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A kind of preparation method of silica-alumina molecular sieve

A silicon-alumina molecular sieve and aluminum source technology, which is applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of occupying land resources and inventory space, and cannot be recycled, and achieves the effect of high relative crystallinity and high yield

Active Publication Date: 2016-08-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the ammonia oximation catalyst TS-1 is permanently deactivated, it cannot be recycled at present, and it is mainly disposed of by stacking and landfilling
In this way, valuable land resources and storage space are taken up, and the recovery and utilization technology development of deactivated ammoximation catalysts is urgently needed

Method used

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  • A kind of preparation method of silica-alumina molecular sieve

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Effect test

preparation example Construction

[0009] The method for preparing silica-alumina molecular sieve provided by the present invention is characterized in that the deactivated cyclohexanone oximation catalyst is mixed with an acid solution for slurry treatment, and after solid-liquid separation, the solid, aluminum source and alkali solution are mixed at 100-200°C After processing, the product is taken out and recovered to obtain silica-alumina molecular sieve.

[0010] In more detail, the preparation method of silico-alumina molecular sieve provided by the present invention is characterized in that the deactivated cyclohexanone oximation catalyst and the molar concentration are first under normal temperature and pressure. 0.1mol / L acid solution is mixed and beaten, and then the mixed slurry is treated at 10~200℃ for 0.5~36h. After solid-liquid separation, the solid, aluminum source and alkali solution are mixed and treated at 100~200℃ for 0.5~24h, and then taken out The product is recovered to obtain a silica-alumina...

Embodiment 1

[0031] Under normal temperature and pressure, first mix the deactivated cyclohexanone oximation catalyst SH-1 with 1 mol / L hydrochloric acid solution to make a slurry, and then mix and stir the mixed slurry at 80°C for 12h. After solid-liquid separation, the solid, aluminum source aluminum sulfate and sodium hydroxide alkaline solution were mixed and treated at 170°C for 12 hours, where the mass of the material consisted of deactivated cyclohexanone oximation catalyst: aluminum source: acid: alkali: water = 100 :1:10:5:250, the deactivated cyclohexanone oximation catalyst is SiO 2 Calculated by H + Based on OH - meter. The obtained product was filtered, washed with water, dried at 110°C for 2 hours, and then calcined at 550°C for 3 hours to obtain molecular sieves. The XRD crystalline phase diagram has the same characteristics as the comparative sample, indicating that the obtained silica-alumina molecular sieve with MFI structure.

Embodiment 2

[0033] Under normal temperature and pressure, first mix the deactivated cyclohexanone oximation catalyst SH-1 with a 5mol / L hydrochloric acid solution to make a slurry, and then mix and stir the mixed slurry at 60°C for 1h. After solid-liquid separation, the solid, aluminum source aluminum isopropoxide and tetrapropylammonium hydroxide alkali solution were mixed and treated at 150°C for 12 hours, where the mass of the material consisted of deactivated cyclohexanone oximation catalyst: aluminum source: acid: Alkali: water = 100: 2: 15: 15: 200, the deactivated cyclohexanone oximation catalyst is SiO 2 Calculated by H + Based on OH - meter. Then, the crystallization product was recovered according to the method of Example 1 to obtain a silica alumina molecular sieve. Its XRD phase diagram has the same characteristics as the comparative sample.

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Abstract

The invention relates to a silicon-aluminum molecular sieve preparation method, which is characterized by comprising: at a room temperature, under a normal pressure, carrying out mixing pulping on an inactivate cyclohexanone oxime catalyst and an acid solution with a molar concentration of more than 0.1 mol / L, treating the obtained mixed pulp for 0.5-36 h at a temperature of 10-200 DEG C, carrying out solid-liquid separation, mixing the solid, an aluminum source and an alkali solution, treating for 0.5-24 h at a temperature of 100-200 DEG C, taking out the product, and recovering to obtain the silicon-aluminum molecular sieve, wherein the mass ratio of the inactivate cyclohexanone oxime catalyst (calculated as SiO2) to the aluminum source to the acid (calculated as H<+>) to the alkali (calculated as OH<->) to the water is 100:(0.1-10):(0.005-50):(0.5-50):(20-1000). With the method of the present invention, the inactivate cyclohexanone oxime catalyst can be utilized so as to turn the waste into treasure, and the relatively crystallinity of the molecular sieve is high.

Description

Technical field [0001] The invention relates to a method for preparing molecular sieves, and more specifically to a method for preparing silica-alumina molecular sieves by using a deactivated ammoximation catalyst. Background technique [0002] Molecular sieves are an important class of catalytic materials. For example, silica-alumina molecular sieve is a molecular sieve whose framework is composed of silicon, aluminum, and oxygen. Among them, ZSM-5 molecular sieve is a molecular sieve with (MFI) structure, which is widely used in petroleum refining and petrochemical industry. [0003] TS-1 molecular sieve is a new type of titanium silicate molecular sieve with excellent catalytic and selective oxidation performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. It ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
CPCC01B39/02C01P2006/12C01P2006/14
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP