CN115504807B - Method for preparing porous ceramic with uniform pore diameter - Google Patents

Method for preparing porous ceramic with uniform pore diameter Download PDF

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CN115504807B
CN115504807B CN202211194613.4A CN202211194613A CN115504807B CN 115504807 B CN115504807 B CN 115504807B CN 202211194613 A CN202211194613 A CN 202211194613A CN 115504807 B CN115504807 B CN 115504807B
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porous ceramic
potassium feldspar
pore diameter
bottom ash
uniform pore
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CN115504807A (en
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蒲锡鹏
黄民浩
赵凌峰
王菁
李景凯
张大凤
刘君昌
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Liaocheng University
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Abstract

The invention discloses a method for preparing potassium feldspar water washing waste with uniform pore diameter and garbage incinerator bottom ash-based porous ceramic by taking cotton fibers as a foaming agent, which comprises the following steps: mixing and grinding waste incinerator bottom ash, potassium feldspar tailings and cotton fibers, and drying and sieving to obtain a porous ceramic powder raw material; uniformly spreading the porous ceramic powder raw material into a crucible with air permeability on the outer wall and the bottom for compaction, heating to a foaming temperature in nitrogen atmosphere at high temperature, introducing a certain amount of air in the heat preservation process, continuously introducing nitrogen after heat preservation is finished, and cooling along with a furnace to obtain the porous ceramic with uniform pore diameter; the method has simple technical process and low production cost, can enable the secondary use of the potassium feldspar water washing waste and the waste incineration bottom ash, is beneficial to environmental protection, and can prepare the porous ceramic with uniform pore diameter without special treatment means.

Description

Method for preparing porous ceramic with uniform pore diameter
Technical Field
The invention relates to the technical field of porous ceramics, in particular to a method for preparing potassium feldspar water washing waste materials with uniform pore diameters and waste incineration furnace bottom ash-based porous ceramics by taking cotton fibers as a foaming agent.
Background
At present, the urban garbage treatment modes in China mainly comprise incineration, sanitary landfill and high-temperature composting, wherein the incineration can kill germs in the garbage, saves land and has wide use cost. However, the bottom ash after the garbage incineration is accumulated in a large amount, and the disposal is urgently needed. Because the bottom ash of the garbage incinerator has silicon, aluminum and calcium elements, the elements required by ceramics are satisfied. The porous ceramic material has the characteristics of high temperature resistance, corrosion resistance, large specific surface, low density, high porosity and the like, is widely applied to the fields of building materials such as heat insulation materials, sound insulation materials and the like, and has great market prospect.
The uniformity of pore size greatly affects the performance of porous ceramics. The uniform pore size can enable all parts of the porous ceramic to have the same physical properties, so that the stability of the porous ceramic can be improved. When the porous ceramic with uniform pores bears external force, the uniformly distributed air holes can balance forces from all directions, so that the stress of each part of the porous ceramic is uniform, and the compressive strength is improved. The porosity of the porous ceramic can be improved to a certain extent by uniformly distributing the air holes, and the heat conductivity of the air is lower than that of the porous ceramic, so that the whole heat conductivity of the porous ceramic is greatly reduced, and the porous ceramic is favorable for obtaining a high heat preservation effect.
In order to obtain a porous ceramic material with uniform pore diameter, the prior invention patent CN202010190704.5 discloses a porous ceramic with uniformly distributed sub-micropores prepared by using inorganic co-molten salt and a preparation method thereof. The preparation method comprises the steps of dispersing inorganic co-molten salt and ceramic powder into a solvent to obtain mixed slurry, and drying and forming the slurry to obtain a porous ceramic biscuit; and (3) preserving the temperature of the obtained porous ceramic biscuit at 1300-1850 ℃ for 1-3 hours, and forming porous ceramic with uniformly distributed micropores after melting and volatilizing the co-melted salt. However, the size and distribution of the pores obtained by the method depend on the dispersion condition of the eutectic salt, the dispersion non-uniformity of the eutectic salt can lead to the dispersion of the pores to be different in size and uneven in dispersion, and the condition of pore connection can also occur at the place with large concentration of the eutectic salt, so that the quality of the porous ceramic is reduced.
Chinese patent No. CN201911411235.9 discloses a method for sintering porous ceramic by mixing waste ceramic with waste incineration fly ash, which uses waste ceramic powder, cement, clay, feldspar and fly ash as raw materials, and adds foaming slurry to stir and solidify, and the porous ceramic material is prepared by sintering. The sintered porous ceramic product has low leaching toxicity, realizes solidification of heavy metal, and has the characteristics of low normal temperature heat conductivity coefficient, low volume density, high porosity, small volume change after sintering, high compressive strength, low cost, simple process and capability of realizing comprehensive utilization of resources. However, the method has the defects of complicated technical process and overlong ceramic processing and preparation period, needs to stir the foaming agent, water and the foam stabilizer uniformly, prepares foam by mechanical high-speed stirring, needs to naturally dry 12-h after the foam is cast and molded, dries 6-10 h at 60-90 ℃, and keeps the temperature at 950-1100 ℃ for 1-3 hours to prepare the porous ceramic, so that the porous ceramic consumes too long time in industrial production.
Based on the above problems, the present invention provides a method for washing waste materials with potassium feldspar water and waste incineration bottom ash-based porous ceramics with highly uniform pore diameters.
Disclosure of Invention
In order to solve the technical defects, the technical scheme adopted by the invention is that the method for preparing the potassium feldspar water washing waste material with uniform pore diameter and the garbage incinerator bottom ash-based porous ceramic by taking cotton fiber as a foaming agent comprises the following steps:
(1) Pretreatment of potassium feldspar water washing ore and bottom ash: respectively washing potassium feldspar with water and drying waste incinerator bottom ash, removing water, and primarily crushing large particles;
(2) Uniformly mixing the powder materials: uniformly mixing pretreated potassium feldspar water washing ore and waste incineration bottom ash powder in proportion, putting the mixture into a ball milling tank, adding a certain amount of cotton fibers as a foaming agent, adding a certain amount of water, and putting the mixture into a ball mill for ball milling; putting the ball-milled slurry into a baking oven for drying, and grinding to obtain porous ceramic raw material mixed powder;
(3) Filling the mixed powder into a mould, compacting, heating to a foaming temperature in a nitrogen atmosphere, and introducing a certain amount of air to foam; after heat preservation for a certain time, cooling along with the furnace in the nitrogen atmosphere to obtain the porous ceramic with high pore diameter uniformity.
Since the natural chemical structural components of cotton fibers mainly include primary cellulose, fat, pectin, wax, ash, and the like. Wherein, the content of cellulose and wax account for 95 percent wt percent. The cotton fiber mainly consists of three hierarchical structures of an epidermal layer, a primary layer and a secondary epidermal layer. Cotton fiber is a natural material, is composed of many fine microfibres, and is easily separated, compared to other commonly used foaming agents such as coke, charcoal, activated carbon, coal dust, graphite, etc. After ball milling, the microfibrils of the cotton fibers can be uniformly dispersed in the raw materials, and the fiber morphology of the microfibrils enables the biscuit to have a very fluffy and uniform porous structure, so that the subsequent formation of uniform pore diameters is facilitated.
In order to avoid premature oxidation of the cotton fibers, they are kept under nitrogen protection. At temperatures above 120 ℃, the internal fat, pectin and waxy components will decompose and carbonize: on one hand, the decomposition can shrink the volume of the fiber, so that the air hole channel in the blank structure is more unobstructed; on the other hand, the newly decomposed carbon particles have higher reactivity than other carbon-containing foaming agents, and are favorable for the subsequent oxidation foaming process.
Preferably, in the step (2), the mixing ratio of the pretreated potassium feldspar water-washed ore to the garbage incineration is 2.5:1-1:1, and the content of the foaming agent is 1.0-2.0 wt%; the ball milling time of the prepared powder in the ball mill is 2-6 hours.
Preferably, in the step (3), the temperature rising speed in the high-temperature foaming process is 5-10 ℃/min, the foaming temperature is 1120-1135 ℃, and the air quantity is [ the carbon content (g) of the foaming agent (1-9.15) ] (liter) after the foaming temperature is reached; the heat preservation time after a certain amount of air is introduced is 10-60 min.
Compared with the prior art, the invention has the following beneficial effects:
1. the raw materials used in the experiment are solid wastes except the foaming agent, so that the production cost is greatly reduced, the environment is indirectly protected, and the environmental pollution is reduced;
2. the foaming agent adopted by the invention is cotton fiber, the cotton fiber is convenient to obtain, is easy to obtain, has low production cost, and has the advantages of uniform dispersion, high reaction activity and the like;
3. the invention can only obtain the structure with uniform aperture height, and can control the aperture size by controlling the amount of foaming agent and air inlet, thereby adapting to different requirements;
4. the invention has simple production process, no need of pressing into embryo, industrialized production, simple temperature raising program, safety and reliability and no safety risk.
Drawings
FIG. 1 is a vertical cross-sectional view of the porous ceramic prepared in example 1;
FIG. 2 is a vertical cross-sectional view of the porous ceramic prepared in example 2.
Detailed Description
In order that the manner in which the above recited features, objects and advantages of the present invention are obtained will become readily apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. Based on the examples in the embodiments, those skilled in the art can obtain other examples without making any inventive effort, which fall within the scope of the invention. The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
Embodiment one:
(1) Prefabrication and batching of raw materials: 33 g of garbage incinerator bottom ash, 66 g of potash feldspar water-washed ore waste residue and 1 g of cotton fiber accounting for 66 wt%,33 wt% and 1 wt% of the total mass of the sample are added, and the mixture is uniformly ground at a high speed in a ball mill, wherein the grinding medium is distilled water; drying the ground slurry at 90 ℃ for 4 h, and sieving the ground slurry with a 90-mesh sieve to obtain the porous ceramic powder raw material.
(2) Foaming procedure and cooling: spreading the porous ceramic powder raw material into a crucible with air permeability on the outer wall and the bottom, scraping, compacting, heating to 1150 ℃ at a heating rate of 5 ℃/min in nitrogen atmosphere, keeping the temperature for 45 min, introducing air 200 and mL during the heat preservation, keeping the nitrogen atmosphere after the heat preservation, and obtaining the porous ceramic with uniform air holes. As shown in the first graph, the porous ceramic prepared in the first example has the characteristics of uniform air holes and high porosity.
Embodiment two:
(1) Prefabrication and batching of raw materials: 49.335 g of garbage incinerator bottom ash, 49.335 g of potassium feldspar water-washed ore waste residue, 1.33 g of cotton fiber accounting for 49.335 wt%,49.335 wt% and 1.33 wt% of the total mass of the sample are added, and the mixture is uniformly ground in a ball mill at a high speed, wherein the grinding medium is distilled water. Drying the ground slurry at 90 ℃ for 4 h, and sieving the ground slurry with a 90-mesh sieve to obtain the porous ceramic powder raw material.
(2) Foaming procedure and cooling: spreading the porous ceramic powder raw material into a crucible with air permeability on the outer wall and the bottom, scraping, compacting, heating to 1150 ℃ at a heating rate of 5 ℃/min in nitrogen atmosphere, keeping the temperature for 30 min, introducing air 500 and mL during the heat preservation, keeping the nitrogen atmosphere after the heat preservation, and obtaining the porous ceramic with uniform air holes. As shown in the second graph, the porous ceramic prepared in the second example has the characteristics of uniform air holes and high porosity.
Embodiment III:
(1) Prefabrication and batching of raw materials: 49.1 g of garbage incinerator bottom ash, 49.1 g of potassium feldspar water-washed ore waste residue and 1.8 g of cotton fiber are added, the weight of the waste incinerator bottom ash is 49.1 wt%,49.1 wt% and 1.8 wt% of the total mass of a sample are respectively calculated, the waste incinerator bottom ash is uniformly ground in a ball mill at a high speed, and a grinding medium is distilled water. Drying the ground slurry at 90 ℃ for 4 h, and sieving the ground slurry with a 90-mesh sieve to obtain the porous ceramic powder raw material.
(2) Foaming procedure and cooling: spreading the porous ceramic powder raw material into a crucible with air permeability on the outer wall and the bottom, scraping, compacting, heating to 1165 ℃ at a heating rate of 5 ℃/min in nitrogen atmosphere, keeping the temperature for 45 min, introducing air 100 mL during the heat preservation, keeping the nitrogen atmosphere after the heat preservation, and obtaining the porous ceramic with uniform pore diameter.
Embodiment four:
(1) Prefabrication and batching of raw materials: 49 g of garbage incinerator bottom ash, 49 g of potassium feldspar water-washed ore waste residue, 2.0 g of cotton fiber accounting for 49wt%,49wt% and 2.0 wt% of the total mass of the sample are added, and the mixture is uniformly ground at a high speed in a ball mill, wherein the grinding medium is distilled water. Drying the ground slurry at 90 ℃ for 4 h, and sieving the ground slurry with a 90-mesh sieve to obtain the porous ceramic powder raw material.
(2) Foaming procedure and cooling: spreading the porous ceramic powder raw material into a crucible with air permeability on the outer wall and the bottom, scraping, compacting, heating to 1120 ℃ at a heating rate of 5 ℃/min in nitrogen atmosphere, keeping the temperature for 45 min, introducing air 500 and mL during the heat preservation, and keeping the nitrogen atmosphere after the heat preservation, thus obtaining the porous ceramic with uniform pore diameter.
The patent invention is subsidized by projects on the foundation of nature science in Shandong province (ZR 2021ME 046) and projects on the national development planning policy guidance class (social issuing field) (2022 YDSF 89).
The embodiments of the present invention have been described in detail with reference to the drawings, but the present invention is not limited thereto, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.

Claims (1)

1. A method for preparing porous ceramic with uniform pore diameter is characterized by comprising the following steps:
(1) Pretreatment of potassium feldspar water washing ore and bottom ash: respectively washing potassium feldspar with water and drying waste incinerator bottom ash, removing water, and primarily crushing large particles;
(2) Uniformly mixing the powder materials: uniformly mixing pretreated potassium feldspar water washing ore and waste incineration bottom ash powder in proportion, putting the mixture into a ball milling tank, adding a certain amount of cotton fibers as a foaming agent, adding a certain amount of water, and putting the mixture into a ball mill for ball milling; putting the ball-milled slurry into a baking oven for drying, and grinding to obtain porous ceramic raw material mixed powder; the mixing ratio of the pretreated potassium feldspar water washing ore to the garbage incineration is 2.5:1-1:1, the content of cotton fibers is 1.0-2.0 wt%, and the ball milling time of the raw materials in a ball mill is 2-6 hours;
(3) Filling the mixed powder into a mould, compacting, heating to a foaming temperature in a nitrogen atmosphere, and introducing a certain amount of air to foam; after heat preservation for a certain time, cooling along with the furnace in the nitrogen atmosphere to obtain porous ceramic with uniform pore diameter; in the high-temperature foaming process, the heating speed is 5-10 ℃/min, the foaming temperature is 1120-1135 ℃, and the air volume is [ the carbon content (g) of the foaming agent (1-8.15) ] (liter) after the foaming temperature is reached; the heat preservation time after a certain amount of air is introduced is 10-60 min.
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Publication number Priority date Publication date Assignee Title
CN101417215A (en) * 2008-11-24 2009-04-29 伍协 Ordered porous ceramic film and preparation method thereof
CN101597178A (en) * 2009-07-03 2009-12-09 陕西科技大学 A kind of method of utilizing the fly-ash Preparation foamed ceramic insulation board
CN108467258A (en) * 2018-05-25 2018-08-31 北方民族大学 A kind of perforation stomata porous ceramics standby using coal ash for manufacturing and preparation method thereof
CN113788704A (en) * 2021-11-01 2021-12-14 山东瀚实环保设备有限公司 Preparation method of porous ceramic with gradient pore structure
CN113968722A (en) * 2021-11-01 2022-01-25 山东瀚实环保设备有限公司 Method for preparing porous ceramic by using potassium feldspar washing waste

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417215A (en) * 2008-11-24 2009-04-29 伍协 Ordered porous ceramic film and preparation method thereof
CN101597178A (en) * 2009-07-03 2009-12-09 陕西科技大学 A kind of method of utilizing the fly-ash Preparation foamed ceramic insulation board
CN108467258A (en) * 2018-05-25 2018-08-31 北方民族大学 A kind of perforation stomata porous ceramics standby using coal ash for manufacturing and preparation method thereof
CN113788704A (en) * 2021-11-01 2021-12-14 山东瀚实环保设备有限公司 Preparation method of porous ceramic with gradient pore structure
CN113968722A (en) * 2021-11-01 2022-01-25 山东瀚实环保设备有限公司 Method for preparing porous ceramic by using potassium feldspar washing waste

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