Preparation method of non-binder titaniferous mercerizing molecular sieve catalyst

A technology without binder and catalyst, applied in the field of chemical catalytic materials and chemical applications, can solve the problems of easy blockage of molecular sieve channels, difficult separation, shortening, etc., and achieves the effects of obvious industrialization promotion and application prospects, solving separation difficulties, and convenient preparation.

Active Publication Date: 2013-08-21
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to provide a method for preparing a binder-free titanium-containing mercerized molecular sieve catalyst for the deficiencies of the prior art. The silica-alumina mordenite prepared by the dry glue method is exchanged with ammonium, and then the titanium is replaced by gas phase replacement. A binder-free titanium-containing mercerized molecular sieve catalyst is obtained, which effectively solves the separation difficulties in the ammoximation process of ketones, and the problems caused by the use of nano-scale titanium-silicon molecular sieve powder or micron-scale spray-formed titanium-silicon molecular sieve due to the presence of binders Effective utilization and reduced activity, easy blockage of molecular sieve channels, severe carbon deposition and shortened service life have certain prospects for industrialization and application and significant economic value.

Method used

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  • Preparation method of non-binder titaniferous mercerizing molecular sieve catalyst
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  • Preparation method of non-binder titaniferous mercerizing molecular sieve catalyst

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Embodiment 1

[0038] a. Preparation of catalyst precursor particles

[0039]Mix 100g of fumed silica gel and 120g of sodium mordenite raw powder evenly, then dissolve 20g of sodium metaaluminate and 2g of sodium hydroxide in an appropriate amount of water and add to the above materials, mix and stir, extrude and shape into a clover-shaped catalyst Precursor, the shaped catalyst precursor is dried at 80°C for 10 hours to obtain catalyst precursor particles with a particle size of 0.1mm~1cm.

[0040] b, the preparation of mordenite

[0041] The catalyst precursor particles prepared by the above dry glue method were statically crystallized under water vapor at 170°C for 72 hours, and binder-free mordenite was synthesized in situ by an amine-free method.

[0042] c. Ammonium exchange of mordenite

[0043] The mordenite prepared above without binder was washed twice with water and mixed with NH at a concentration of 1mol / L 4 The Cl aqueous solution is mixed at a weight ratio of 1:30, heated i...

Embodiment 2

[0053] a. Preparation of catalyst precursor particles

[0054] Mix 160g of alkaline silica sol and 120g of sodium mordenite raw powder evenly, then dissolve 18g of aluminum chloride and 9g of potassium hydroxide in an appropriate amount of water and add to the above materials, mix and stir, extrude and shape into a clover-shaped catalyst Precursor, the shaped catalyst precursor is dried at 80°C for 10 hours to obtain catalyst precursor particles with a particle size of 0.1mm~1cm.

[0055] b, the preparation of mordenite

[0056] The catalyst precursor particles prepared by the dry glue method were statically crystallized under water vapor at 140° C. for 120 hours, and binder-free mordenite was synthesized in situ by an amine-free method.

[0057] c. Ammonium exchange of mordenite

[0058] The mordenite prepared above without binder was washed twice with water and mixed with NH at a concentration of 1mol / L 4 The Cl aqueous solution is mixed at a weight ratio of 1:30, heated ...

Embodiment 3

[0068] a. Preparation of catalyst precursor particles

[0069] Mix 70g of water glass and 120g of sodium-type mordenite raw powder evenly, then dissolve 33g of aluminum sulfate and 40g of potassium carbonate in an appropriate amount of water and add them to the above materials, mix and stir, extrude and shape into cylindrical catalyst precursors, and form The catalyst precursor was dried at 80° C. for 10 h to prepare the catalyst precursor particles with a particle size of 0.1 mm to 1 cm.

[0070] b, the preparation of mordenite

[0071] The catalyst precursor particles prepared by the dry glue method were statically crystallized under water vapor at 150° C. for 96 hours, and binder-free mordenite was synthesized in situ by an amine-free method.

[0072] c. Ammonium exchange of mordenite

[0073] The mordenite prepared above without binder was washed twice with water and mixed with NH at a concentration of 1mol / L 4 The Cl aqueous solution is mixed at a weight ratio of 1:30,...

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Abstract

The invention discloses a preparation method of a non-binder titaniferous mercerizing molecular sieve catalyst. The preparation method is characterized by comprising the following steps of: mixing sodium mercerizing zeolite raw powder as seed crystal with a silicon source, an aluminum source and an alkali source so as to prepare sial mercerizing zeolite with a dry rubber method; and then exchanging the sial mercerizing zeolite with ammonium, pickling, dealuminizing and reinforcing silicon in a gas-phase manner so as to prepare the non-binder titaniferous mercerizing molecular sieve catalyst, specifically comprising the steps of preparation of a catalyst precursor and mercerizing zeolite and crystallization, calcination, pickling and dealuminizing. Compared with the prior art, the method is simple, and the catalyst is convenient to prepare, so that the problems of separation difficulty, shortening of service life and the like during a ketones ammoximation process are efficiently solved, and effective utilization ratio and activity of the catalyst are greatly improved; and the non-binder titaniferous mercerizing molecular sieve catalyst has certain industrialized popularization and application prospects and obvious economic benefit.

Description

technical field [0001] The invention relates to the technical field of chemical catalytic materials and chemical applications, in particular to a method for preparing a binder-free titanium-containing mercerized molecular sieve catalyst for catalyzing the oximation reaction of cyclohexanone. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve first developed by Italian Eni company in the early 1980s. Ti-Si molecular sieves with microporous structures have been reported by research groups from various countries at present, including TS-1, Ti-MOR, Ti-MWW, Ti-Beta, and TS-2. Due to the four-coordinated titanium in the framework of titanium-silicon molecular sieves has the characteristics of oxidation-reduction catalysis, coupled with the shape selectivity of the molecular sieve framework itself, titanium-silicon molecular sieves have excellent directional catalytic oxidation performance. [0003] Wu et al. synthesized Ti-M...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/18C07C251/44C07C249/04
Inventor 吴鹏杨玉林丁姜宏吴海虹
Owner EAST CHINA NORMAL UNIV
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