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Solid strong acid catalyst and its preparing method

A solid strong acid and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of low isomerization selectivity and many cracking products

Inactive Publication Date: 2004-09-01
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] CN1229368A discloses a preparation method of a solid acid catalyst, which is to mix and knead the hydroxide or oxide of zirconium with the hydroxide or oxide of aluminum and a sulfur compound, and load a kind of 8, 9, 10 after roasting Group metals, finally calcined at 300-700°C, but the catalyst zirconia has only tetragonal phase and no monoclinic phase. Since the activity of the tetragonal phase is higher than that of the monoclinic phase, the catalyst is cracked when it is used in the isomerization reaction of alkanes More products, resulting in low isomerization selectivity

Method used

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  • Solid strong acid catalyst and its preparing method

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preparation example Construction

[0016] The preparation method of the catalyst provided by the invention comprises mixing the hydrated zirconia with monoclinic and tetragonal mixed crystal phases, the mixture of silicon oxide and aluminum oxide, and using sulfuric acid, ammonium sulfate or hydrogen sulfate with a concentration of 0.1-4.0 mol / liter The ammonium aqueous solution is impregnated, the solid is dried and shaped, and then roasted at 400-800°C.

[0017] The above shaped and calcined solids are further impregnated with a solution containing Group VIII metals, dried and calcined at 400-700° C. to obtain a catalyst supporting Group VIII metals.

[0018] The method of introducing Group VIII metal can be carried out by conventional impregnation method, that is, the soluble Group VIII metal compound is formulated into an impregnation liquid to impregnate solid substances. The liquid / solid ratio is 0.8-1.2 during impregnation, the temperature is room temperature, and the time is 2-6 hours. . The soluble Gr...

example 1

[0031] Preparation of hydrated zirconia in mixed crystal phases.

[0032] Zirconium oxychloride (ZrOCl 2 ·8H 2 (0) be made into 5 mass % aqueous solution, while stirring, slowly add the ammoniacal liquor that concentration is 25 mass %, adjust pH value to certain value, move gained zirconium hydroxide precipitation to autoclave sealing together with solution, at set temperature Water heat treatment for a period of time. The solid was washed with deionized water and filtered until the filtrate was free of Cl - . Dry at 110°C for 24 hours to obtain hydrated zirconia powder. The crystal phase composition of hydrated zirconia prepared under different hydrothermal treatment conditions is shown in Table 1. Among them, the X-diffraction spectrum of hydrated zirconia b is shown in figure 1 , figure 1 T represents the diffraction peak of tetragonal zirconia, and M represents the diffraction peak of monoclinic zirconia.

example 2

[0034] A mixture of silica and alumina is prepared.

[0035] Take a certain amount of silica sol (SiO 2 content is 41% by mass) was added to the solid powder of a certain amount of aluminum hydroxide (Germany, Condea company, brand SB), ground uniformly, dried at 110 ° C for 24 hours, and added 10% NH 4 200 ml of Cl solution was refluxed under stirring at 80°C for 3 hours, washed with deionized water, filtered, repeated three times, and dried at 110°C for 24 hours to prepare a mixture of silicon oxide and aluminum oxide. See Table 2 for the amount of raw materials added and the composition of the mixture during preparation.

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Abstract

The invention is a solid strong-acid catalyst, containing a mixed oxide sulfated by sulfocompound, its sulfur content 1.0-2.5 m%, where the mixed oxide is composed of zirconia, silicon oxide and alumina in the dry-based mass ratio of 30-90 to 1-30 to 9-40, and the monoclinic crystal phase proportion of zirconia is 10-70 m% and the rest square crystal phases. It is applied to isomerization reaciton of C4-C7 alkanes and has higher isomerization activity and selectivity.

Description

technical field [0001] The invention relates to a solid superacid catalyst and a preparation method thereof, in particular to a solid strong acid catalyst containing zirconia and sulfate radicals and a preparation method thereof. Background technique [0002] Acid catalysts play an important role in the petrochemical industry. Commonly used acid catalysts include liquid acid catalysts, such as H 2 SO 4 , HF and halogen-containing solid acid catalysts. These two types of catalysts have problems such as polluting the environment and corroding equipment. Halogen-containing solid acid catalysts have strict requirements on the water in the raw material because the halogens are easily lost, and the halogens need to be replenished frequently to maintain the activity of the catalyst. The solid strong acid catalyst disclosed in Japanese Laid-Open Patent Publication No. 59-6181 is prepared by treating the oxide or hydroxide of Group IV metal with a sulfur-containing compound and ca...

Claims

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Application Information

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IPC IPC(8): B01J27/053
Inventor 于中伟潘晖华濮仲英
Owner CHINA PETROLEUM & CHEM CORP
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