CN113277873A - Preparation method of slag fiber-based porous filtering ceramic - Google Patents

Preparation method of slag fiber-based porous filtering ceramic Download PDF

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CN113277873A
CN113277873A CN202110539656.0A CN202110539656A CN113277873A CN 113277873 A CN113277873 A CN 113277873A CN 202110539656 A CN202110539656 A CN 202110539656A CN 113277873 A CN113277873 A CN 113277873A
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slag
fiber
slag fiber
based porous
ceramic
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钱磊
谢娇
岳凯成
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Shandong University
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    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0038Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract

The invention belongs to the field of materials, and discloses a preparation method of slag fiber-based porous filtering ceramic, which comprises the following steps: putting the slag fiber into a mould to be pressurized for one time to form slag short fiber; uniformly mixing the slag short fibers with a binder, and putting the mixture into a die for secondary pressurization to form a pressed sheet; and sintering the pressed sheets, preserving heat and cooling to obtain the slag fiber-based porous filtering ceramic. The product obtained by the invention is slag fiber porous ceramic, has certain strength, high temperature resistance and low cost, and can effectively reduce the high cost of treating high-temperature waste gas at present.

Description

Preparation method of slag fiber-based porous filtering ceramic
Technical Field
The invention belongs to the field of materials, and particularly relates to a preparation method of slag fiber-based porous filtering ceramic.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the rapid development of economy, the environmental pollution problem caused by heavy industrial production of steel, chemical industry, cement and the like is increasingly serious. The heavy industrial production has the characteristics of low fuel heat utilization rate, high energy consumption, large waste gas emission, high temperature, complex components, fine dust particles and the like. The fine industrial waste gas dust floats in the atmosphere and is difficult to settle, haze is very easy to be induced, and great harm is brought to the health and daily life of residents. At present, in the aspect of industrial filtration and dust removal treatment, the research and development of domestic industrial technologies are late and slow, the technical content of methods and equipment used by enterprises is low, the energy consumption is high, the efficiency is poor, and the gap between the methods and the equipment used by enterprises and developed countries is large. Therefore, the research and development of a novel high-efficiency industrial filtering and dedusting technology becomes an urgent problem to be solved, the application value is high, the market prospect is wide, and the method has important significance for promoting the sustainable development of industrial economy in China.
However, at present, domestic porous filtering ceramics generally use ceramic powder as a raw material, and are prepared by adding pore-forming agents, plasticizers, binders and the like through molding and sintering processes. The price of the ceramic powder is higher, the production efficiency is reduced and the cost is increased due to the addition of the pore-forming agent, and the sintering temperature of the ceramic is higher, so that the defects restrict the industrialization and the popularization of the practical engineering application of the high-temperature resistant porous filtering ceramic.
Disclosure of Invention
In order to overcome the problems, the invention provides a preparation method of slag fiber-based porous filtering ceramic, which takes slag fibers as raw materials, does not add pore-forming agents, adopts a normal-pressure sintering process to prepare high-temperature-resistant fiber-based porous ceramic for filtering and dedusting, optimizes a high-efficiency, environment-friendly and low-cost preparation technology of porous filtering ceramic, provides a safe, green, high-efficiency, low-cost preparation method of porous filtering ceramic capable of being produced in large scale, and is expected to be applied to the fields of industrial waste gas dedusting, high-temperature-resistant filtering, catalyst carriers and the like.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a method for preparing a slag fiber-based porous filter ceramic, comprising:
putting the slag fiber into a mould to be pressurized for one time to form slag short fiber;
uniformly mixing the slag short fibers with a binder, and putting the mixture into a die for secondary pressurization to form a pressed sheet;
and sintering the pressed sheets, preserving heat and cooling to obtain the slag fiber-based porous filtering ceramic.
The research of the invention finds that: slag produced in the steel making process is made into slag fiber, the main component of which is aluminosilicate and also contains small amounts of Mg, Ca and Fe. The slag fiber is low in price, has a good fiber structure and good high temperature resistance and corrosion resistance, and is an ideal raw material for preparing porous ceramic. Meanwhile, because the fibers have the characteristic of low strength, the fibers are sheared into short fibers in a pressurizing mode, the obtained short fibers have better dispersibility, and the porosity of the prepared porous ceramic is higher after subsequent pressurizing and sintering.
In a second aspect of the invention, there is provided a slag fiber-based porous filter ceramic produced by any of the above-described methods.
The operation method is simple, low in cost, universal and easy for large-scale production.
In a third aspect of the present invention, there is provided the use of the above-described slag fiber-based porous filter ceramic in the fields of industrial exhaust gas dust removal, high temperature filtration and catalyst support.
The slag fiber-based porous filtering ceramic prepared by the invention has low cost, high porosity and excellent performance, so the slag fiber-based porous filtering ceramic is expected to be widely applied to the fields of industrial waste gas dust removal, high-temperature-resistant filtration and catalyst carriers.
The invention has the beneficial effects that:
(1) the product obtained by the invention is slag fiber porous ceramic, has certain strength, high temperature resistance and low cost, and can effectively reduce the high cost of treating high-temperature waste gas at present.
(2) The slag fiber is used as a raw material, the short fiber is obtained by pressing, and the porous ceramic obtained by pressure forming and sintering has high porosity and excellent performance.
(3) The operation method is simple, low in cost, universal and easy for large-scale production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is an electron microscope image and an object image of the porous ceramic prepared by the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
A preparation method of slag fiber-based porous filtering ceramic comprises the following steps:
putting the slag fiber into a mould to be pressurized for one time to form slag short fiber;
uniformly mixing the slag short fibers with a binder, and putting the mixture into a die for secondary pressurization to form a pressed sheet;
and sintering the pressed sheets, preserving heat and cooling to obtain the slag fiber-based porous filtering ceramic.
In order to obtain the slag fiber-based porous ceramic, the system provided by the invention researches the relationship between the shearing pressure of the slag fiber, the forming pressure and the sintering temperature of a ceramic blank and the porosity of the ceramic, so that in some embodiments, the diameter of the slag fiber is 2-7 μm, the length can reach a millimeter level, and the length-diameter ratio can reach more than 800, so as to prepare the porous ceramic with adjustable porosity.
In order to effectively shape the porous ceramic and obtain better mechanical properties, a certain amount of binder is added into slag fiber. In some embodiments, the mass ratio of slag fiber to binder is 100: 1-7, and the test result shows that: within the dosage range, the prepared slag fiber-based porous filtering ceramic has higher porosity.
The type of binder is not particularly limited in this application and in some embodiments, the binder is sodium silicate to better mix with the slag fibers and disperse them thoroughly, resulting in good flow characteristics when heated.
The research finds that: the shearing effect on the slag fibers is enhanced as the pressurizing pressure is increased, but if the pressure is too high, the porosity of the porous ceramic is affected. Therefore, in some embodiments, the primary pressurization pressure is 3MPa to 20MPa to ensure that the prepared ceramic has high porosity.
Compared with a chopping machine, the pressurizing device has the advantages of simplicity, quickness and convenience in operation, can effectively shear slag fibers, can be operated only by a simple hydraulic press, does not need to purchase other equipment, and has no influence on fiber components and microstructures.
The research finds that: the bonding of slag fibers and densification of the material are promoted with the increase of the pressure, but if the pressure is too high, the subsequent increase of the opening ratio is not facilitated. Therefore, in some embodiments, the secondary pressurization pressure is 5MPa to 20MPa, so that the prepared slag fiber-based porous filtering ceramic has high porosity.
In some embodiments, the sintering is performed by a burying method, and preferably, the burying medium is aluminum oxide.
In some embodiments, the sintering temperature is 800-1000 ℃, preferably, sintering is performed at 5-8 ℃/min, and heat preservation is performed for 2-2.5 h.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
In the following examples, the slag fibers were examined and analyzed to have the following main components: SiO 22:~38.5%;Al2O3: -21.2%; MgO accounts for 16.8 percent; CaO 23.5%, wherein "" represents "about";
the porosity of the sample was measured using the archimedes drainage method.
The modulus of sodium silicate is 1.06.
Example 1:
s1, taking out 2g of slag fiber, putting the slag fiber into a die, and shearing the slag fiber under the pressure of a hydraulic press (the pressure range is 3MPa-20MPa), so as to obtain 2g of slag short fiber.
S2, putting the obtained slag short fibers into a beaker, adding sodium silicate binders (1 wt%, 3 wt%, 5 wt% and 7 wt% respectively) in different mass ratios, and uniformly mixing by using a medicine spoon.
S3, putting the mixture obtained in the step 2 into a mold, and pressurizing by using a hydraulic press (the pressurizing range is 5MPa-20MPa) to obtain a circular tablet with the diameter of 20 mm.
S4, sintering the round pressed sheet obtained in the step 3 by adopting a burial method, wherein the burial medium is aluminum oxide, the sintering temperature is variable (experiments are respectively carried out at 800 ℃, 900 ℃ and 1000 ℃), the sintering rate is 5 ℃/min, and the temperature is kept for 2 h.
And S5, obtaining a molded sample after the molded sample is naturally cooled to the temperature in the furnace.
And S6, measuring physical properties such as porosity and the like of the sample, and replacing variables for multiple experiments to obtain an optimal scheme.
The detection result shows that: the porosity of the prepared porous ceramic ranges from 30 to 55 percent.
Example 2:
s1, taking out 2g of slag fiber, putting the slag fiber into a die, and shearing the slag fiber under the pressure of a hydraulic press (the pressure is 10MPa), so as to obtain 2g of slag short fiber.
S2, putting the obtained slag short fibers into a beaker, adding a sodium silicate binder (taking 3 wt%), and uniformly mixing by using a spoon.
S3, putting the mixture obtained in the step 2 into a mold, and pressurizing by using a hydraulic press (pressurization is 20MPa) to obtain a circular tablet with the diameter of 20 mm.
S4, sintering the round pressed sheet obtained in the step 3 by adopting a burial method, wherein a burial medium is aluminum oxide, the sintering temperature is 800 ℃, the sintering speed is 5 ℃/min, and the temperature is kept for 2 h.
And S5, obtaining a molded sample after the molded sample is naturally cooled to the temperature in the furnace.
S6, measuring the porosity of the sample, wherein the porosity of the obtained porous ceramic is 37.8 percent respectively.
Example 3:
s1, taking out 2g of slag fiber, putting the slag fiber into a die, and shearing the slag fiber under the pressure of a hydraulic press (the pressure is 10MPa), so as to obtain 2g of slag short fiber.
S2, putting the obtained slag short fibers into a beaker, adding a sodium silicate binder (taking 3 wt%), and uniformly mixing by using a spoon.
S3, putting the mixture obtained in the step 2 into a mold, and pressurizing by using a hydraulic press (pressurization is 20MPa) to obtain a circular tablet with the diameter of 20 mm.
S4, sintering the round pressed sheet obtained in the step 3 by adopting a burial method, wherein a burial medium is aluminum oxide, the sintering temperature is 1000 ℃, the sintering speed is 5 ℃/min, and the temperature is kept for 2 h.
And S5, obtaining a molded sample after the molded sample is naturally cooled to the temperature in the furnace.
S6, measuring the porosity of the sample, wherein the porosity of the obtained porous ceramic is 34.6 percent respectively.
Example 4
S1, taking out 2g of slag fiber, putting the slag fiber into a die, and shearing the slag fiber under the pressure of a hydraulic press (the pressure is 3MPa) to obtain 2g of slag short fiber.
S2, putting the obtained slag short fibers into a beaker, adding a sodium silicate binder (1 wt%), and uniformly mixing by using a spoon.
S3, putting the mixture obtained in the step 2 into a mold, and pressurizing by using a hydraulic press (pressurization of 5MPa) to obtain a circular tablet with the diameter of 20 mm.
S4, sintering the round pressed sheet obtained in the step 3 by adopting a burial method, wherein a burial medium is aluminum oxide, the sintering temperature is 1000 ℃, the sintering speed is 5 ℃/min, and the temperature is kept for 2 h.
And S5, obtaining a molded sample after the molded sample is naturally cooled to the temperature in the furnace.
S6, measuring the porosity of the sample, wherein the porosity of the obtained porous ceramic is 51.5 percent respectively.
Example 5
S1, taking out 2g of slag fiber, putting the slag fiber into a die, and shearing the slag fiber under the pressure of a hydraulic press (the pressure is 3MPa) to obtain 2g of slag short fiber.
S2, putting the obtained slag short fibers into a beaker, adding a sodium silicate binder (taking 3 wt%), and uniformly mixing by using a spoon.
S3, putting the mixture obtained in the step 2 into a mold, and pressurizing by using a hydraulic press (pressurization of 5MPa) to obtain a circular tablet with the diameter of 20 mm.
S4, sintering the round pressed sheet obtained in the step 3 by adopting a burial method, wherein a burial medium is aluminum oxide, the sintering temperature is 1000 ℃, the sintering speed is 5 ℃/min, and the temperature is kept for 2 h.
And S5, obtaining a molded sample after the molded sample is naturally cooled to the temperature in the furnace.
S6, measuring the porosity of the sample, wherein the porosity of the obtained porous ceramic is 44.6 percent respectively.
Example 6
S1, taking out 2g of slag fiber, putting the slag fiber into a die, and shearing the slag fiber under the pressure of a hydraulic press (the pressure is 3MPa) to obtain 2g of slag short fiber.
S2, putting the obtained slag short fibers into a beaker, adding a sodium silicate binder (taking 5 wt%), and uniformly mixing by using a spoon.
S3, putting the mixture obtained in the step 2 into a mold, and pressurizing by using a hydraulic press (pressurization of 5MPa) to obtain a circular tablet with the diameter of 20 mm.
S4, sintering the round pressed sheet obtained in the step 3 by adopting a burial method, wherein a burial medium is aluminum oxide, the sintering temperature is 1000 ℃, the sintering speed is 5 ℃/min, and the temperature is kept for 2 h.
And S5, obtaining a molded sample after the molded sample is naturally cooled to the temperature in the furnace.
S6, measuring the porosity of the sample, wherein the porosity of the obtained porous ceramic is 39.4 percent respectively.
In conclusion, the porous ceramic prepared by pressing the slag fiber used as the raw material to obtain the short fiber, and then performing pressure forming and sintering has high porosity and excellent performance.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (10)

1. A preparation method of slag fiber-based porous filter ceramic is characterized by comprising the following steps:
putting the slag fiber into a mould to be pressurized for one time to form slag short fiber;
uniformly mixing the slag short fibers with a binder, and putting the mixture into a die for secondary pressurization to form a pressed sheet;
and sintering the pressed sheets, preserving heat and cooling to obtain the slag fiber-based porous filtering ceramic.
2. The method of claim 1, wherein the slag fiber-based porous filter ceramic has a diameter of 2 to 7 μm, a length of millimeter or more, and an aspect ratio of 800 or more.
3. The method of preparing slag fiber-based porous filtering ceramic according to claim 1, wherein the mass ratio of the slag fiber to the binder is 100: 1 to 7.
4. The method of making slag fiber-based porous filter ceramic of claim 1, wherein the binder is sodium silicate.
5. The method of producing slag fiber-based porous filtering ceramic according to claim 1, wherein the primary pressurization pressure is 3MPa to 20 MPa.
6. The method of producing slag fiber-based porous filtering ceramic according to claim 1, wherein the secondary pressurization is performed at a pressure of 5MPa to 20 MPa.
7. The method of claim 1, wherein the sintering is performed by a burial process, and preferably, the burial medium is alumina.
8. The method of claim 7, wherein the sintering temperature is 800-1000 ℃, preferably 5-8 ℃/min, and the temperature is maintained for 2-2.5 hours.
9. Slag fiber based porous filter ceramic produced by the method of any one of claims 1 to 8.
10. Use of the slag fiber-based porous filtering ceramic according to claim 9 in the fields of industrial exhaust gas dedusting, high temperature filtration resistance and catalyst support.
CN202110539656.0A 2021-05-18 2021-05-18 Preparation method of slag fiber-based porous filtering ceramic Pending CN113277873A (en)

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