to obtain an aluminum sol; and (2) mixing an inorganic aluminum salt, polyethylene glycol, the aluminum sol, titanium alkoxide, an amide group-containing organic compound and a low-carbon alcohol aqueous solution, then adding epoxypropane and / or pyridine, casting the mixture into an anti-honeycomb mold, and molding. According to the method, no organic template is added, the preparation process is environmentally friendly, the process is simple, convenient and easy to implement, and the product has a macroscopic macroporous structure and a microcosmicmacroporous structure, is suitable for serving as a heterogeneous catalytic carrier and is easy for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic materials, and in particular relates to an integral titanium oxide-alumina material and a preparation method thereof. Background technique [0002] Monolithic macroporous oxides are widely used in heterogeneous catalysts, catalyst supports, adsorption and separation materials, chromatographic packing, electrode materials, acoustic resistance and thermal stability due to their large pore structure, high specific surface area and good thermal stability. Resistive materials and other fields. [0003] "Synthesis of Hierarchically Porous Silica and Metal Oxide Beads Using Emulsion-Templated Polymer Scaffolds" (Chemical Material, 2004, 16:4245-4256.) reported that using acrylamide as an organic monomer, N, N-methylenebisacrylamide As a joint agent, Triton X-405 and PVA were used as surfactant and stabilizer respectively, mineral oil was used as dispersed phase, ammonium persulfate and tetramethy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/10C04B35/46C04B35/622B01J21/06
CPCC04B35/10C04B35/46C04B35/622B01J21/063C04B2235/3217C04B2235/3232C04B2235/602C04B2235/606C04B2235/656C04B2235/6567C04B2235/94C04B2235/96
Inventor 杨卫亚凌凤香张会成王少军沈智奇
Owner CHINA PETROLEUM & CHEM CORP
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