CN108910902B - Method for synthesizing tobermorite composite heat-insulating material from high-alumina fly ash - Google Patents
Method for synthesizing tobermorite composite heat-insulating material from high-alumina fly ash Download PDFInfo
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Abstract
The invention relates to a method for synthesizing tobermorite composite heat-insulating fireproof material by using high-alumina fly ash, belonging to the field of inorganic heat-insulating materials. The method comprises the steps of taking high-alumina fly ash as a main raw material, mixing the high-alumina fly ash with calcium oxide or calcium hydroxide, grinding the mixture, adding a trace amount of additive, uniformly mixing the two raw materials with water, pulping, performing dynamic hydrothermal synthesis reaction, and sequentially filtering and drying the mixture after the reaction to obtain the mullite and tobermorite composite heat-insulating fireproof material. The main raw material of the high-alumina fly ash is solid waste obtained after high-alumina coal is combusted in a pulverized coal furnace of a power plant; the invention greatly reduces the production cost of the composite material, has wide raw material sources, and meanwhile, the method for preparing the mullite and tobermorite composite heat-insulating fireproof material is simple, has short reaction time, can absorb solid wastes generated by a thermal power plant in a large scale, and is suitable for industrialized popularization.
Description
Technical Field
The invention relates to a method for synthesizing tobermorite composite heat-insulating material by using high-alumina fly ash, in particular to a method for hydrothermally synthesizing mullite and tobermorite type composite heat-insulating fireproof plate by using high-alumina fly ash, belonging to the field of inorganic heat-insulating materials. The fireproof door core board is mainly used in the fields of fireproof door core boards, ship compartment boards, steel structure heat preservation and fire prevention, building outer wall fireproof heat preservation, building inner flue air pipes, electrolytic bath heat preservation and insulation boards and the like.
Background
4 billions of tons of fly ash are discharged from thermal power plants in China every year, and the transportation and mass accumulation of high-alumina fly ash cause serious problems of land occupation and environmental pollution, easily cause dust pollution, cause the problem that heavy metal in underground water exceeds the standard, and the like. The high-alumina fly ash is generally rich in alumina, the alumina content of the fly ash after combustion in most coal fields in the inner Mongolia autonomous region is up to more than 40%, and particularly in the middle and western regions of the inner Mongolia, because of special geological background, several large coal fields in the region are rich in alumina. Taking a quasi-Geer coal field as an example, the coal storage capacity of the coal field is up to 260 hundred million tons, the average content of alumina in the fly ash formed after the coal is combusted is up to 48-52 percent, which is equivalent to the content of alumina in medium-grade bauxite, the coal ash is a fly ash type with the highest known alumina content in the world, and the potential storage capacity of the fly ash is up to 70-80 hundred million tons. The high-alumina fly ash has the characteristics of low density, high alumina content and abundant reserves. The Ore-Doss basin late ancient coal bed and gangue are rich in minerals such as boehmite, kaolinite and the like, the content of alumina in the fly ash generated after combustion is up to 50 percent, and the content of the alumina in the fly ash is equivalent to that in medium-grade bauxite, so the coal ash is a valuable alumina production raw material. According to statistics, the potential storage amount of the high-alumina fly ash in the midwest region of inner Mongolia is up to 150 hundred million tons. The comprehensive development and utilization of the aluminum silicon elements in the high-alumina fly ash resources are beneficial to the protection and development of the local environment, can improve the economic value of the high-alumina fly ash, and has a strategic and important circular economy industry.
The tobermorite is synthesized by generally needing a calcium raw material and a silicon raw material, and the heat preservation time is different from 4 hours to 28 days under the hydrothermal condition of 80-200 ℃. The calcareous raw materials mainly comprise lime or carbide slag, and the siliceous raw materials mainly comprise quartz, silica fume, silica gel, cement, kaolin, fly ash and the like. The main chemical reactions that take place are: 5CaO +6SiO2+5H2O→Ca5Si6O16(OH)2·4H2O。
Tobei mullite is the main mineral component of calcium silicate heat-insulating material, the use temperature of the heat-insulating material formed by the Tobei mullite can reach 650 ℃, and the Tobei mullite has the advantages of small volume weight, high-temperature thermal stability, low heat conductivity coefficient and the like, so the Tobei mullite is widely used as the main raw material of light heat-insulating fireproof material. At present, the preparation method of tobermorite is mainly a hydrothermal synthesis method, and the method is to use a calcareous raw material (mainly providing CaO) and a siliceous raw material (mainly providing SiO)2) Mixing the materials according to a certain proportion, placing the mixture into a high-pressure reaction kettle for reaction to obtain tobermorite, adding an additive and reinforcing fibers, and carrying out compression molding and drying to obtain the tobermorite type calcium silicate heat-insulating material. Most of siliceous raw materials adopted in the method are solid such as quartz sand with perfect crystallization or expensive white carbon black and the likeThe material, the time required by the reaction process is long, and the reaction temperature is high. Therefore, the method for producing tobermorite in the prior art has the defects of high production cost and long production time. How to find a siliceous raw material and a calcareous raw material which are low in cost and sufficient in market supply and can shorten the production time of tobermorite is a problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the problems of environmental pollution and resource waste of the existing high-alumina fly ash, and provides a method for synthesizing tobermorite composite heat-insulating material by using high-alumina fly ash.
The purpose of the invention is realized by the technical scheme.
A method for synthesizing tobermorite composite heat-insulating material by using high-alumina fly ash comprises the following steps:
step one, uniformly mixing high-alumina fly ash and a calcareous raw material, then adding a trace additive with the total mass not more than 3%, and grinding to be below 0.12mm to obtain a mixed raw material; the sum of the mass of the high-alumina fly ash and the calcium raw material is the total mass, and the mass of the high-alumina fly ash is 70-85% of the total mass; the mass of the calcareous raw material is 15-30% of the total mass;
and step two, mixing the mixed raw material obtained in the step one with water according to the liquid-solid mass ratio of 5-40, performing dynamic hydrothermal synthesis reaction after uniform pulping, and then sequentially performing filtration, washing and drying treatment to obtain the composite heat-insulating fireproof material with the main crystal phase of mullite and tobermorite.
The source of the raw material high-alumina fly ash used in the present invention is not limited, and may be, for example, solid waste obtained by burning high-alumina coal in a pulverized coal furnace of a power plant. In one embodiment, fly ash having an alumina content greater than 40% as described in the patent publication CN 102249253B is used; particularly, the mineral component of the high-alumina fly ash is mainly mullite (3 Al)2O3·2SiO2) The mass content is more than 50 percent, and in addition, the composition also comprisesWith a small amount of corundum (Al)2O3) Less than 10% of quartz (SiO)2) Less than 5%, and other mineral components and amorphous glass phase > 30%.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the high-alumina fly ash contains 40-50% of alumina, 35-45% of silicon oxide, 2-6% of calcium oxide, 1-4% of ferric oxide and less than 1% of sodium oxide.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the calcareous raw material can be one or more of quick lime, lime milk, chemically pure calcium oxide and chemically pure calcium hydroxide.
The inventor finds that the molar ratio of calcium oxide to silicon oxide in tobermorite is 5:6, the crystallization reaction temperature is 140-.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the trace additive has the function of standardizing the crystal growth direction in the crystal synthesis process so as to synthesize the qualified whiskers with the required long-jing ratio, and can be one or more of aluminum sulfate, sodium sulfate, barium sulfate, calcium sulfate, barium chloride, aluminum chloride and aluminum nitrate.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the dynamic hydrothermal synthesis reaction process in the control step 2) is to carry out multiple segmented temperature rise from room temperature, and finally the temperature is raised to 160-230 ℃, and the temperature is the final reaction temperature, and the final reaction time is 2-8 h.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the temperature rise in the reaction process in the step 2) is segmented temperature rise: if the final reaction temperature is not more than 180 ℃, keeping the temperature at 90-100 ℃ for 60min, keeping the temperature at 150 ℃ for 30min, and keeping the final reaction temperature for 2-8 h; if the final reaction temperature is higher than 180 ℃, keeping the temperature at 90-100 ℃ for 60min, keeping the temperature at 150 ℃ for 30min, keeping the temperature at 180 ℃ for 20min, and keeping the final reaction temperature for 2-8 h; wherein the stirring speed is 100-400rpm in the temperature rising process; the stirring speed during the heat preservation process is 100-.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the temperature rise rate of the sectional temperature rise is 1-3 ℃/min.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the reaction pressure in the dynamic hydrothermal synthesis reaction in the step 2) is controlled to be 0.61-2.80 MPa.
In the method for synthesizing the mullite and tobermorite composite heat-insulating fireproof material by using the high-alumina fly ash, the drying temperature in the step 2) is controlled to be 90-100 ℃, and the drying time is controlled to be 4-16 h.
Advantageous effects
1. High-alumina fly ash is used as a main raw material. Precious industrial resources such as high-grade limestone ore, quartz ore, bauxite and the like do not need to be consumed, and the raw materials are wide in source and low in price; on the other hand, the coal price of the high-alumina fly ash production place is lower than that of the bauxite production place; therefore, the production cost of independently synthesizing the mullite and the tobermorite can be reduced from the consideration of the raw material cost and the calcination cost.
2. In the traditional tobermorite synthesis process, as the raw material systems of quicklime, quartz sand and the like are adopted, the crystallization process is longer, the hydrothermal synthesis time in a high-pressure reaction kettle is longer, generally 8-16 hours are needed, and the synthesis method of the mullite and tobermorite composite material provided by the invention only needs 2-8 hours, so that the production efficiency can be greatly improved, and the unit production cost can be reduced.
3. The preparation method of the mullite and tobermorite composite material has the advantages of wide source of raw materials, low cost, simple preparation process, easy operation, low energy consumption, no three-waste discharge and good popularization and application prospect.
Drawings
FIG. 1 is an XRD spectrum of the mullite and tobermorite composite heat-insulating fireproof material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The high-alumina fly ash adopted in the embodiment is taken from a power plant in the area called and Haote in inner Mongolia, and the quick lime is taken from the clear river county in the city called and Haote in inner Mongolia, and the chemical compositions of the quick lime are shown in Table 1.
TABLE 1 chemical composition of high alumina fly ash and quicklime
The mullite and tobermorite type composite heat-insulating fireproof material of the embodiment is prepared by mixing 80kg of the high-alumina fly ash and 20kg of the quick lime, then 0.5kg of aluminum chloride, 0.3kg of aluminum sulfate and 0.7kg of barium chloride are added, the mixture is milled by a ball mill until all the particle sizes are less than 0.12mm, then 3045kg of water is added according to the liquid-solid ratio of 30 and is uniformly mixed, and then the mixture is put into a high-pressure reaction kettle, controlling the reaction temperature to be 200 ℃, the reaction pressure to be 1.58MPa, keeping the temperature of 90-100 ℃ for 60min, keeping the temperature of 150 ℃ for 30min, keeping the temperature of 180 ℃ for 20min, keeping the temperature of 200 ℃ for reaction for 5.0h, wherein the stirring speed in the temperature rise process is 300rpm, the stirring speed in the temperature rise process is 180rpm, the temperature rise rate is 3 ℃/min, cooling the product to 90 ℃ after the reaction is finished, and then filtering the reaction product, and drying the obtained filter cake at the temperature of 95 ℃ for 8.0h to obtain the mullite and tobermorite composite material.
The test shows that:
1) the water content of the obtained mullite and tobermorite composite material is 4.2 percent by mass, and the density of the obtained mullite and tobermorite composite material is 304kg/m3The thermal conductivity coefficient is 0.069W/(m.K), the compressive strength is 1.24MPa, and the flexural strength is 0.57 MPa.
2) As shown in fig. 1, we can know in the X-ray diffraction pattern that: the product obtained after drying is the mullite and tobermorite composite material.
Example 2
The high-alumina fly ash used in this example was obtained from a power plant of rubus, japan, shanxi province, and the quicklime was obtained from a lime plant of rubus, shanxi province, and the chemical composition thereof is shown in table 2.
TABLE 2 chemical compositions of high alumina fly ash and quicklime
The mullite and tobermorite type composite heat-insulating fireproof material of the embodiment is prepared by mixing 85kg of the high-alumina fly ash and 15kg of the quick lime, then 0.1kg of aluminum nitrate, 0.4kg of barium sulfate and 0.7kg of sodium sulfate are added, the mixture is milled by a ball mill until all the particle sizes are less than 0.08mm, then 1821.6kg of water is added according to the liquid-solid ratio of 18 and is evenly mixed and then is put into a high-pressure reaction kettle, controlling the reaction temperature to be 190 ℃, the reaction pressure to be 1.27MPa, keeping the temperature of 90-100 ℃ for 60min, keeping the temperature of 150 ℃ for 30min, keeping the temperature of 180 ℃ for 20min, keeping the temperature of 190 ℃ for 7.0h, wherein the stirring speed in the temperature rise process is 350rpm, the stirring speed in the temperature rise process is 150rpm, the temperature rise rate is 2 ℃/min, cooling the product to 90 ℃ after the reaction is finished, and then filtering the reaction product, and drying the obtained filter cake at the temperature of 95 ℃ for 12.0h to obtain the mullite and tobermorite composite material.
The test shows that:
the test shows that: the water content of the obtained mullite and tobermorite composite material is less than 3.4 percent by mass, and the density is 365kg/m3The thermal conductivity coefficient is 0.074W/(m.K), the compressive strength is 1.47MPa, and the flexural strength is 0.68 MPa.
The X-ray diffraction test was carried out thereon to obtain the same results as in example 1.
Example 3
The high-alumina fly ash used in this example was obtained from a power plant of Shuozhou, Shanxi province, and the chemically pure lime was obtained from a reagent factory of east China, Tianjin, and the chemical composition thereof is shown in Table 3.
TABLE 3 chemical composition of high alumina fly ash and quicklime
The mullite and tobermorite type composite heat-insulating fireproof material of the embodiment is prepared by mixing 89kg of the high-alumina fly ash and 11kg of the quick lime, then 0.8kg of barium chloride and 0.4kg of aluminum chloride are added, the mixture is milled by a ball mill until all the particle sizes are less than 0.10mm, then 2530kg of water is added according to the liquid-solid ratio of 25 and is uniformly mixed, and then the mixture is put into a high-pressure reaction kettle, controlling the reaction temperature to be 210 ℃, the reaction pressure to be 1.93MPa, keeping the temperature of 90-100 ℃ for 60min, keeping the temperature of 150 ℃ for 30min, keeping the temperature of 180 ℃ for 20min, keeping the temperature of 210 ℃ for 7.0h, wherein the stirring speed in the heating process is 320rpm, the stirring speed in the heat preservation process is 140rpm, the heating rate is 2 ℃/min, cooling the product to 90 ℃ after the reaction is finished, and then filtering the reaction product, and drying the obtained filter cake at the temperature of 95 ℃ for 16.0h to obtain the mullite and tobermorite composite material.
Tests show that:
the test shows that: the water content of the obtained mullite and tobermorite composite material is less than 2.8 percent by mass, and the density is 287kg/m3The thermal conductivity coefficient is 0.065W/(m.K), the compressive strength is 1.04MPa, and the flexural strength is 0.43MPa。
The X-ray diffraction test was carried out thereon to obtain the same results as in example 1.
Example 4
The high-alumina fly ash adopted in the embodiment is taken from a power plant in the area called and Haote in inner Mongolia, and the quick lime is taken from the clear river county in the city called and Haote in inner Mongolia, and the specific components are the same as those in the embodiment 1.
The mullite and tobermorite composite heat-insulating fireproof material of the embodiment is prepared by mixing 75kg of the high-alumina fly ash and 25kg of the quick lime, then 0.6kg of aluminum sulfate, 0.7kg of calcium sulfate and 0.4kg of barium chloride are added, the mixture is milled by a ball mill until all the particle sizes are less than 0.14mm, then 2440.8kg of water is added according to the liquid-solid ratio of 24 and is evenly mixed and then is put into a high-pressure reaction kettle, controlling the reaction temperature to be 175 ℃, the reaction pressure to be 0.91MPa, keeping the temperature of 90-100 ℃ for 60min, keeping the temperature of 150 ℃ for 30min, keeping the temperature of 175 ℃ for reaction for 20.0h, wherein the stirring speed in the heating process is 300rpm, the stirring speed in the heat preservation process is 160rpm, the heating rate is 1 ℃/min, cooling the product to 90 ℃ after the reaction is finished, and then filtering the reaction product, and drying the obtained filter cake at the temperature of 95 ℃ for 10.0h to obtain the mullite and tobermorite composite material.
The test shows that:
1) the water content of the obtained mullite and tobermorite composite material is 4.3 percent by mass, and the density is 342kg/m3The thermal conductivity coefficient is 0.075W/(m.K), the compressive strength is 1.07MPa, and the flexural strength is 0.49 MPa.
2) As shown in fig. 1, we can know in the X-ray diffraction pattern: the product obtained after drying is the mullite and tobermorite composite material.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
The above detailed description is further intended to illustrate the objects, technical solutions and advantages of the present invention, and it should be understood that the above detailed description is only an example of the present invention and should not be used to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A method for synthesizing tobermorite composite heat-insulating material by using high-alumina fly ash is characterized by comprising the following steps: the method comprises the following steps:
step one, uniformly mixing high-alumina fly ash and a calcareous raw material, then adding a trace additive with the total mass not more than 3%, and grinding to be below 0.12mm to obtain a mixed raw material; the sum of the mass of the high-alumina fly ash and the mass of the calcareous raw materials is 70-85% of the total mass; the mass of the calcareous raw material is 15-30% of the total mass;
step two, mixing the mixed raw material obtained in the step one with water according to the liquid-solid mass ratio of 5-40, performing dynamic hydrothermal synthesis reaction after uniform pulping, and then sequentially performing filtration and drying treatment to obtain the composite heat-insulating fireproof material with the main crystal phase of mullite and tobermorite;
the micro additive is one or more of aluminum sulfate, sodium sulfate, barium sulfate, calcium sulfate, barium chloride, aluminum chloride and aluminum nitrate;
step two, the dynamic hydrothermal synthesis reaction process is as follows: heating from room temperature for multiple times in sections, and finally heating to 160-230 ℃, wherein the temperature is the final reaction temperature, and the final reaction time at the final reaction temperature is 2-8 h; the reaction pressure in the dynamic hydrothermal synthesis reaction is 0.61-2.80 MPa;
the high-alumina fly ash is fly ash with the content of alumina more than 40 percent.
2. The method for synthesizing tobermorite composite thermal insulation material by using high-alumina fly ash as claimed in claim 1, is characterized in that: the calcareous raw material is one or more of quicklime, lime milk, chemically pure calcium oxide and chemically pure calcium hydroxide.
3. The method for synthesizing tobermorite composite thermal insulation material by using high-alumina fly ash as claimed in claim 1, is characterized in that: the segmented temperature rise method comprises the following steps: if the final reaction temperature is not more than 180 ℃, preserving heat for 60min at 90-100 ℃, preserving heat for 30min at 150 ℃, and preserving heat for 2-8h at the final reaction temperature; if the final reaction temperature is higher than 180 ℃, keeping the temperature of 90-100 ℃ for 60min, keeping the temperature of 150 ℃ for 30min, keeping the temperature of 180 ℃ for 20min, and keeping the final reaction temperature for 2-8 h.
4. The method for synthesizing tobermorite composite thermal insulation material by using high-alumina fly ash as claimed in claim 3, is characterized in that: the stirring speed is 100-400rpm in the temperature rising process; the stirring speed during the heat preservation process is 100-200 rpm.
5. The method for synthesizing tobermorite composite thermal insulation material by using high-alumina fly ash according to claim 3 or 4, is characterized in that: the temperature rise rate of the sectional temperature rise is 1-3 ℃/min.
6. The method for synthesizing tobermorite composite thermal insulation material by using high-alumina fly ash as claimed in claim 1, is characterized in that: and step two, drying, wherein the drying temperature is 90-100 ℃, and the drying time is 4-16 h.
7. The method for synthesizing tobermorite composite thermal insulation material by using high-alumina fly ash as claimed in claim 6, wherein: the content of alumina in the high-alumina fly ash is 40-50%.
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