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ZrO2-SiO2 compound oxides, its preparation method and application

A technology of composite oxides and oxides, applied in chemical instruments and methods, catalyst activation/preparation, hydrocarbons, etc., can solve problems such as poor hydrothermal stability, achieve concentrated pore size distribution, good structural thermal stability, and specific The effect of large surface area

Active Publication Date: 2007-08-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, whether it is a natural zeolite molecular sieve or a synthetic zeolite molecular sieve, its pore diameter is less than 1.5 nm, and its hydrothermal stability is relatively poor.
This limits the use of zeolite molecular sieves to catalytic reactions involving small molecules and relatively mild hydrothermal conditions, but not suitable for catalytic reactions involving organic macromolecules or harsh hydrothermal conditions.

Method used

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  • ZrO2-SiO2 compound oxides, its preparation method and application
  • ZrO2-SiO2 compound oxides, its preparation method and application
  • ZrO2-SiO2 compound oxides, its preparation method and application

Examples

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preparation example Construction

[0019] The preparation method of the composite oxide provided by the present invention comprises adding the silicon-containing compound and the surfactant into the zirconium-containing compound solution under stirring to form a mixture, adding the basic compound solution, and adjusting the pH value of the system from 10 to 12 to Form a sol, age the sol under stirring and standing respectively, obtain a hydrogel after washing and filtering, then dry and roast, and the surfactant has the general formula R(CH 3 ) 3 The quaternary ammonium salt of NX, R is an alkyl group containing 12-22 carbons, X is a halogen, preferably chlorine or bromine, and the ratio of surfactant to Zr in the zirconium compound is 2-8% by mass.

[0020] The zirconium-containing compound described in the above preparation method is preferably ZrOCl 2 , ZrCl 4 , Zr(NO 3 ) 2 or Zr(NO 3 ) 4 , the silicon-containing compound is preferably sodium silicate, silicon dioxide or ethyl orthosilicate, and the su...

example 1

[0030] Prepare ZrO of the present invention 2 -SiO 2 composite oxides.

[0031] (1) 1.74 grams of ethyl orthosilicate (produced by Shanghai Pharmaceutical Co., Ltd., analytically pure) and 0.28 grams of cetyltrimethylammonium bromide C 16 h 33 (CH 3 ) 3 NBr (produced by Tianjin Chemical Reagent Factory, analytically pure) was dripped into 22.09 grams of ZrOCl respectively under the condition of continuous stirring 2 ·6H 2 O (produced by Shanghai Pharmaceutical Co., Ltd., analytically pure) and 300 milliliters of deionized water were prepared, and the stirring was continued until a transparent mixed liquid was formed.

[0032] (2) Aqueous ammonia solution with a concentration of 2% by mass is added dropwise at a rate of 10 to 15 ml / min to the liquid mixture prepared in step (1) under continuous stirring until finally milky white hydrosol is formed, and the mixture system is controlled The pH value is 11.

[0033] (3) Continue to stir and age the hydrosol at 25°C for 4 h...

example 2～6

[0040] Example 2~6 adopts different zirconium compounds, prepares ZrO according to the method for example 1 2 -SiO 2 . The zirconium compound used in each example and the addition of each raw material and the ZrO produced 2 -SiO 2 The physical and chemical properties of the composite oxides are listed in Table 1.

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Abstract

A ZrO2 - SiO2 composite oxides includes 85~98 wt% ZrO2 and 2-15wt% SiO2, the most probable aperture is 3-8nm and at least diameter of 90% hole is 3~8 nm, hole structure is the cylinder-shaped hollow structure; and the specific surface area of BET is 120 to 150 m 2 / g, the index H0 of acid strength Hammet is -8.4--5.6. Said preparation method of ZrO2 - SiO2 includes: adding silicon-containing compound and surface activator into zirconium-containing compound solution under the condition of continuous stirring to form mixture, then adding alkaline solution into said mixture under the condition of continuous stirring to form sol, after ageing, washing and filtering the sol and preparing gel, then producing the ZrO2 - SiO2 solid after drying and roasting gel. The activator using the composite oxide as carrier is used for transfer reaction of pseudocumene and toluene alkyl group and has higher pseudocumene conversion rate and better dimethylbenzene selective.

Description

technical field [0001] The invention relates to a composite oxide and its preparation method and application. Specifically, a ZrO 2 -SiO 2 Composite oxide, its preparation method and its application in aromatic hydrocarbon transalkylation reaction. Background technique [0002] In the field of catalysis, how to prepare high-activity, high-selectivity, and long-life high-efficiency catalysts has always been a topic of concern. The development of new catalytic materials is the key to solve this problem. The preparation of catalysts by using catalytic materials with large specific surface area, certain acid-alkaline or / and certain oxidation-reduction properties, stable and special pore structure, and specific pore size can improve the reactivity and selectivity of the catalyst and improve the use of the catalyst life, which is conducive to the regeneration of the catalyst. [0003] Zeolite molecular sieves are an important class of catalytic materials. They have the charac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J35/02B01J37/00C07C6/00
Inventor 张昕王建伟钟进姚志龙刘爱松高俊魁
Owner CHINA PETROLEUM & CHEM CORP
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