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Preparation method of diatomite-based porous ceramic microspheres

A technology of diatomite and porous ceramics, which is applied in the field of catalyst carrier preparation, can solve the problems of complex process, single pore size distribution, and high production cost, and achieve the effects of simple process, large specific surface area, and low production cost

Inactive Publication Date: 2012-03-28
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent "Preparation Method of Microspherical Silica as Carrier of Olefin Polymerization Catalyst" (200410039492.1) discloses a technology for preparing microspherical silica by sol-gel method, but the process conditions are complicated, the production cost is high, and the sphericity is poor ; U.S. Patent "Macroporous Microspheroids and a Process for Their Manufacture" (US4070286) discloses a method for preparing silica microspheres with a single pore distribution by polycondensation, but the particle size is small, and the average particle size is only 5-9 μm. Difficult to control, single pore size distribution, low yield, poor sphericity; U.S. Patent "Bodies of Siliceous Gels Having Large Pores and Process for Preparing Same" (US3975293) discloses a method for preparing silica microspheres in an autoclave, and also The same harsh reaction conditions, high production cost, low yield, poor sphericity; U.S. Patent "Process for the Production of Hydrocarbons" (US5504118) and Chinese Patent Application "Production Method of Hydrocarbons" (CN1113905A) disclose a method for Catalyst carrier for the synthesis of slurry bed reaction, but the sphericity is poor and the particle size is small, only 5-50 μm, which is not conducive to the online separation of wax and catalyst in the slurry bed; Zhao et al., University of Pittsburgh, USA in Ind. Eng. Chem. Res., 2001, 40, 1065~1075 discloses a preparation method of a catalyst for a slurry bed and a carrier thereof. This technology uses ethyl orthosilicate, copper nitrate, and iron nitrate as raw materials, and obtains precipitation by adding ammonia water slurry, then add KHCO 3 Aqueous solution and a certain amount of SiO 2 Binder, made by beating, spray drying, calcination and other processes
This method adopts ethyl orthosilicate as raw material, the cost is high, and the technological process is complicated at the same time

Method used

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  • Preparation method of diatomite-based porous ceramic microspheres
  • Preparation method of diatomite-based porous ceramic microspheres
  • Preparation method of diatomite-based porous ceramic microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 200g of diatomite raw material, 0.2g of carbon powder, add 0.2g of sodium carboxymethyl cellulose, and add 250mL of water at the same time, wet ball milling, the ratio of material to ball is 1: 0.2, ball milling for 0.5h, and the slurry is passed through 250 mesh Sieve; then spray dry the slurry into balls, the spray drying process parameters are: drying air temperature 350°C, spray head speed 2000rpm, spray tower internal pressure -80Pa; the microspheres prepared by spray drying are fired at 1200°C, and Keep warm for 1 hour to form porous ceramic microspheres. The results of phase analysis before and after the calcination of the microspheres are shown in the attached figure 1 As shown, the main crystal phase of the microspheres before calcination is opal, and after calcination at 1200°C, the main crystal phase is cristobalite. attached figure 2 It is the scanning electron microscope image of microspheres after calcination. It can be seen from the figure that t...

Embodiment 2

[0027] Take the diatomite raw material of 200g, 15g calcium carbonate, add 0.3g sodium carboxymethyl cellulose and 0.2g sodium hexametaphosphate, add 160mL water simultaneously, wet method ball milling, material-ball ratio is 1: 0.5, ball milling 5h, The slurry is passed through a 250-mesh sieve; then the slurry is spray-dried into balls. The spray-drying process parameters are: drying air temperature 250°C, spray head speed 5000rpm, spray tower internal pressure -110Pa; spray-dry the prepared microspheres at 900 ℃ firing, and heat preservation 0.1h, that is, porous ceramic microspheres.

Embodiment 3

[0029] Weigh 200g of diatomite raw material, 12.5g of polyethylene glycol, 40g of soluble starch, add 1g of sodium hexametaphosphate, and add 160mL of water at the same time, wet ball milling, the ratio of material to ball is 1: 2, ball milling for 10h, and the slurry is passed 250 mesh sieve; then spray dry the slurry into balls, the spray drying process parameters are: drying air temperature 250°C, spray head speed 12000rpm, spray tower internal pressure -200Pa; the microspheres prepared by spray drying are fired at 1200°C , and keep warm for 3h, that is, porous ceramic microspheres.

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Abstract

The invention discloses a preparation method of diatomite-based porous ceramic microspheres. According to the invention, diatomite is adopted as a main material, and the ceramic microspheres with high sphericity (good fluidity), large specific area, and controllable particle sizes are prepared through spray-drying. The diatomite-based porous ceramic microspheres can be used as catalyst carriers in slurry-bed reactions such as Fischer-Tropsch synthesis. The method provided by the invention is advantaged in wide material source, simple technological process, low production cost, and suitabilityfor large-scale continuous industrialized productions. The method has good application values.

Description

technical field [0001] The invention relates to a method for preparing a catalyst carrier, in particular to a method for preparing porous ceramic microspheres using diatomite as a raw material. Background technique [0002] With the progress and development of human civilization, the world's fossil resources are increasingly depleted, and the supply situation of mineral oil is becoming increasingly severe. The problem of energy shortage has become one of the important factors restricting the economic development of all countries in the world. As a green and renewable energy source, new biodiesel (i.e. second-generation biodiesel) has become a research hotspot all over the world due to its many advantages such as wide source of raw materials, low production cost, less pollution, and high quality. The second-generation biodiesel is prepared from biomass (such as rice straw, sawdust, etc.) through gasification, Fischer-Tropsch synthesis, hydrogenation and other processes. Prep...

Claims

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Application Information

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IPC IPC(8): C04B38/00C04B35/14C04B35/622
Inventor 税安泽汪强虹程小苏刘平安潘志东王燕民
Owner SOUTH CHINA UNIV OF TECH
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