CN118005027A - Method for preparing calcium silicate powder by using desert sand - Google Patents

Method for preparing calcium silicate powder by using desert sand Download PDF

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CN118005027A
CN118005027A CN202410423852.5A CN202410423852A CN118005027A CN 118005027 A CN118005027 A CN 118005027A CN 202410423852 A CN202410423852 A CN 202410423852A CN 118005027 A CN118005027 A CN 118005027A
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desert sand
calcium silicate
powder
mixed
mixed powder
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CN118005027B (en
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罗雯莉
史志铭
王文彬
刘镇
刘志文
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Inner Mongolia University of Technology
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Inner Mongolia University of Technology
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Abstract

The invention provides a method for preparing calcium silicate powder by using desert sand, belonging to the technical field of calcium silicate preparation. The invention mixes the desert sand, the calcium carbonate, the ferric oxide and the aluminum oxide and then grinds the mixture to obtain mixed powder; the mixed desert sand comprises first desert sand and second desert sand; the grain size of the first desert sand is 20-100 meshes, and the grain size of the second desert sand is more than 100 meshes; the mass content of the second desert sand in the mixed powder is 5-10%; the mixed powder is subjected to presintering and calcination in sequence to obtain calcium silicate powder; the calcination temperature is 1200-1350 ℃, and the heat preservation time is 20-40 min. The invention synthesizes the calcium silicate powder by using the desert sand as the main raw material, the raw material resources are rich, the SiO 2 content is high, no additional siliceous correction material is needed, and the feldspar in the desert sand can obviously reduce the sintering temperature and sintering time of the calcium silicate powder.

Description

Method for preparing calcium silicate powder by using desert sand
Technical Field
The invention belongs to the technical field of calcium silicate preparation, and particularly relates to a method for preparing calcium silicate powder by using desert sand.
Background
Calcium silicate (Ca xSiOy, x=2 or 3;y =4 or 5) is mainly used as a building material, a biological material, a refractory material and a ceramic material, and has an incomparable advantage of other materials such as a metal material, a polymer material and the like: good mechanical property, fire resistance and carbonization resistance, and becomes the most important and irreplaceable material in human society.
In the condition of calcium silicate calcination, the calcination temperature is very important, and not only affects the content of each mineral in the system, but also affects the crystal structure of the mineral, the phase characteristics of the mineral, the mineral distribution and the like, and further affects the performance of the mineral. Studies have shown that the higher the tricalcium silicate content in the system, the more complete the crystallization and the higher the strength of the system. Therefore, in order to pursue high tricalcium silicate content, the calcination temperature needs to be increased or the calcination time needs to be prolonged, in the prior art, the calcination temperature of the calcium silicate powder prepared by adopting shale, siltstone and other raw materials is 1350-1500 ℃ for 2-3 hours, which can certainly increase the sintering heat consumption and the cost.
Disclosure of Invention
In view of the above, the present invention aims to provide a calcium silicate powder prepared from desert sand and a preparation method thereof. The method for preparing the calcium silicate has the advantages of low sintering temperature, short sintering time, easily obtained raw materials, low preparation cost and high tricalcium silicate content in the prepared calcium silicate powder.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a method for preparing calcium silicate powder by using desert sand, which comprises the following steps:
Mixing the mixed desert sand, calcium carbonate, ferric oxide and aluminum oxide, and grinding to obtain mixed powder; the mixed desert sand comprises first desert sand and second desert sand; the grain size of the first desert sand is 20-100 meshes, and the grain size of the second desert sand is more than 100 meshes; the mass content of the second desert sand in the mixed powder is 5-10%;
the mixed powder is subjected to presintering and calcination in sequence to obtain calcium silicate powder; the calcination temperature is 1200-1350 ℃, and the heat preservation time is 20-40 min.
Preferably, the mass content of the silicon dioxide in the mixed desert sand is 70-84%.
Preferably, the mixed desert sand comprises :CaO 3~5%,Al2O3 5~10%,Fe2O3 2~4%,K2O 2~4%,Na2O 3~5%,MgO 0.7~1.2%,TiO2 0.3~0.8%.
Preferably, the mixed powder comprises, based on the mass content of the oxide :70~85%CaO,12~20%SiO2,1.3~4%Al2O3,1.3~4%Fe2O3,0.1~0.6%MgO,0.1~0.5%NaO,0.1~0.5%K2O,0.1~0.4%TiO2.
Preferably, the particle size of the mixed powder is 10-30 μm.
Preferably, the presintering temperature is 800-1000 ℃, and the heat preservation time is 20-40 min.
Preferably, the pre-firing atmosphere is an air atmosphere.
Preferably, the calcination temperature is 1250-1300 ℃.
Preferably, the calcination is carried out for a holding time of 30min.
Preferably, the calcined atmosphere is an air atmosphere.
The invention provides a method for preparing calcium silicate powder by using desert sand, which comprises the following steps: mixing the mixed desert sand, calcium carbonate, ferric oxide and aluminum oxide, and grinding to obtain mixed powder; the mixed desert sand comprises first desert sand and second desert sand; the grain size of the first desert sand is 20-100 meshes, and the grain size of the second desert sand is more than 100 meshes; the mass content of the second desert sand in the mixed powder is 5-10%; the mixed powder is subjected to presintering and calcination in sequence to obtain calcium silicate powder; the calcination temperature is 1200-1350 ℃, and the heat preservation time is 20-40 min. According to the invention, the calcium silicate powder is synthesized by using the desert sand as a main raw material, the desert sand has the advantage of abundant resources, the main component of the desert sand is SiO 2, and meanwhile, the main component of the second desert sand with the grain diameter of more than 100 meshes is feldspar phase, wherein the feldspar phase has good fluxing action, can form liquid phase at a lower temperature, has promotion effect on the formation and growth of crystal phase, and promotes the densification of a calcium silicate structure, so that the calcium silicate powder meeting the requirements with higher tricalcium silicate content can be prepared in a shorter time and at a lower calcination temperature (at 1200-1350 ℃ for 20-40 min). The method for preparing the calcium silicate powder by using the desert sand has the advantages of rich resources and low cost, does not need blasting, crushing and mud washing during exploitation, is suitable for industrial production, and has great practical value and economic benefit. According to the embodiment data, the content of tricalcium silicate in the calcium silicate powder prepared by calcining at 1200-1350 ℃ for 20-40 min is 55-65%, which is higher than that of the existing tricalcium silicate powder under the same calcining condition (generally 40-50%).
In addition, the production of existing calcium silicate consumes a great deal of natural resources, resulting in over-exploitation of mineral resources and serious environmental damage. Currently, the industry is challenged by inadequate raw material supplies and environmental protection, and is required to find alternative raw materials for the production of calcium silicate. At present, siliceous raw materials mainly adopted in China comprise clay, loess, shale powder, sandstone, aggregate mud and the like, and in order to protect cultivated land from occupying farmlands, the raw materials such as shale, siltstone and the like are mainly adopted in recent years to prepare calcium silicate, but the siliceous raw materials have lower silicic acid rate, the SiO 2 content with loss on ignition removed is only 55-65%, and siliceous correction materials are generally required to be added in the process of batching, so that extra cost is increased. According to the invention, the calcium silicate powder is synthesized by using the desert sand as the main raw material, the desert sand has the advantage of rich resources, the SiO 2 content in the desert sand is 70-84%, and no additional siliceous correction material is needed, so that the preparation cost of the calcium silicate is further reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM image of calcium silicate powder prepared according to example 1;
FIG. 2 is an XRD pattern of the calcium silicate powder prepared in example 1;
FIG. 3 is a graph showing the particle size distribution of C 2 S and C 3 S in the calcium silicate powder prepared in example 1;
FIG. 4 is an SEM image of calcium silicate powder prepared according to example 2;
FIG. 5 is an XRD pattern of the calcium silicate powder prepared in example 2;
FIG. 6 is a graph showing the particle size distribution of C 2 S and C 3 S in the calcium silicate powder prepared in example 2;
FIG. 7 is an SEM image of calcium silicate powder prepared according to example 3;
FIG. 8 is an XRD pattern of the calcium silicate powder prepared in example 3;
FIG. 9 is a graph showing the particle size distribution of C 2 S and C 3 S in the calcium silicate powder prepared in example 3;
FIG. 10 is an SEM image of calcium silicate powder prepared according to comparative example 1;
FIG. 11 is an XRD pattern of the calcium silicate powder prepared in comparative example 1;
FIG. 12 is a graph showing the particle size distribution of C 2 S and C 3 S in the calcium silicate powder prepared in comparative example 1.
Detailed Description
The invention provides a method for preparing calcium silicate powder by using desert sand, which comprises the following steps:
Mixing the mixed desert sand, calcium carbonate, ferric oxide and aluminum oxide, and grinding to obtain mixed powder; the mixed desert sand comprises first desert sand and second desert sand; the grain size of the first desert sand is 20-100 meshes, and the grain size of the second desert sand is more than 100 meshes; the mass content of the second desert sand in the mixed powder is 5-10%;
The mixed powder is subjected to presintering and calcination in sequence to obtain desert sand calcium silicate powder; the calcination temperature is 1200-1350 ℃, and the heat preservation time is 20-40 min.
In the present invention, the raw materials used are commercially available products well known in the art, unless specifically described otherwise.
The invention mixes the desert sand, the calcium carbonate, the ferric oxide and the aluminum oxide and then grinds the mixture to prepare the mixed powder.
In the present invention, the mixed desert sand includes a first desert sand and a second desert sand; the grain size of the first desert sand is 20-100 meshes, and the grain size of the second desert sand is more than 100 meshes. In the invention, the main component of the second desert sand is feldspar phase, and the main component of the first desert sand with the particle size of 20-100 meshes is SiO 2. According to the invention, the first desert sand with the particle size of 20-100 meshes and the second desert sand with the particle size of more than 100 meshes (the main component is feldspar phase) are preferably obtained by screening the desert sand, and the two desert sand with different particle sizes are mixed to obtain the mixed desert sand. The invention controls the content of feldspar phase by controlling the dosage of the second desert sand. In the invention, the mass content of the second desert sand in the mixed powder is 5-10%, preferably 6-8%, and more preferably 7%. The invention can prevent the content of the feldspar phase from being too low to play a role in fluxing by controlling the content of the second desert sand in the mixed powder in the range, and can prevent the content of the feldspar phase from being too high to adversely affect the physical and mechanical properties of the calcium silicate powder in the later stage (such as reducing the strength of the calcium silicate).
In the invention, the content of silicon dioxide in the mixed desert sand is preferably 70-84%, more preferably 75-80%, and even more preferably 77-79%. The sand has high silicon dioxide content, and no additional siliceous correction material is needed.
In the present invention, the mixed desert sand preferably further comprises :CaO 3~5%,Al2O3 5~10%,Fe2O3 2~4%,K2O 2~4%,Na2O 3~5%,MgO 0.7~1.2%,TiO2 0.3~0.8%;, more preferably comprises CaO 3.5~4.8%,Al2O3 6.0~9.5%,Fe2O3 2.2~3.8%,K2O 2.3~3.7%,Na2O 3.2~4.8%,MgO 0.8~1.0%,TiO2 0.4~0.6%,, and further preferably comprises, based on the mass content of the oxides CaO 4.8%,Al2O3 6.32%,Fe2O3 2.3%,K2O 2.4%,Na2O 3.3%,MgO 0.9%,TiO2 0.5%.
In the present invention, the calcium carbonate is preferably industrial calcium carbonate, the iron oxide is preferably industrial iron oxide, and the alumina is preferably industrial alumina. Calcium carbonate is used as a reactant, and aluminum oxide and iron oxide are used as sintering aids.
In the present invention, the amounts of the mixed desert sand, calcium carbonate, iron oxide and aluminum oxide are determined according to the composition of the mixed powder. In the present invention, the mixed powder preferably comprises :70~85%CaO,12~20%SiO2,1.3~4%Al2O3,1.3~4%Fe2O3,0.1~0.6%MgO,0.1~0.5%NaO,0.1~0.5%K2O,0.1~0.4%TiO2,, more preferably :70~85%CaO,12~20%SiO2,1.3~4%Al2O3,1.3~4%Fe2O3,0.1~0.6%MgO,0.1~0.5%NaO,0.1~0.5%K2O,0.1~0.4%TiO2,, based on the mass content of the oxide 72~80%CaO,14~18%SiO2,2.1~3.5%Al2O3,2.2~3.3%Fe2O3,0.2~0.3%MgO,0.24~0.45%NaO,0.25~0.32%K2O,0.25~0.32%TiO2.
In the present invention, the particle diameter of the mixed powder is preferably 10 to 30. Mu.m, more preferably 15 to 25. Mu.m, still more preferably 19 to 22. Mu.m. The invention has no special requirements for the grinding, and the grinding is performed by means well known in the art.
After the mixed powder is obtained, the mixed powder is subjected to presintering and calcination in sequence to obtain the calcium silicate powder.
In the invention, the temperature of the presintering is preferably 800-1000 ℃, more preferably 900-950 ℃, and the heat preservation time is preferably 20-40 min, more preferably 25-30 min; the pre-firing atmosphere is preferably an air atmosphere. The invention ensures that calcium carbonate is fully decomposed by presintering and reacts with SiO 2 more quickly. In the invention, the calcination temperature is 1200-1350 ℃, preferably 1250-1300 ℃, more preferably 1250-1280 ℃, the heat preservation time is 20-40 min, preferably 25-30 min, more preferably 30 min, and the calcination atmosphere is preferably air atmosphere. The invention preferably carries out presintering and calcining in two muffle furnaces, specifically, the mixed powder is presintered first, and the mixed powder is immediately put into the other muffle furnace with heated after presintering is finished for calcining. In the present invention, the calcined atmosphere is preferably an air atmosphere. In the calcination process, calcium carbonate reacts with SiO 2 to mainly generate dicalcium silicate and tricalcium silicate.
In the present invention, the calcined product is preferably immediately taken out and cooled in air.
In the invention, the main crystal phases formed in the calcium silicate powder are preferably tricalcium silicate and dicalcium silicate, the content of tricalcium silicate in the calcium silicate powder is 55-65%, more preferably 58-63%, and the average grain size of tricalcium silicate is preferably 10-15 μm, more preferably 12-14 μm. The content of dicalcium silicate in the calcium silicate powder is preferably 15-25%, more preferably 18-22%, and the average grain size of dicalcium silicate is preferably 9-14 μm, more preferably 10-13 μm.
In the present invention, the calcium silicate powder preferably further includes an intermediate phase, and the intermediate phase preferably includes a glass phase, tricalcium aluminate, and tetracalcium aluminoferrite.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to specific examples, and the described embodiments are only some embodiments of the present invention, but not all embodiments. Any modification, equivalent replacement, improvement, etc. of the embodiments of the present invention without making any creative effort shall fall within the protection scope of the present invention according to the technical spirit and general principles of the present invention.
Sources of second desert sand used in the following examples:
screening the Kubuji desert sand under a 100-mesh screen, wherein the 100-mesh screen is a second desert sand, and the main composition is feldspar phase.
Example 1
Mixing 20-100 mesh first desert sand, calcium carbonate, aluminum oxide, ferric oxide and second desert sand, and ball milling for 2h to obtain mixed powder, wherein the mass ratio of the second desert sand in the mixed powder is 5%. The mass percentage of each component in the mixed powder is 70%CaO、18%SiO2、3%Al2O3、8%Fe2O3、0.2%MgO、0.4%Na2O、0.3%K2O、0.1%TiO2., the mixed powder is presintered at 900 ℃ for 30min, the mixed powder is transferred into a muffle furnace heated to 1250 ℃, the mixed powder is continuously calcined in air atmosphere for 30min, and the mixed powder is immediately taken out and rapidly cooled in air after the calcination is finished, and the calcium silicate powder is obtained after cooling to room temperature.
SEM observation of the calcium silicate powder prepared in example 1 showed that the main phases were dicalcium silicate and tricalcium silicate, as shown in fig. 1. The particle diameters of C 2 S and C 3 S in the calcium silicate powder prepared in example 1 were characterized, and the results are shown in FIG. 3. As can be seen from fig. 3, the average grain size of the synthesized dicalcium silicate is 12.6 μm and the average grain size of tricalcium silicate is 10 μm. Fig. 2 is an XRD pattern of the calcium silicate powder prepared in example 1. As can be seen from the figure, the main crystal phases formed in the prepared calcium silicate powder are tricalcium silicate and dicalcium silicate, the contents of which are 55% and 20% respectively, and the second phase is an intermediate phase comprising a glass phase, tricalcium aluminate and tetracalcium aluminoferrite.
Example 2
Mixing 20-100 mesh first desert sand, calcium carbonate, aluminum oxide, ferric oxide and second desert sand, ball milling for 2h to obtain mixed powder, wherein the mass ratio of the second desert sand in the mixed powder is 7%. The mass percentage of each component in the mixed powder is 75%CaO、16%SiO2、2.2%Al2O3、6%Fe2O3、0.2%MgO、0.2%Na2O、0.3%K2O、0.1%TiO2., the mixed powder is presintered at 900 ℃ for 30min, the mixed powder is transferred into a muffle furnace heated to 1300 ℃, the mixed powder is continuously calcined in air atmosphere for 30min, and the mixed powder is immediately taken out and rapidly cooled in air after the calcination is finished, and the calcium silicate powder is obtained after cooling to room temperature.
SEM observation of the calcium silicate powder prepared in example 2 showed that the main phases were dicalcium silicate and tricalcium silicate, as shown in fig. 4. The particle diameters of C 2 S and C 3 S in the calcium silicate powder prepared in example 2 were characterized, and the results are shown in FIG. 6. As can be seen from FIG. 6, the average grain size of the synthesized dicalcium silicate is 10.7 μm and the average grain size of tricalcium silicate is 11.5. Mu.m. Fig. 5 is an XRD pattern of the calcium silicate powder prepared in example 2. As can be seen from the figure, the main crystal phases formed in the prepared calcium silicate powder are tricalcium silicate and dicalcium silicate, the contents of which are respectively 60% and 20%, and the second phase is an intermediate phase comprising a glass phase, tricalcium aluminate and tetracalcium aluminoferrite.
Example 3
Mixing 20-100 mesh first desert sand, calcium carbonate, aluminum oxide, ferric oxide and second desert sand, ball milling for 2h to obtain mixed powder, wherein the mass ratio of the second desert sand in the mixed powder is 10%. The mass percentage of each component in the mixed powder is 80%CaO、15%SiO2、2%Al2O3、2.4%Fe2O3、0.1%MgO、0.2%Na2O、0.2%K2O、0.1%TiO2., the mixed powder is presintered at 900 ℃ for 30min, the mixed powder is transferred into a muffle furnace heated to 1350 ℃, the mixed powder is continuously calcined in air atmosphere for 30min, and the mixed powder is immediately taken out and rapidly cooled in air after the calcination is finished, and the calcium silicate powder is obtained after cooling to room temperature.
SEM observation of the calcium silicate powder prepared in example 3 showed that the main phases were dicalcium silicate and tricalcium silicate, as shown in fig. 7. The particle diameters of C 2 S and C 3 S in the calcium silicate powder prepared in example 3 were characterized, and the results are shown in FIG. 9. As can be seen from fig. 9, the average grain size of the synthesized dicalcium silicate is 9.6 μm and the average grain size of tricalcium silicate is 13.4 μm. Fig. 8 is an XRD pattern of the calcium silicate powder prepared in example 3. As can be seen from the figure, the main crystal phases formed in the prepared calcium silicate powder are tricalcium silicate and dicalcium silicate, the contents of which are 57% and 20% respectively, and the second phase is an intermediate phase comprising a glass phase, tricalcium aluminate and tetracalcium aluminoferrite.
Comparative example 1
Mixing clay, calcium carbonate, aluminum oxide and ferric oxide, and ball milling for 2h to obtain mixed powder (the tested clay mixed powder only contains trace feldspar phase). The mass percentage of each component in the mixed powder is 82.2%CaO、13%SiO2、2%Al2O3、2.4%Fe2O3、0.1%MgO、0.1%Na2O、0.1%K2O、0.1%TiO2., the mixed powder is presintered at 900 ℃ for 30min, the mixed powder is transferred into a muffle furnace heated to 1350 ℃, the mixed powder is continuously calcined in air atmosphere for 30min, and the mixed powder is immediately taken out and rapidly cooled in air after the calcination is finished, and the calcium silicate powder is obtained after cooling to room temperature.
SEM observation of the calcium silicate powder prepared in comparative example 1 showed that the sample was still in the firing stage, as shown in fig. 10, and the morphology of dicalcium silicate and tricalcium silicate was not prominent. The particle diameters of C 2 S and C 3 S in the calcium silicate powder prepared in comparative example 1 were characterized, and the results are shown in FIG. 12. As can be seen from fig. 12, the average grain size of the synthesized dicalcium silicate is 15.1 μm and the average grain size of tricalcium silicate is 8 μm. Fig. 11 is an XRD pattern of the calcium silicate powder prepared in comparative example 1. As can be seen from the figure, the main crystal phases formed in the prepared calcium silicate powder are tricalcium silicate and dicalcium silicate, the contents of which are 30% and 29% respectively, and the second phase is an intermediate phase comprising a glass phase, tricalcium aluminate and tetracalcium aluminoferrite. The calcium silicate powder finally obtained in comparative example 1 by calcination at 1350 ℃ for 30min has a significantly lower content of tricalcium silicate than the present application, because the feldspar phase content in the clay is too low to act as a fluxing agent, thereby resulting in the inability to form more tricalcium silicate at lower calcination temperatures.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (10)

1. The method for preparing the calcium silicate powder by using the desert sand is characterized by comprising the following steps of:
Mixing the mixed desert sand, calcium carbonate, ferric oxide and aluminum oxide, and grinding to obtain mixed powder; the mixed desert sand comprises first desert sand and second desert sand; the grain size of the first desert sand is 20-100 meshes, and the grain size of the second desert sand is more than 100 meshes; the mass content of the second desert sand in the mixed powder is 5-10%;
the mixed powder is subjected to presintering and calcination in sequence to obtain calcium silicate powder; the calcination temperature is 1200-1350 ℃, and the heat preservation time is 20-40 min.
2. The method of claim 1, wherein the mass content of silica in the mixed desert sand is 70-84%.
3. The method according to claim 1 or 2, wherein the mixed desert sand comprises, based on the mass content of oxides :CaO 3~5%,Al2O3 5~10%,Fe2O3 2~4%,K2O 2~4%,Na2O 3~5%,MgO 0.7~1.2%,TiO2 0.3~0.8%.
4. The method according to claim 1, wherein the mixed powder comprises, based on the mass content of the oxide :70~85%CaO,12~20%SiO2,1.3~4%Al2O3,1.3~4%Fe2O3,0.1~0.6%MgO,0.1~0.5%NaO,0.1~0.5%K2O,0.1~0.4%TiO2.
5. The method according to claim 1 or 4, wherein the particle size of the mixed powder is 10 to 30 μm.
6. The method according to claim 1, wherein the pre-sintering temperature is 800-1000 ℃ and the heat preservation time is 20-40 min.
7. The method according to claim 1 or 6, wherein the pre-burned atmosphere is an air atmosphere.
8. The method of claim 1, wherein the calcination temperature is 1250-1300 ℃.
9. The method of claim 1, wherein the calcination is performed for a soak time of 30 min.
10. The method of claim 1, wherein the calcined atmosphere is an air atmosphere.
CN202410423852.5A 2024-04-10 2024-04-10 Method for preparing calcium silicate powder by using desert sand Active CN118005027B (en)

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