CN117776703A - Preparation method of aluminate binder - Google Patents
Preparation method of aluminate binder Download PDFInfo
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- CN117776703A CN117776703A CN202311603255.2A CN202311603255A CN117776703A CN 117776703 A CN117776703 A CN 117776703A CN 202311603255 A CN202311603255 A CN 202311603255A CN 117776703 A CN117776703 A CN 117776703A
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- 150000004645 aluminates Chemical class 0.000 title claims abstract description 28
- 239000011230 binding agent Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 58
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000292 calcium oxide Substances 0.000 claims abstract description 17
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 17
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 239000001110 calcium chloride Substances 0.000 claims abstract description 12
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims description 44
- 238000001816 cooling Methods 0.000 claims description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 25
- 239000012065 filter cake Substances 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000007767 bonding agent Substances 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 10
- 239000011268 mixed slurry Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 13
- 238000001238 wet grinding Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract description 2
- 238000000265 homogenisation Methods 0.000 abstract description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
- 239000011707 mineral Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000004568 cement Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013081 microcrystal Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000008707 rearrangement Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to the technical field of aluminate binder production, and particularly relates to a preparation method of aluminate binder. The superfine powder raw material with extremely high fineness and extremely high homogenization degree can be obtained by adopting the main raw materials of aluminum hydroxide, calcium chloride, calcium oxide and aluminum oxide, precisely and finely compounding according to chemical components corresponding to mineral phase composition, and adopting a ceramic grinding process for wet grinding. After the powder is subjected to filter pressing separation, the powder is subjected to drying treatment, and then is pressed into a raw material blank by adopting automatic forming equipment, and the raw material blank enters a tunnel kiln for calcination. Crushing and grinding the calcined green body to finally prepare the aluminate binder.
Description
Technical Field
The invention belongs to the technical field of aluminate binder production, and particularly relates to a preparation method of aluminate binder.
Background
Aluminate binder is an important inorganic material with excellent physical and chemical properties such as high melting point, good thermal stability, excellent corrosion resistance, etc. These properties make aluminate binders widely used in ceramic, glass, metallurgical and other fields. However, the conventional aluminate binder preparation method generally has problems such as complex reaction process, high energy consumption, low product purity and the like.
Patent application CN103922764B, publication time 2015.08.19. A binder for unshaped refractory and its preparing process are disclosed. The binding agent for the unshaped refractory material comprises the following raw materials in percentage by mass: 30-70% of aluminum oxide, 20-60% of magnesium oxide and 5-20% of excitant, wherein the excitant is a mixture of metasilicic acid, polycarboxylic acid and simple substance silicon, the mass fraction of the metasilicic acid in the excitant mixture is 40-80%, the mass fraction of the polycarboxylic acid in the excitant mixture is 0-40%, and the mass fraction of the simple substance silicon in the excitant mixture is 0-50%. However, the preparation method requires the addition of an exciting agent, thereby improving the preparation difficulty and the production cost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of aluminate bonding agent, which adopts aluminum hydroxide, calcium chloride, calcium oxide and aluminum oxide as main raw materials, precisely and finely prepares materials according to chemical components corresponding to mineral phase composition, adopts a ceramic grinding process to grind by a wet method, and can obtain superfine powder raw materials with extremely high fineness and extremely high homogenization degree. After the powder is subjected to filter pressing separation, the powder is subjected to drying treatment, and then is pressed into a raw material blank by adopting automatic forming equipment, and the raw material blank enters a tunnel kiln for calcination. Crushing and grinding the calcined green body to finally prepare the aluminate binder.
The technical scheme adopted by the invention is as follows:
the preparation method of the aluminate bonding agent comprises the following steps:
(1) Placing the aluminum hydroxide fine powder into a high-temperature furnace, heating to 370-420 ℃, preserving heat for 3-4 hours, heating to 1100-1200 ℃, preserving heat for 3-4 hours, and cooling to obtain alumina powder with high porosity;
(2) Adding the alumina powder with high porosity obtained in the step (1) into a calcium chloride solution, stirring for 15 minutes in vacuum, adding the calcium oxide powder and the alumina powder, and adding water to wet-grind and mix for 15-30 minutes to obtain a mixture;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets;
(4) Drying the blank in the step (3) at 50-80 ℃ for 3-5 hours, then placing the blank into a muffle furnace for heating and firing at 1550-1600 ℃ for 3-5 hours, and crushing the blank after cooling to obtain the aluminate binder.
The heating rate in the step (1) is 2-2.5 ℃/h, and the cooling rate is 1-1.5 ℃/h.
The mass ratio of the aluminum hydroxide to the calcium chloride to the calcium oxide to the aluminum oxide is (3-4): (1-2): (2-3): (1-2).
The particle size of the mixture in the step (2) is 0.045-0.065mm.
In the vacuum stirring process of the step (2), the pressure is 1kPa.
The concentration of the calcium chloride solution in the step (2) is 15-20wt%.
In the filter pressing process of the step (3), the pressure of the filter press is 80-120MPa.
The heating rate in the step (3) is 2.5-3 ℃/h, and the cooling rate is 0.5-1.5 ℃/h.
The reaction principle of the preparation method is as follows:
the invention utilizes aluminum hydroxide fine powder to decompose at 370-420 ℃ to generate nano-scale air holes to form aluminum oxide microcrystals, and utilizes the aluminum oxide microcrystals to generate surface diffusion at 1100-1200 ℃ so as to generate links among the aluminum oxide microcrystals to limit the rearrangement of particles in the middle and later stages of sintering, thus obtaining aluminum oxide powder with high porosity; introducing a calcium chloride solution into the alumina powder with high porosity, and enriching calcium chloride in the calcium chloride solution at a particle linking part under a vacuum condition to prevent the merging and growth of the nano holes; calcium oxide powder and aluminum oxide powder are added into high-porosity aluminum oxide powder to fill gaps among the aluminum oxide powder, so that rearrangement of aluminum oxide particles in a high-temperature sintering process is prevented, and performance of aluminate bonding agent is improved.
Compared with the prior art, the invention has the following beneficial effects:
(1) The reaction process is simple, the energy consumption is low, and the industrial production is easy to realize;
(2) Through mixing raw materials and wet grinding, the raw materials are fully mixed, calcium oxide of one of the raw materials is converted into calcium hydroxide, and meanwhile, the alumina of the other raw material is subjected to particle surface activation.
(3) The compressive strength of the aluminate binder is greatly improved and the performance of the aluminate binder is improved through the preparation of the aluminum hydroxide, the calcium chloride, the calcium oxide and the aluminum oxide by compounding and pre-sintering and then roasting.
Detailed Description
The invention is further illustrated below with reference to examples, which are not intended to limit the practice of the invention.
The testing method comprises the following steps:
compressive strength: GB201-2000 aluminate Cement;
flexural strength: GB201-2000 aluminate Cement;
initial setting time: GB201-2000 aluminate Cement;
final setting time: GB201-2000 aluminate Cement.
Example 1
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Placing 35g of aluminum hydroxide fine powder into a high-temperature furnace, heating to 400 ℃, preserving heat for 3.5 hours, heating to 1150 ℃, preserving heat for 4 hours, and cooling to obtain alumina powder with high porosity, wherein the heating rate is 2.25 ℃/hour, and the cooling rate is 1.25 ℃/hour;
(2) Adding the alumina powder with high porosity obtained in the step (1) into a calcium chloride solution, stirring for 15 minutes in vacuum, adding 25g of the calcium oxide powder and 15g of the alumina powder, adding water, wet-grinding and mixing for 25 minutes to obtain a mixture, wherein the particle size of the mixture is 0.055mm, the pressure is 1kPa during the vacuum stirring process, the concentration of the calcium chloride solution is 18wt%, and the calcium chloride content in the calcium chloride solution is 15g;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 100MPa;
(4) Drying the blank in the step (3) for 4 hours at 65 ℃, then placing the blank into a muffle furnace for heating and firing at 1580 ℃ for 4 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 2.8 ℃/hour, and the cooling rate is 1 ℃/hour.
Example 2
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Placing 30g of aluminum hydroxide fine powder into a high-temperature furnace, heating to 370 ℃, preserving heat for 3 hours, heating to 1100 ℃, preserving heat for 3 hours, and cooling to obtain alumina powder with high porosity, wherein the heating rate is 2 ℃/hour, and the cooling rate is 1 ℃/hour;
(2) Adding the alumina powder with high porosity obtained in the step (1) into a calcium chloride solution, stirring for 15 minutes in vacuum, adding 10g of the calcium oxide powder and 20g of the alumina powder, adding water, wet-grinding and mixing for 15 minutes to obtain a mixture, wherein the particle size of the mixture is 0.045mm, the pressure is 1kPa during the vacuum stirring process, the concentration of the calcium chloride solution is 15wt%, and the calcium chloride content in the calcium chloride solution is 10g;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 80MPa;
(4) Drying the blank in the step (3) for 3 hours at 50 ℃, then placing the blank into a muffle furnace for heating and firing at 1550 ℃ for 3 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 2.5 ℃/hour, and the cooling rate is 0.5 ℃/hour.
Example 3
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Placing 40g of aluminum hydroxide fine powder into a high-temperature furnace, heating to 420 ℃, preserving heat for 4 hours, heating to 1200 ℃, preserving heat for 4 hours, and cooling to obtain alumina powder with high porosity, wherein the heating rate is 2.5 ℃/hour, and the cooling rate is 1.5 ℃/hour;
(2) Adding the alumina powder with high porosity obtained in the step (1) into a calcium chloride solution, stirring for 15 minutes in vacuum, adding 30g of the calcium oxide powder and 20g of the alumina powder, adding water, wet-grinding and mixing for 30 minutes to obtain a mixture, wherein the particle size of the mixture is 0.065mm, the pressure is 1kPa during the vacuum stirring process, the concentration of the calcium chloride solution is 20wt%, and the calcium chloride content in the calcium chloride solution is 20g;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 120MPa;
(4) Drying the blank in the step (3) for 5 hours at 80 ℃, then placing the blank into a muffle furnace for heating and firing at 1600 ℃ for 5 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 3 ℃/hour, and the cooling rate is 1.5 ℃/hour.
Example 4
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Placing 32g of aluminum hydroxide fine powder into a high-temperature furnace, heating to 400 ℃, preserving heat for 4 hours, heating to 1200 ℃, preserving heat for 4 hours, and cooling to obtain alumina powder with high porosity, wherein the heating rate is 2.5 ℃/hour, and the cooling rate is 1.5 ℃/hour;
(2) Adding the alumina powder with high porosity obtained in the step (1) into a calcium chloride solution, stirring for 15 minutes in vacuum, adding 23g of the calcium oxide powder and 13g of the alumina powder, adding water, wet-grinding and mixing for 25 minutes to obtain a mixture, wherein the particle size of the mixture is 0.065mm, the pressure is 1kPa during the vacuum stirring process, the concentration of the calcium chloride solution is 20wt%, and the calcium chloride content in the calcium chloride solution is 12g;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 80MPa;
(4) Drying the blank in the step (3) for 3 hours at 50 ℃, then placing the blank into a muffle furnace for heating and firing at 1550 ℃ for 4 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 2.5 ℃/hour, and the cooling rate is 0.5 ℃/hour.
Example 5
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Placing 38g of aluminum hydroxide fine powder into a high-temperature furnace, heating to 420 ℃, preserving heat for 4 hours, heating to 1200 ℃, preserving heat for 4 hours, and cooling to obtain alumina powder with high porosity, wherein the heating rate is 2.5 ℃/hour, and the cooling rate is 1 ℃/hour;
(2) Adding the alumina powder with high porosity obtained in the step (1) into a calcium chloride solution, stirring for 15 minutes in vacuum, adding 27g of the calcium oxide powder and 18g of the alumina powder, adding water, wet-grinding and mixing for 30 minutes to obtain a mixture, wherein the particle size of the mixture is 0.065mm, the pressure is 1kPa during the vacuum stirring process, the concentration of the calcium chloride solution is 20wt%, and the calcium chloride content in the calcium chloride solution is 12g;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 120MPa;
(4) Drying the blank in the step (3) for 5 hours at 80 ℃, then placing the blank into a muffle furnace for heating and firing at 1580 ℃ for 4 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 3 ℃/hour, and the cooling rate is 0.5 ℃/hour.
Comparative example 1
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Mixing 35g of aluminum hydroxide fine powder, 25g of calcium oxide powder, 15g of aluminum oxide powder and 15g of calcium chloride by adding water and wet grinding for 25 minutes to obtain a mixture, wherein the particle size of the mixture is 0.055mm;
(2) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 100MPa;
(3) Drying the blank in the step (2) for 4 hours at 65 ℃, then placing the blank into a muffle furnace for heating and firing at 1580 ℃ for 4 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 2.8 ℃/hour, and the cooling rate is 1 ℃/hour.
Comparative example 2
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Placing 30g of aluminum hydroxide fine powder into a high-temperature furnace, heating to 370 ℃, preserving heat for 3 hours, heating to 1100 ℃, preserving heat for 3 hours, and cooling to obtain alumina powder with high porosity, wherein the heating rate is 2 ℃/hour, and the cooling rate is 1 ℃/hour;
(2) Adding 10g of calcium oxide powder and 20g of aluminum oxide powder into the high-porosity aluminum oxide powder obtained in the step (1), adding water, wet-milling and mixing for 15 minutes to obtain a mixture, wherein the particle size of the mixture is 0.045mm;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 80MPa;
(4) Drying the blank in the step (3) for 3 hours at 50 ℃, then placing the blank into a muffle furnace for heating and firing at 1550 ℃ for 3 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 2.5 ℃/hour, and the cooling rate is 0.5 ℃/hour.
Comparative example 3
The preparation method of the aluminate bonding agent comprises the following steps:
(1) Adding 50g of calcium oxide powder and 60g of alumina powder into a wet mill, adding water, wet-milling and mixing for 30 minutes to obtain a mixture, wherein the particle size of the mixture is 0.065mm;
(2) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets, wherein the pressure of the filter press is 120MPa;
(3) Drying the blank in the step (2) for 5 hours at 80 ℃, then placing the blank into a muffle furnace for heating and firing at 1600 ℃ for 5 hours, and then crushing the blank to obtain the aluminate binder, wherein the heating rate is 3 ℃/hour, and the cooling rate is 1.5 ℃/hour.
The test data for examples 1-5 and comparative examples 1-3 are shown in Table 1.
TABLE 1 test data for examples 1-5 and comparative examples 1-3
| Compressive Strength/MPa | Flexural Strength/MPa | Initial setting time/min | Final setting time/min | |
| Example 1 | 61 | 10.4 | 155 | 210 |
| Example 2 | 59.8 | 10.0 | 160 | 212 |
| Example 3 | 59.5 | 10.1 | 164 | 215 |
| Example 4 | 60 | 10.1 | 163 | 214 |
| Example 5 | 60.3 | 10.2 | 166 | 218 |
| Comparative example 1 | 52.1 | 9.5 | 172 | 225 |
| Comparative example 2 | 51.2 | 9.2 | 177 | 228 |
| Comparative example 3 | 45.3 | 8.7 | 175 | 226 |
Claims (8)
1. The preparation method of the aluminate binder is characterized by comprising the following steps:
(1) Placing the aluminum hydroxide fine powder into a high-temperature furnace, heating to 370-420 ℃, preserving heat for 3-4 hours, heating to 1100-1200 ℃, preserving heat for 3-4 hours, and cooling to obtain alumina powder with high porosity;
(2) Adding the alumina powder with high porosity obtained in the step (1) into a calcium chloride solution, stirring for 15 minutes in vacuum, adding the calcium oxide powder and the alumina powder, and adding water to wet-grind and mix for 15-30 minutes to obtain a mixture;
(3) Carrying out filter pressing on the mixed slurry, respectively collecting filtrate and filter cakes, and drying and compacting the filter cakes to obtain billets;
(4) Drying the blank in the step (3) at 50-80 ℃ for 3-5 hours, then placing the blank into a muffle furnace for heating and firing at 1550-1600 ℃ for 3-5 hours, and crushing the blank after cooling to obtain the aluminate binder.
2. The method of claim 1, wherein the heating rate in step (1) is 2-2.5 ℃/hr and the cooling rate is 1-1.5 ℃/hr.
3. The preparation method of the aluminate bonding agent according to claim 1, wherein the mass ratio of the aluminum hydroxide to the calcium chloride to the calcium oxide to the aluminum oxide is (3-4): (1-2): (2-3): (1-2).
4. The method of claim 1, wherein the particle size of the mixture in the step (2) is 0.045-0.065mm.
5. The method of claim 1, wherein the pressure in the vacuum stirring process in the step (2) is 1kPa.
6. The method of claim 1, wherein the concentration of the calcium chloride solution in the step (2) is 15-20wt%.
7. The method of claim 1, wherein the pressure of the filter press is 80-120MPa in the press filtration process of step (3).
8. The method of claim 1, wherein the heating rate in the step (3) is 2.5-3 ℃/hr and the cooling rate is 0.5-1.5 ℃/hr.
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