CN109180169B - Ceramic membrane support with high thermal shock resistance and preparation method thereof - Google Patents
Ceramic membrane support with high thermal shock resistance and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic membrane filters, and discloses a ceramic membrane support with high thermal shock resistance and a preparation method thereof. The ceramic membrane support body with high thermal shock resistance is prepared from fused quartz, boron nitride, a pore-forming agent and a binder; the dosage of the fused quartz and the boron nitride meets the following conditions: according to the mass percentage, the fused quartz is 90-99 percent, and the boron nitride is 1-10 percent. The method comprises the following steps: mixing and molding fused quartz, boron nitride, a pore-forming agent and a binder, and then sintering to obtain a ceramic membrane support body with high thermal shock resistance; the sintering temperature is 1000-1200 ℃. The ceramic membrane support prepared by the invention has the characteristics of high mechanical strength, large permeation flux, high thermal shock resistance, lower cost, good stability and the like.
Description
Technical Field
The invention belongs to the technical field of ceramic membrane filters, and particularly relates to a high-thermal shock resistance ceramic membrane support body for high-temperature filtration and dust removal in industries such as power plants, coal chemical industry, inorganic non-metallic materials, metallurgy and the like and a preparation method thereof.
Background
Scientists began studying ceramic filtration membranes in the 40 th 20 th century and used them for the separation of gas mixtures, and porous ceramic membranes in the 80 th 20 th century realized industrial applications in a variety of fields. High-temperature dust discharged by industries such as power plants, coal chemical industry, inorganic non-metallic materials and metallurgy pollutes the atmospheric environment and wastes heat energy, the temperature of smoke discharged by common coal-fired boilers is 500-600 ℃, and the high-temperature and acidic environment causes that filtering materials such as organic material filters and metal filters cannot work for a long time in the severe environment, so that the purification treatment of high-temperature dust-containing smoke becomes a problem which troubles the sustainable development of the industries. In the prior art, when the high-temperature flue gas is purified, the high-temperature flue gas is generally cooled and then treated by various methods. The method can not fully utilize the waste heat of the high-temperature flue gas, thereby causing the waste of a large amount of heat energy. If gas-solid separation and purification treatment can be carried out on the dust-containing flue gas at high temperature, the utilization rate of energy and resources can be improved, and environmental protection is realized; and the abrasion of dust to related equipment can be reduced, and the service life of the equipment is prolonged. Although there are many methods for high temperature dust removal, the existing cyclone dust removal, electric dust removal, filter dust removal and the like have technical defects. The ceramic membrane filter with high temperature resistance, excellent thermal stability and chemical stability is considered to be one of the most promising high-temperature dust removal technologies.
The traditional ceramic membrane is usually an asymmetric structure composed of three layers, namely a separation layer, a transition layer and a support body. The support body used as the high-temperature flue gas filtering membrane has certain mechanical strength, high permeation flux and high thermal shock resistance, and can be manufactured at low cost on the premise of ensuring excellent performance. At present, ceramic membrane filters for high-temperature filtration and dust removal in industries such as thermal power plants, coal chemical industry, inorganic non-metallic materials, metallurgy and the like are mainly ceramic fiber tubes and SiC tubes. The existing ceramic membrane support mainly has the following defects: 1. the mechanical strength and the permeation flux are difficult to be coordinated, when the flux is large, the mechanical strength is greatly reduced, and a support body with the coordination of the flux and the mechanical strength needs to be searched; 2. in the support body used for filtering high-temperature dust at present, silicon carbide belongs to a material with the best thermal shock resistance, but the silicon carbide is high in cost and difficult to burn, and the thermal shock resistance of other materials can not meet the requirement although the cost of other materials is lower than that of the silicon carbide.
Disclosure of Invention
In order to overcome the defects of low mechanical strength, poor thermal shock resistance and small permeation flux of the conventional ceramic membrane support body, the invention aims to provide a ceramic membrane support body and a preparation method thereof. The ceramic membrane support body has the characteristics of low firing temperature, excellent thermal shock resistance, large permeation flux, higher mechanical strength, acid corrosion resistance and the like. The ceramic membrane support body with high thermal shock resistance is prepared by using the fused quartz which is a low-cost raw material and adopting a liquid phase sintering mode, and the mechanical strength is higher on the premise of meeting the permeation flux, so that the fused quartz and the ceramic membrane support body are coordinated with each other.
The purpose of the invention is realized by the following technical scheme:
a ceramic membrane support with high thermal shock resistance is prepared from fused quartz, boron nitride, a pore-forming agent and a binder; the dosage of the fused quartz and the boron nitride meets the following conditions: according to the mass percentage, the fused quartz is 90-99 percent, and the boron nitride is 1-10 percent.
The pore-forming agent is organic matter, such as: starch, wood dust, carbon powder and the like, and the binder is polyvinyl alcohol.
The amount of the pore-forming agent is 15-45% of the total mass of the fused quartz and the boron nitride.
The dosage of the binder is 0.5-4% of the total mass of the fused quartz and the boron nitride.
The preparation method of the ceramic membrane support with high thermal shock resistance comprises the following steps:
and mixing and molding the fused quartz, the boron nitride, the pore-forming agent and the binder, and then sintering to obtain the ceramic membrane support with high thermal shock resistance.
The sintering temperature is 1000-1200 ℃. The sintering time is 4-9 h.
The preparation method of the ceramic membrane support with high thermal shock resistance specifically comprises the following steps:
uniformly mixing fused quartz and boron nitride to obtain a mixture; and then mixing the mixture with a pore-forming agent and a binder, forming and firing to obtain the ceramic membrane support with high thermal shock resistance.
The uniform mixing refers to uniformly mixing the fused quartz and the boron nitride in water, such as: ball milling, stirring and the like.
And the forming means drying and granulating the mixture, then performing press forming or performing filter pressing and pugging on the mixture, and then performing plastic forming to obtain a support blank body.
The ceramic membrane support is porous or hollow tabular, tubular or honeycomb. The boron nitride is hexagonal boron nitride.
The ceramic membrane support is applied to the field of high-temperature filtration and dust removal and is used as a support of a separation membrane.
According to the invention, fused quartz with a very low thermal expansion coefficient is used as aggregate, boron nitride is used as an inhibitor and a sintering aid for fused quartz crystallization, boron nitride is wrapped on the surfaces of fused quartz particles, the powder is mixed with a pore-forming agent (such as starch) and a binder PVA (polyvinyl alcohol), a green body is prepared by pressing, extruding and the like, and the green body is sintered at 1000-1200 ℃, so that the ceramic membrane support body with good thermal shock resistance, large permeation flux and composite requirements on mechanical strength is prepared.
According to the invention, boron nitride is coated on the surface of the fused quartz, so that the fused quartz is inhibited from crystallizing to generate cristobalite, and the structural damage caused by volume change due to crystal form conversion is avoided, the sintering uniformity and the high-temperature crystallization of the fused quartz are fundamentally solved, the large particles are connected with each other at the neck part, the mechanical strength of the support body is improved by liquid phase sintering, and the thermal shock resistance of the support body is improved by the fused quartz with a low expansion coefficient.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the porous ceramic membrane support body has the advantages of low sintering temperature, large permeation flux, good thermal shock resistance, high mechanical strength and the like; compared with the preparation cost of other high-temperature filtration and dust removal ceramic membrane supports, the method is simple and has low preparation cost.
The support body prepared by the invention has the bending strength of 15-35 MPa, the porosity of 30-55 vol%, the average pore diameter of 20-95 mu m and the nitrogen flux of 0.7-8.0 multiplied by 105m3·m-2·h-1·bar-1. The ceramic membrane support prepared by the invention has the characteristics of high mechanical strength, acid resistance, large permeation flux, high thermal shock resistance, lower cost, good stability and the like.
Drawings
Fig. 1 is a graph of the thermal shock resistance test of the ceramic membrane support prepared in example 7.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) The mass percentages of the fused quartz and the boron nitride are respectively 99 percent and 1 percent; respectively weighing fused quartz and boron nitride, mixing, pouring into a container filled with water which is 20% of the total mass of the fused quartz and the boron nitride, and placing a stirring paddle in the container for uniformly stirring;
(2) adding starch which is 15 percent of the total mass of the fused quartz and the boron nitride and PVA (molecular weight 205000) aqueous solution which is 40 percent of the total mass of the fused quartz and the boron nitride (the PVA aqueous solution has 8 percent of mass percentage content) into a stirrer to be uniformly stirred with the mixture of the fused quartz and the boron nitride.
(3) Drying, granulating, sieving and pressing the mixed powder;
(4) drying the support body blank until the water content is below 2%;
(5) and firing the green support body at 1200 ℃ for 9h to obtain the ceramic membrane support body.
The support prepared by the process has the bending strength of 30MPa, the average pore diameter of 25 mu m and the nitrogen flux of 0.9 multiplied by 105m3·m-2·h-1·bar-1. The ceramic membrane support prepared in this example was subjected to 30 cycles of cooling and heating, and had a flexural strength of 98.6% of that of the untreated ceramic membrane support. Therefore, the ceramic membrane support of the present embodiment has high thermal shock resistance.
Example 2
(1) The mass percentages of the fused quartz and the boron nitride are respectively 90 percent and 10 percent; respectively weighing fused quartz and boron nitride, mixing, pouring into a container filled with water which is 20% of the total mass of the fused quartz and the boron nitride, and placing a stirring paddle in the container for uniformly stirring;
(2) adding starch which is equivalent to 40 percent of the total mass of the fused quartz and the boron nitride and PVA (polyvinyl alcohol with molecular weight of 205000) aqueous solution (the PVA aqueous solution with mass percent of 8 percent) which is equivalent to 40 percent of the total mass of the fused quartz and the boron nitride into a stirrer to be uniformly stirred with the mixture of the fused quartz and the boron nitride;
(3) filter-pressing the mixed powder into mud cakes, then carrying out vacuum pugging twice, and ageing for 48 hours;
(4) forming a hollow plate-shaped support body and a porous columnar support body by extrusion molding;
(5) and firing the green support body at 1000 ℃ for 4h to obtain the ceramic membrane support body.
The support prepared by the process has the bending strength of 22MPa, the average pore diameter of 65 mu m and the nitrogen flux of 2 multiplied by 105m3·m-2·h-1·bar-1. The ceramic membrane support prepared in this example was subjected toThe flexural strength of the steel sheet after 30 cycles of cold and heat treatment was 97.5% of the flexural strength of the steel sheet without treatment. Therefore, the ceramic membrane support of the present embodiment has high thermal shock resistance.
Example 3
(1) The mass percentages of the fused quartz and the boron nitride are respectively 95 percent and 5 percent; respectively weighing fused quartz and boron nitride, mixing, pouring into a container filled with water which is 20% of the total mass of the fused quartz and the boron nitride, and placing a stirring paddle in the container for uniformly stirring;
(2) adding starch which is equal to 40 percent of the total mass of the fused quartz and the boron nitride and PVA aqueous solution which is equal to 35 percent of the total mass of the fused quartz and the boron nitride (aqueous solution with the PVA content of 8 percent by mass) into a stirrer to be uniformly stirred with the mixture of the fused quartz and the boron nitride;
(3) drying, granulating, sieving and pressing the mixed powder;
(4) drying the support body blank until the water content is below 2%;
(5) and sintering the green support body at 1130 ℃ for 7h to obtain the ceramic support body.
The support prepared by the process has the bending strength of 19MPa, the average pore diameter of 75 mu m and the nitrogen flux of 4.5 multiplied by 105m3·m-2·h-1·bar-1. The ceramic membrane support prepared in this example was subjected to 30 cycles of cooling and heating, and the flexural strength was 97.9% of the flexural strength of the untreated ceramic membrane support. Therefore, the ceramic membrane support of the present embodiment has high thermal shock resistance.
Example 4
(1) The mass percentages of the fused quartz and the boron nitride are respectively 94 percent and 6 percent; respectively weighing fused quartz and boron nitride, mixing, pouring into a container filled with water which is 20% of the total mass of the fused quartz and the boron nitride, and placing a stirring paddle in the container for uniformly stirring;
(2) adding starch which is 15 percent of the total mass of the fused quartz and the boron nitride and PVA aqueous solution which is 40 percent of the total mass of the fused quartz and the boron nitride (aqueous solution with the PVA content of 8 percent by mass) into a stirrer to be uniformly stirred with the mixture of the fused quartz and the boron nitride.
(3) And (3) press-filtering the mixed powder into mud cakes, then carrying out vacuum pugging twice, and ageing for 48 hours.
(4) Extrusion molding of hollow plate-like support and porous columnar support
(5) The green support was fired at 1170 ℃ for 8h to obtain a ceramic support.
The support prepared by the process has the bending strength of 30MPa, the average pore diameter of 25 mu m and the nitrogen flux of 0.9 multiplied by 105m3·m-2·h-1·bar-1. The ceramic membrane support prepared in this example was subjected to 30 cycles of cooling and heating cycles, and had a flexural strength of 98.1% of the flexural strength of the untreated ceramic membrane support. Therefore, the ceramic membrane support of the present embodiment has high thermal shock resistance.
Example 5
(1) The mass percentages of the fused quartz and the boron nitride are respectively 95 percent and 5 percent; respectively weighing fused quartz and boron nitride, mixing, pouring into a container filled with water which is 20% of the total mass of the fused quartz and the boron nitride, and placing a stirring paddle in the container for uniformly stirring;
(2) adding starch which is equivalent to 45 percent of the total mass of the fused quartz and the boron nitride and PVA aqueous solution which is equivalent to 40 percent of the total mass of the fused quartz and the boron nitride (aqueous solution with the PVA content of 8 percent by mass) into a stirrer to be uniformly stirred with the mixture of the fused quartz and the boron nitride.
(3) Drying, granulating, sieving and pressing the mixed powder;
(4) drying the support body blank until the water content is below 2%;
(5) and sintering the green support body at 1100 ℃ for 5h to obtain the ceramic support body.
The support prepared by the process has the bending strength of 27MPa, the average pore diameter of 95 mu m and the nitrogen flux of 8.0 multiplied by 105m3·m-2·h-1·bar-1. The ceramic membrane support prepared in this example was subjected to 30 cycles of cooling and heating cycles, and had a flexural strength of 98% of that of the untreated ceramic membrane support. Thus, it is possible to provideThe ceramic membrane support of the present embodiment has high thermal shock resistance.
Example 6
(1) The mass percentages of the fused quartz and the boron nitride are respectively 92% and 8%; respectively weighing fused quartz and boron nitride, mixing, pouring into a container filled with water which is 20% of the total mass of the fused quartz and the boron nitride, and placing a stirring paddle in the container for uniformly stirring;
(2) adding starch which is 30 percent of the total mass of the fused quartz and the boron nitride and PVA aqueous solution which is 40 percent of the total mass of the fused quartz and the boron nitride (aqueous solution with the PVA content of 8 percent by mass) into a stirrer to be uniformly stirred with the mixture of the fused quartz and the boron nitride.
(3) Filter-pressing the mixed powder into mud cakes, then carrying out vacuum pugging twice, and ageing for 48 hours;
(4) forming a hollow plate-shaped support body and a porous columnar support body by extrusion molding;
(5) and sintering the green support body at 1150 ℃ for 7.5h to obtain the ceramic support body.
The support prepared by the process has the bending strength of 26MPa, the average pore diameter of 50 mu m and the nitrogen flux of 1.5 multiplied by 105m3·m-2·h-1·bar-1. The ceramic membrane support prepared in this example was subjected to 30 cycles of cooling and heating, and the flexural strength was 97.6% of the flexural strength of the untreated ceramic membrane support. Therefore, the ceramic membrane support of the present embodiment has high thermal shock resistance.
Example 7
(1) The mass percentages of the fused quartz and the boron nitride are respectively 90 percent and 10 percent; respectively weighing fused quartz and boron nitride, mixing, pouring into a container filled with water which is 20% of the total mass of the fused quartz and the boron nitride, and placing a stirring paddle in the container for uniformly stirring;
(2) adding starch which is 16 percent of the total mass of the fused quartz and the boron nitride and PVA aqueous solution which is 15 percent of the total mass of the fused quartz and the boron nitride (aqueous solution with the PVA content of 8 percent by mass) into a stirrer to be uniformly stirred with the mixture of the fused quartz and the boron nitride;
(3) drying, granulating, sieving and pressing the mixed powder;
(4) drying the support body blank until the water content is below 2%;
(5) and sintering the green support body at 1000 ℃ for 5h to obtain the ceramic support body.
The thermal shock resistance test results of the ceramic membrane support prepared in this example are shown in fig. 1. As can be seen from FIG. 1, the flexural strength was maintained at 16.5MPa after 4 cycles of cooling and heating, and after 30 cycles of cooling and heating, the flexural strength was 16 MPa. After 30 times of cold-hot cycles, the bending strength is reduced by 0.5MPa, which shows that the material has high thermal shock resistance.
The method for measuring the thermal shock resistance comprises the following steps: firing to prepare a ceramic block with the size of 3 multiplied by 4 multiplied by 30mm, placing the ceramic block in a high-temperature electric furnace at 800 ℃ for heat preservation for 0.5h, immediately taking out the ceramic block when the heat preservation time reaches 0.5h, and placing the ceramic block in air for natural cooling. And when the temperature of the ceramic block is cooled to room temperature, opening the furnace door again, placing the ceramic block in a high-temperature electric furnace at 800 ℃ for heat preservation for 0.5h, and when the heat preservation time reaches 0.5h, immediately taking out the ceramic block and placing the ceramic block in the air for natural cooling. The experiment was repeated according to the above procedure. The thermal shock resistance of the material is characterized according to the change conditions of the bending strength of the ceramic block before and after the ceramic block is subjected to severe temperature field change.
Claims (1)
1. The application of the ceramic membrane support body with high thermal shock resistance in the field of high-temperature filtration and dust removal is characterized in that: the ceramic membrane support with high thermal shock resistance is prepared from fused quartz, boron nitride, a pore-forming agent and a binder; the dosage of the fused quartz and the boron nitride meets the following conditions: according to the mass percentage, 92% -99% of fused quartz and 1% -8% of boron nitride;
the pore-forming agent is starch, wood dust or carbon powder, and the binder is polyvinyl alcohol; the amount of the pore-forming agent is 15-45% of the total mass of the fused quartz and the boron nitride; the using amount of the binder is 0.5-4% of the total mass of the fused quartz and the boron nitride;
the preparation method of the ceramic membrane support with high thermal shock resistance comprises the following steps:
uniformly mixing fused quartz and boron nitride to obtain a mixture; then mixing the mixture with a pore-forming agent and a binder, forming and firing to obtain a ceramic membrane support body with high thermal shock resistance; the firing temperature is 1000-1200 ℃; the sintering time is 4-9 h; the uniform mixing refers to uniformly mixing the fused quartz and the boron nitride in water.
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| CN113336567B (en) * | 2021-07-08 | 2022-09-02 | 河南省高新技术实业有限公司 | Preparation method of quartz ceramic membrane support |
| CN114105671B (en) * | 2021-12-28 | 2022-11-18 | 河南省高新技术实业有限公司 | Coal gangue-quartz-based ceramic support and preparation method thereof |
| CN115321948A (en) * | 2022-08-25 | 2022-11-11 | 山西工程技术学院 | Method for preparing ceramic filtering membrane by using wulan thea-crystal stone |
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| CN101628821A (en) * | 2009-07-22 | 2010-01-20 | 河北理工大学 | Composite material supporter and preparation method thereof |
| US20140147664A1 (en) * | 2012-11-29 | 2014-05-29 | Corning Incorporated | Fused Silica Based Cellular Structures |
| CN106186708A (en) * | 2016-07-12 | 2016-12-07 | 河南维时汉金科技有限公司 | The preparation method of crystallite vitreous silica low-pressure casting lift tube |
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| CN101628821A (en) * | 2009-07-22 | 2010-01-20 | 河北理工大学 | Composite material supporter and preparation method thereof |
| US20140147664A1 (en) * | 2012-11-29 | 2014-05-29 | Corning Incorporated | Fused Silica Based Cellular Structures |
| CN106186708A (en) * | 2016-07-12 | 2016-12-07 | 河南维时汉金科技有限公司 | The preparation method of crystallite vitreous silica low-pressure casting lift tube |
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