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Preparation method of wear-resistant large-pore-volume microspherical silica carrier

A technology of spherical silica and large pore volume, used in catalyst supports, chemical instruments and methods, chemical/physical processes, etc., can solve the problem of reducing the mechanical strength and wear resistance of the carrier, the wear resistance of the carrier cannot be greatly improved, and the sintering Poor performance and other problems, to achieve the effect of stable catalytic reaction performance, not easy to break, and good sintering performance

Inactive Publication Date: 2016-03-30
钟俊超
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, preparing a microspherical silica carrier with suitable pore structure, mechanical strength and wear resistance is a technical problem in this field, because silica raw materials such as precipitated silica and fumed silica are usually sintered The performance is poor; using silica sol as a binder can improve the mechanical strength and wear resistance of the silica carrier, but the effect is limited. Even after recrystallization treatment such as hydrothermal treatment, the wear resistance of the carrier cannot be greatly improved
Using alumina, calcium oxide, kaolin, etc. as a binder can also improve the mechanical strength and wear resistance, but under acidic conditions, the acid-resistant components contained in the binder will be eroded, making the mechanical strength and wear resistance of the carrier Abrasiveness will gradually decrease

Method used

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  • Preparation method of wear-resistant large-pore-volume microspherical silica carrier
  • Preparation method of wear-resistant large-pore-volume microspherical silica carrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take 1000g of calcined silica powder A, put it into a mixing tank, add 3000g of deionized water, start stirring and beating, after the dispersion is uniform, use a homogenizer to grind and disperse to the average particle diameter of 5um, transfer to an autoclave, add 200g of acetic acid, acetic acid Ammonium 50g sizing liquid pH value to 3.5, crystallization treatment at 150°C for 40hrs, cooling to 60°C, the specific surface area of ​​silica particles was measured to be 122m 2 / g; add 2000g activated carbon emulsion M (containing activated carbon 200g, the average diameter of activated carbon microparticles is 1.5um), mix well after stirring for 10 minutes, add 600g acidic silica sol D (SiO mass concentration 30%, Na 2 (00.06%, colloidal average diameter 10nm), mix after stirring 10 minutes, pump into the centrifugal spray granulator that has been preheated to 200 ℃ of working temperature and carry out granulation and adjust the rotating speed of feed pump and centrifug...

Embodiment 2

[0042] The other half of the granulated micropowder in Example 1 was calcined at 720° C. for 3 hours to obtain the microspherical silica carrier with large pore volume of the present invention. The average diameter of the measured carrier is 213um, the sphericity is good, and the strength is good; the specific surface area is 100m 2 / g, the pore volume is 0.90ml / g, and the average pore diameter is 39nm; the measured wear rate and fragmentation rate are relatively low, see the data listed in the table below for details.

Embodiment 3

[0044] Take 1000g of calcined silica powder B, put it into the mixing tank, add 3000g of deionized water, start stirring and beating, after the dispersion is uniform, use a homogenizer to grind and disperse to the average particle diameter of 5um, transfer to the autoclave, add 200g of acetic acid, acetic acid Ammonium 100g sizing liquid pH value to 4.0, crystallization treatment at 165°C for 20hrs, cooling to 60°C, measured specific surface area of ​​silica particles 102m 2 / g, add 2500g activated carbon emulsion M (containing activated carbon 250g, the average diameter of activated carbon microparticles is 1.5um), mix well after stirring for 10 minutes, add 1200g acidic silica sol E (silica mass concentration 20%, Na 2 (00.10%, colloidal average diameter 20nm), mix after stirring 10 minutes, pump into the centrifugal spray granulator that has been preheated to 240 ℃ of working temperature and carry out granulation and adjust the rotating speed of feed pump and centrifuge, mak...

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Abstract

The invention provides a preparation method of a wear-resistant large-pore-volume microspherical silica carrier. The preparation method comprises the steps: roasting a precipitated silicon dioxide powder or white carbon black with the specific surface area of 250-600 m<2> / g at the temperature of 730-760 DEG C to make the specific surface area reduced to 100-220 m<2> / g; adding water, mixing evenly, and grinding silicon dioxide micro-particles to the average diameter of 2-5 [mu]m; adding acetic acid and ammonium acetate, and performing crystallization treatment at the temperature of 150-180 DEG C; and adding an activated carbon emulsion and acidic silica sol, mixing evenly, performing spray granulation, and roasting the granulation powder at the temperature of 650-720 DEG C. The prepared carrier has proper pore structure including higher specific surface area, pore volume and larger average pore size, has higher mechanical strength, higher wear resistance and higher impact resistance, is suitable for further loading active components, and is used for preparation of a catalyst for fluidized beds.

Description

technical field [0001] The invention belongs to the field of catalysts, and relates to a method for preparing a microspherical silica carrier, in particular to a method for preparing a wear-resistant microspherical silica carrier with a large pore volume. Background technique [0002] In addition to having a suitable pore structure, the catalyst should also have high mechanical strength and wear resistance, especially in the fluidized bed, between catalyst particles, between catalyst particles and the inner wall of the reactor, between catalyst particles and the solid phase in the fluidized bed There will be frequent friction and collision between the reaction raw materials or products, and the formed broken particles will expand the fluidized bed layer, and the formed finer powder, such as the part below 10-15um, is easy to blow off the fluidized bed, basically Scrapped. [0003] Preparing the carrier first, and then impregnating the active component is the most commonly u...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J21/08B01J35/10
CPCB01J21/08B01J35/613B01J35/615B01J35/638B01J35/635B01J35/647
Inventor 钟俊超
Owner 钟俊超
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