CN108905377B - Preparation method of high-temperature ultrafine dust filter tube - Google Patents

Preparation method of high-temperature ultrafine dust filter tube Download PDF

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CN108905377B
CN108905377B CN201810794195.XA CN201810794195A CN108905377B CN 108905377 B CN108905377 B CN 108905377B CN 201810794195 A CN201810794195 A CN 201810794195A CN 108905377 B CN108905377 B CN 108905377B
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temperature
parts
purity
ultrafine dust
mixed powder
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CN108905377A (en
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顾益平
崔永杰
周成
许学良
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Jiangsu Kaichuang Environmental Protection Technology Co ltd
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Jiangsu Kaichuang Environmental Protection Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires

Abstract

The invention discloses a preparation method of a high-temperature ultrafine dust filter tube, which comprises the steps of uniformly mixing 50-85% of silicon carbide, 5-30% of cosmetic soil, 5-30% of epoxy grease, 2-20% of fused quartz sand, 2-20% of water glass and 0.05-3% of preservative by mass percent, grinding to obtain mixed powder, mixing with deionized water to obtain slurry, extruding the material by using a variable-frequency speed-regulating rotating rod in a rotary extrusion forming mode, forming the material under a certain pressure, covering with a film, and finally firing in a kiln to obtain the high-temperature ultrafine dust filter tube. The preparation process has the advantages of simple operation, good repeatability, uniform mixing and reaction, short preparation time, low sintering temperature, low energy and cost, good high-temperature oxidation resistance and suitability for filtering ultrafine dust at high temperature.

Description

Preparation method of high-temperature ultrafine dust filter tube
Technical Field
The invention belongs to the technical field of dust filter pipe manufacturing, and particularly relates to a preparation method of a high-temperature ultrafine dust filter pipe.
Background
In chemical industry, metallurgy, petroleum, electric power and other industries, a large amount of high-temperature dust-containing gas is often discharged, so that the atmospheric environment is seriously polluted, and meanwhile, the health of a human body is also greatly threatened. On the basis, the high-temperature dust-containing gas needs to be subjected to dust removal treatment, so that the standard of environmental protection emission is met, and the pollution is reduced. However, under high temperature conditions, the fine particle agglomeration phenomenon is greatly reduced, the separation of the fine particles is difficult, and engineering problems such as equipment material, structural form and thermal expansion adopted at high temperature often influence the effective normal operation of the equipment. Therefore, how to effectively remove dust under high temperature is a problem with high difficulty.
In the field of high-temperature dust removal, a large part of the problems are solved for purifying high-temperature flue gas, and the atmospheric pollution in China is mainly bituminous coal type pollution, so that the high-temperature dust removal technology is closely related to the clean coal technology. The traditional thermal power generation technology mainly using coal not only has low energy utilization efficiency, but also has serious dust pollution, and brings serious threat to the environment. Therefore, new thermal power generation systems with high energy utilization rate and almost no dust emission, such as clean coal power generation systems of Integrated Gasification Combined Cycle (IGCC), pressurized fluidized bed combustion combined cycle (PFBC), and the like, have been widely favored by scientific researchers. Under the dual pressure of increasing energy demand and aggravating environmental pollution, the development of clean coal technology combines resource conservation with environmental protection, and is beneficial to realizing the sustainable development of national economy in China. In the clean coal power generation systems, coal is gasified at high temperature to form crude gas containing a large amount of dust, the crude gas is subjected to dust removal by a high-temperature dust removal subsystem, and then the clean gas can be combusted in a gas turbine to generate power after sulfur and nitrogen removal. If the content of dust in the clean coal gas exceeds the standard, the blade of the gas turbine is seriously damaged, and the service life of the gas turbine is shortened. Wherein, the development and research of the high-temperature dust removal technology is the favorable guarantee for implementing the clean coal technology.
The high-temperature high-efficiency dust removal technology is characterized in that: the temperature of the dust-containing gas to be purified is high (600-pLess than 5-10 μm, high purification standard (outlet concentration is required to be 10-50 mg/m)3). The simple gas-solid separation device is far from meeting the requirement of high-temperature and high-efficiency dust removal. The commonly used dust removal methods include wet dust removal, electrostatic dust removal, multi-tube dust removal, high-temperature filtration dust removal and the like. The high temperature filter has high separation efficiency, and the filtering material is special metal and microporous ceramic. However, the filter materials made of high-temperature resistant materials are generally high in cost and difficult to regenerate after failure, and the filter materials are damaged, deformed and failed quickly under severe working conditions of high temperature and high dust, so that the problems of high operation cost, low working efficiency and the like exist, and the industrial application of the high-temperature filter is restricted. Therefore, the development and research of a novel high-temperature filter is a problem which needs to be solved urgently in the current high-temperature dust removal research.
At present, researchers at home and abroad are working on Al2O3A series of studies have been made on the dust removal efficiency of porous materials such as (corundum), MAS (cordierite), and aluminum titanate. Plum health care and other people have prepared porous ceramic filter tubes for dust filtration by taking mullite fiber and the like as main materials (Chinese invention patent, ZL 201010265544.2). Wu Xiaolin et al proposed a high temperature filtration tube fabrication apparatus and method (Chinese invention patent, ZL 201310058575.4). But corundum resistanceThe materials are difficult to popularize and use due to the problems of poor thermal shock property, high price, non-corrosion resistance of cordierite, high price of mullite fiber and the like. Silicon carbide is a compound with extremely strong covalent bond, has good high temperature resistance and chemical corrosion resistance, high strength, good thermal shock stability, high filtration precision and long service life, can be used as a filter element of a high-temperature dust removal device, is irreplaceable for other filter materials, and is difficult to fully exert the excellent performance of related products due to the shortage of the existing formula and sintering technology. So far, the best performance parameters of similar products at home and abroad are 38% of porosity and 20MPa of strength, so that the research and development of silicon carbide filter materials with high strength, high porosity, high uniformity, low resistance drop, corrosion resistance, high temperature resistance and other performances is urgent.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects of the existing preparation technology of the dust filter pipe, the invention provides a preparation method of a high-temperature ultrafine dust filter pipe with high-temperature oxidation resistance and low preparation cost.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of a high-temperature ultrafine dust filter tube comprises the following steps:
(1) uniformly mixing 50-85 parts by mass of silicon carbide, 5-30 parts by mass of cosmetic clay, 5-30 parts by mass of epoxy grease, 2-20 parts by mass of fused quartz sand, 2-20 parts by mass of water glass and 0.05-3 parts by mass of preservative, and grinding to obtain mixed powder;
(2) fully and uniformly mixing the mixed powder obtained in the step (1) with deionized water accounting for 5-15% of the mass of the mixed powder to obtain slurry;
(3) coating the slurry obtained in the step (2) in a mould, extruding the material by using a variable-frequency speed-regulating rotating rod in a rotary extrusion forming mode, and pressing and forming the material under certain pressure;
(4) and (4) coating a mullite film layer on the molded dry material obtained in the step (3).
(5) And (5) placing the material obtained in the step (4) in a kiln, and firing at a certain temperature to obtain a final finished product.
Preferably, in the step (1), the purity of the silicon carbide is more than or equal to 97%, and the granularity is 10-90 μm.
In the step (1), the purity of the makeup soil is more than or equal to 90%, and the granularity is 10-60 mu m.
In the step (1), the purity of the epoxy grease is more than or equal to 98%.
In the step (1), the purity of the fused quartz sand is more than or equal to 97%, and the granularity is 3-50 μm.
In the step (1), the modulus of the water glass is 1.5-3.5.
In the step (1), the pH value of the preservative is 2-4.5.
In the step (3), the specific conditions of the rotary extrusion forming are as follows: the rotating speed of the variable-frequency speed-regulating rotating rod is 10-60r/min, the pressure is 0.5-2MPa, and the pressure maintaining time is 5-30 s.
In the step (4), the firing time is 12-15 h, and the sintering temperature is 1200-1500 ℃.
The performance of the finished product of the high-temperature ultrafine dust filter tube prepared by the method of the invention meets the following indexes: the porosity is 41%, the strength is 28-31 MPa, and the specific gravity is 1.75.
The invention has the beneficial effects that: compared with the prior art, the invention provides the method for preparing the high-temperature ultrafine dust filter tube, which is simple to operate and high in reproducibility. The method is simple to operate, high in reproducibility, safe and reliable; the obtained dust filter pipe has the characteristics of ultrafine dust blockage resistance, excellent high-temperature oxidation resistance, acid and alkali corrosion resistance, low surface resistance, high dust removal efficiency, long service life and the like, and has a very wide application prospect.
Drawings
FIG. 1 is a scanning electron micrograph of the microstructure of the sample of example 1.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
Example 1
The high-temperature ultrafine dust filter tube is prepared according to the following steps:
(1) by mass, uniformly mixing 55 parts of silicon carbide (with the granularity of 90 mu m and the purity of 97 percent), 25 parts of cosmetic soil (with the purity of more than or equal to 93 percent and the granularity of 40 mu m), 8 parts of epoxy grease (with the purity of more than or equal to 98 percent), 6 parts of fused quartz sand (with the purity of more than or equal to 97 percent and the granularity of 40 mu m), 6 parts of water glass (with the modulus of 2.5) and 0.05 part of preservative (with the pH value of 4), and grinding the mixture until the particle size is 80 mu m to obtain mixed powder;
(2) fully and uniformly mixing the mixed powder with deionized water accounting for 15% of the mass of the mixed powder to obtain slurry;
(3) coating the slurry in a die, extruding the material by a variable-frequency speed-regulating rotating rod in a rotary extrusion forming mode, and pressing and forming the material under certain pressure; wherein, the specific conditions of the rotary extrusion forming are as follows: the rotating speed of the variable-frequency speed-regulating rotating rod is 20r/min, the pressure is 1.5MPa, and the pressure maintaining time is 20S.
(4) Coating the formed dry material with a film of 20 μm,
(5) and (3) placing the materials in a kiln, and sintering at 1300 ℃ for 12h to obtain a final finished product.
The cross-sectional electron microscope picture (figure 1) of the obtained high-temperature ultrafine dust filter tube shows that the product produced by the filter tube by adopting the novel formula and the forming process has the properties of high strength, high porosity, high uniformity, low resistance reduction and the like. The detected correlation properties are as follows: the porosity is 41%, the strength is 28-31 MPa, the specific gravity is 1.75, and the precise filtration of high-temperature and high-corrosion gas is completely met.
Example 2
The high-temperature ultrafine dust filter tube is prepared according to the following steps:
(1) uniformly mixing 70 parts of silicon carbide (with the granularity of 60 mu m and the purity of 98%), 10 parts of cosmetic soil (with the purity of more than or equal to 90% and the granularity of 20 mu m), 10 parts of epoxy grease (with the purity of more than or equal to 98%), 5 parts of fused quartz sand (with the purity of more than or equal to 97% and the granularity of 20 mu m), 5 parts of water glass (with the modulus of 3.5) and 0.1 part of preservative (with the pH value of 2) in parts by mass, and grinding the mixture until the particle size is 50 mu m to obtain mixed powder;
(2) fully and uniformly mixing the mixed powder with deionized water accounting for 12% of the mass of the mixed powder to obtain slurry;
(3) coating the slurry in a die, extruding the material by a variable-frequency speed-regulating rotating rod in a rotary extrusion forming mode, and pressing and forming the material under certain pressure; wherein, the specific conditions of the rotary extrusion forming are as follows: the rotating speed of the variable-frequency speed-regulating rotating rod is 50r/min, the pressure is 0.5MPa, and the pressure maintaining time is 5 s;
(4) coating the formed dry material with a film of 20 μm;
(5) and (3) placing the materials in a kiln, and sintering at 1500 ℃ for 15h to obtain a final finished product.
According to the embodiment, the obtained high-temperature ultrafine dust filter pipe has the advantages of 41% of porosity, 28-31 MPa of strength and 1.75 of specific gravity, and the filter pipe has good use value and can be put into production.
Example 3
The high-temperature ultrafine dust filter tube is prepared according to the following steps:
(1) uniformly mixing 50 parts of silicon carbide (the granularity is 50 microns, the purity is 99%), 25 parts of cosmetic soil (the purity is more than or equal to 90%, the granularity is 60 microns), 10 parts of epoxy grease (the purity is more than or equal to 98%), 8 parts of fused quartz sand (the purity is more than or equal to 97%, the granularity is 10 microns), 7 parts of water glass (the modulus is 1.5) and 0.5 part of preservative (the pH is 3) in parts by mass, and grinding the mixture until the particle size is 20 microns to obtain mixed powder;
(2) fully and uniformly mixing the mixed powder with water accounting for 8% of the mass of the mixed powder to obtain slurry;
(3) coating the slurry in a die, extruding the material by a variable-frequency speed-regulating rotating rod in a rotary extrusion forming mode, and pressing and forming the material under certain pressure; wherein, the specific conditions of the rotary extrusion forming are as follows: the rotating speed of the variable-frequency speed-regulating rotating rod is 30r/min, the pressure is 2MPa, and the pressure maintaining time is 30 s.
(4) Coating the formed dry material with a film of 20 μm;
(5) and (3) placing the materials in a kiln, and sintering at 1500 ℃ for 15h to obtain a final finished product.
According to the above example, the obtained high-temperature ultrafine dust filter pipe has the porosity of 41%, the strength of 28-31 MPa and the specific gravity of 1.75, and shows that the filter pipe has good use value and can be put into production.
Example 4
The high-temperature ultrafine dust filter tube is prepared according to the following steps:
(1) uniformly mixing 80 parts of silicon carbide (the granularity is 90 mu m and the purity is 97 percent), 8 parts of cosmetic soil (the purity is more than or equal to 93 percent and the granularity is 40 mu m), 5 parts of epoxy grease (the purity is more than or equal to 98 percent), 3 parts of fused quartz sand (the purity is more than or equal to 97 percent and the granularity is 40 mu m), 4 parts of water glass (the modulus is 2.5) and 0.1 part of preservative (the pH is 4) in parts by mass, and grinding the mixture until the particle size is 80 mu m to obtain mixed powder;
(2) fully and uniformly mixing the mixed powder with deionized water accounting for 15% of the mass of the mixed powder to obtain slurry;
(3) coating the slurry in a die, extruding the material by a variable-frequency speed-regulating rotating rod in a rotary extrusion forming mode, and pressing and forming the material under certain pressure; wherein, the specific conditions of the rotary extrusion forming are as follows: the rotating speed of the variable-frequency speed-regulating rotating rod is 20r/min, the pressure is 1.5MPa, and the pressure maintaining time is 20S.
(4) Coating the formed dry material with a film of 20 μm,
(5) and (3) placing the materials in a kiln, and sintering for 13 hours at 1400 ℃ to obtain a final finished product.
The cross-sectional electron microscope picture (figure 1) of the obtained high-temperature ultrafine dust filter tube shows that the product produced by the filter tube by adopting the novel formula and the forming process has the properties of high strength, high porosity, high uniformity, low resistance reduction and the like. The detected correlation properties are as follows: the porosity is 41%, the strength is 28-31 MPa, the specific gravity is 1.75, and the precise filtration of high-temperature and high-corrosion gas is completely met.

Claims (1)

1. A preparation method of a high-temperature ultrafine dust filter tube is characterized by comprising the following steps:
(1) uniformly mixing 80 parts of silicon carbide, 8 parts of cosmetic clay, 5 parts of epoxy grease with the purity of more than or equal to 98%, 3 parts of fused quartz sand, 4 parts of water glass and 0.1 part of preservative in parts by mass, and grinding the mixture until the particle size is 80 microns to obtain mixed powder; wherein the granularity of the silicon carbide is 90 μm, and the purity of the silicon carbide is 97%; the purity of the makeup soil is more than or equal to 93 percent, and the granularity is 40 mu m; the purity of the fused quartz sand is more than or equal to 97 percent, and the granularity is 40 mu m; the modulus of the water glass is 2.5; the pH of the preservative is 4;
(2) fully and uniformly mixing the mixed powder with deionized water accounting for 15% of the mass of the mixed powder to obtain slurry;
(3) coating the slurry in a die, extruding the material by a variable-frequency speed-regulating rotating rod in a rotary extrusion forming mode, and pressing and forming the material under certain pressure; wherein, the specific conditions of the rotary extrusion forming are as follows: the rotating speed of the variable-frequency speed-regulating rotating rod is 20r/min, the pressure is 1.5MPa, and the pressure maintaining time is 20 s;
(4) coating the formed dry material with a film of 20 μm,
(5) and (3) placing the materials in a kiln, and sintering for 13 hours at 1400 ℃ to obtain a final finished product.
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US6155432A (en) * 1999-02-05 2000-12-05 Hitco Carbon Composites, Inc. High performance filters based on inorganic fibers and inorganic fiber whiskers
FR2911869B1 (en) * 2007-01-29 2011-05-20 Saint Gobain Ct Recherches PROCESS FOR PRODUCING A CERAMIC POROUS CORE BASED ON SIC
CN102964124B (en) * 2011-01-07 2015-02-11 宜兴市鑫帝豪高科陶瓷厂 High-temperature gas-solid ceramic filter tube and preparation method
CN103566778B (en) * 2012-07-27 2015-09-23 佛山市南海区西樵金刚科技有限公司 A kind of inorganic film tube and preparation method thereof
CN103111132B (en) * 2013-02-25 2014-12-24 中国石油大学(北京) Manufacturing device of filtering tube applied to high-temperature gas filtration and method of filtering tube
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CN105000906A (en) * 2015-06-24 2015-10-28 左然 Pressurelessly-sintered silicon carbide foamed ceramic and preparation method thereof
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