CN113213900A - Dispersible alumina and preparation method and application thereof - Google Patents
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Abstract
The invention particularly relates to a dispersible alumina and a preparation method and application thereof, belonging to the technical field of alumina micro powder, wherein the method comprises the following steps: alpha-Al is added2O3Mixing the micro powder, the sintering aid and the dispersing agent to obtain a mixture; the mixture comprises the following components in percentage by mass: alpha-Al2O360% -80% of micro powder, 10% -30% of sintering aid and 5% -15% of dispersing agent; mixing the mixture with a solvent to obtain a slurry; the solvent accounts for 50% -70% of the mixture; and carrying out spray drying on the slurry to obtain the dispersive alumina micropowder. The prepared dispersive alumina is applied to an alumina slurry system, so that the solid content of the alumina slurry can reach 75 percent, and the sintering temperature of alumina ceramic is reduced by more than 50 ℃.
Description
Technical Field
The invention belongs to the technical field of alumina micro powder, and particularly relates to dispersible alumina and a preparation method and application thereof.
Background
With the development of ceramic industry, the variety of chemical additives used in ceramic production is more and more, the application range is wider and wider, the existence and the action of the chemical additives can be seen from the processes of powder preparation, slurry preparation, plastic blank preparation, molding, drying, sintering and the like, the addition amount of the chemical additives is small, but the action is very critical, and the application of the ceramic additives and the development of various novel ceramic additives become an important aspect of the development of the ceramic industry.
The selection of the ceramic additive is generally determined according to the material performance and the construction operation requirement, and can be a single substance or a composite substance. The dispersant is an important one of the ceramic additives, and in the preparation process of the ceramic slurry, the dispersant can be added to improve the delta potential of a system, so that the fluidity of the slurry is improved, and good dispersing and water reducing effects are achieved. Most of ceramic dispersing agents used in the existing market are liquid, transportation and addition are inconvenient, the addition amount of the liquid ceramic dispersing agent is generally 0.05% -0.5%, and the phenomenon of uneven dispersion can exist due to the fact that the addition amount is small, so that the using effect is influenced. In addition, the liquid ceramic dispersant only has a dispersion water-reducing effect in the use process, and needs to be matched with other additives for use so as to achieve the best material performance.
Chinese patent ZL201510892794.1 'A dispersible alumina micropowder and a preparation method thereof' discloses a preparation method of dispersible alumina, which is prepared from 70-85 wt% of alpha-Al2O3Micro powder and 2-15 wt% of nano alpha-Al2O33. 1-5 wt% of nano gamma-Al2O3And 1-10 wt% of nano alumina sol as a raw material, and adding 5-30 wt% of a dispersing agent and 1-10 wt% of organic alcohol as the raw material, and uniformly mixing; standing for 1-12 hours at the temperature of 60-80 ℃, and then carrying out hot high-speed airflow mixed grinding for 0.1-3 hours at the temperature of 80-110 ℃ to obtain the dispersive alumina micro powder. The dispersive alumina prepared by the method is mainly applied to the field of refractory materials and has only a single water reducing function.
Disclosure of Invention
The application aims to provide the dispersible alumina, and the preparation method and the application thereof, so as to solve the problems of transportation and addition, and achieve the effects of reducing the water addition amount, promoting sintering and reducing the sintering temperature.
The embodiment of the invention provides a preparation method of dispersible alumina, which comprises the following steps:
alpha-Al is added2O3Mixing the micro powder, the sintering aid and the dispersing agent to obtain a mixture; the mixture comprises the following components in percentage by mass: alpha-Al2O360% -80% of micro powder, 10% -30% of sintering aid and 5% -15% of dispersing agent;
mixing the mixture with a solvent to obtain a slurry; the solvent accounts for 50% -70% of the mixture;
and carrying out spray drying on the slurry to obtain the dispersive alumina micropowder.
Optionally, the components of the mixture include, by mass fraction: alpha-Al2O365 to 75 percent of micro powder, 15 to 25 percent of sintering aid and 7.5 to 12.5 percent of dispersant.
Optionally, the solvent accounts for 55-65% of the mixture by mass fraction.
Optionally, the sintering aid comprises at least one of magnesium oxide, manganese dioxide and titanium oxide.
Optionally, the dispersant includes at least one of a polycarboxylic acid dispersant, a polycarboxylate dispersant, and a polysulfonate dispersant.
Optionally, the alpha-Al is calculated by mass fraction2O3Al in micro powder2O3The content of (A) is 95-99.5%.
Optionally, the alpha-Al2O3The particle size of the micro powder is 0.5-5 μm.
Optionally, the particle size of the sintering aid is 3 μm-10 μm.
Based on the same inventive concept, the embodiment of the invention also provides the dispersible alumina, and the dispersible alumina is prepared by the preparation method of the dispersible alumina.
Based on the same inventive concept, the embodiment of the invention also provides an application of the dispersive alumina, which comprises the step of applying the dispersive alumina to the preparation of an alumina slurry system.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the preparation method of the dispersible alumina provided by the embodiment of the invention comprises the following steps: alpha-Al is added2O3Mixing the micro powder, the sintering aid and the dispersing agent to obtain a mixture; the mixture comprises the following components in percentage by mass: alpha-Al2O360% -80% of micro powder, 10% -30% of sintering aid and 5% -15% of dispersing agent; mixing the mixture with a solvent to obtain a slurry; the solvent accounts for 50% -70% of the mixture; and carrying out spray drying on the slurry to obtain the dispersive alumina micropowder. The prepared dispersive alumina is applied to an alumina slurry system, so that the solid content of the alumina slurry can reach 75 percent, and the sintering temperature of alumina ceramic is reduced by more than 50 ℃.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a flow chart of a method provided by an embodiment of the invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In order to solve the technical problems, the general idea of the embodiment of the application is as follows:
according to an exemplary embodiment of the present invention, there is provided a dispersible alumina comprising: raw materials and a solvent; in particular, the solvent may be selected from water.
The raw materials comprise the following components in percentage by mass: alpha-Al2O360% -80% of micro powder, 10% -30% of sintering aid and 5% -15% of dispersing agent;
the water accounts for 50-70% of the raw materials in mass fraction.
α-Al2O3The micro powder is mainly used as a carrier, and a dispersing agent and a sintering aid are uniformly loaded on the surface of the micro powder.
The sintering aid mainly has the effects of reducing the sintering temperature and controlling the mass fraction of the sintering aid to be 10-30% so as to ensure that the sintering aid is uniformly dispersed on the surface of the alumina micro powder and obtain reasonable addition amount through tests. If the mass fraction is too large, the best effect of reducing the sintering temperature cannot be achieved, and other components are affected, and if the mass fraction is too small, the purposes of promoting sintering and reducing the sintering temperature cannot be achieved.
The dispersant mainly has the effects of reducing the water adding amount and the solid content of the slurry, and the reason for controlling the mass fraction of the dispersant to be 5-15% is to ensure that the dispersant is uniformly dispersed on the surface of the alumina micropowder and obtain reasonable adding amount through tests. If the mass fraction is too large, the aim of uniform dispersion cannot be achieved, and the using effect is influenced.
The technical problems of transportation and addition of the conventional industrial ceramic dispersant, reduction of water addition, promotion of sintering and reduction of sintering temperature are very difficult to solve by selecting proper raw materials, chemical reactions among all components are required to be avoided, the dispersant and the sintering aid are uniformly loaded on the surface of alumina, the functions of the dispersant and the sintering aid are not lost in the drying process, all components are cooperatively matched, and the effect of the dispersant and the sintering aid is superior to that of the original single component.
The mechanism of the synergistic cooperation of the components is that the alumina micropowder serves as a carrier, the dispersing agent and the sintering aid are uniformly loaded on the surface of the alumina micropowder, and each component can play the greatest role by controlling the reasonable addition amount of the dispersant and the sintering aid.
As an optional embodiment, the raw materials comprise the following components in percentage by mass: alpha-Al2O365 to 75 percent of micro powder, 15 to 25 percent of sintering aid and 7.5 to 12.5 percent of dispersant;
the water accounts for 55-65% of the raw materials in mass fraction.
As an alternative embodiment, the sintering aid comprises one or both of magnesium oxide, manganese dioxide and titanium oxide.
As an alternative embodiment, the dispersant includes one or both of polycarboxylic acid type dispersants, polycarboxylate type dispersants, and polysulfonate type dispersants.
Specifically, the polycarboxylic acid-based dispersant may be selected from polyacrylic acid, maleic anhydride, and the like; the polycarboxylate dispersant can be selected from sodium polyacrylate, ammonium polyacrylate, etc.; the polysulfonate dispersants may be selected from sodium polystyrene sulfonate, sodium polyvinyl sulfonate, and the like.
As an alternative embodiment, the components are divided by massIn number, the alpha-Al2O3Al in micro powder2O3The content of (A) is 95-99.5%.
According to another exemplary embodiment of the present invention, there is provided a method for preparing the dispersible alumina as described above, the method including:
s1, mixing alpha-Al2O3Mixing the micro powder, the sintering aid and the dispersing agent to obtain a mixture;
as an alternative embodiment, alpha-Al2O3The particle size of the micro powder is 0.5-5 μm.
Control of alpha-Al2O3The reason why the particle size of the micro powder is 0.5-5 μm is to ensure that the dispersant and the sintering aid can be uniformly loaded on the surface of the alumina, and the reason why the particle size is too large is not favorable for obtaining stable slurry, and the reason why the particle size is too small is not favorable for loading the dispersant and the sintering aid on the surface of the alumina.
As an alternative embodiment, the particle size of the sintering aid is 3 μm to 10 μm.
The reason for controlling the particle size of the sintering aid to be 3-10 mu m is to ensure that the sintering aid can have the best sintering promoting effect, and the particle size cannot reach the best sintering promoting effect when being too large or too small, so that the sintering temperature is reduced.
S2, mixing the mixture with water to obtain slurry;
and S3, carrying out spray drying on the slurry to obtain the dispersible alumina micro powder.
It should be noted that the specific steps of spray drying are as follows:
(1) igniting and heating to ensure that the inlet temperature of the spray drying tower reaches 250-350 ℃ and the outlet temperature is 100-120 ℃;
(2) starting a slurry pump to enable the slurry to pass through the atomizer, and rapidly contacting with hot air after atomization to obtain a dry product
(3) The atomized slurry is rapidly contacted with hot air, and water is evaporated to obtain a dry product.
According to another exemplary embodiment of the present invention, there is provided a use of the dispersible alumina as described above including applying the dispersible alumina to prepare an alumina slurry system.
The dispersible alumina of the present application, and the preparation method and application thereof will be described in detail below with reference to examples, comparative examples and experimental data.
Example 1
60 wt% of alpha-Al with a particle size of 0.5 mu m2O3The method comprises the following steps of taking micro powder, 25 wt% of titanium oxide with the particle size of 5 mu m and 15 wt% of polycarboxylic acid dispersant as raw materials, adding 50 wt% of water into the raw materials, uniformly mixing the raw materials to prepare slurry, and then carrying out spray drying process to obtain the dispersible alumina micro powder.
The content of Al2O3 in the dispersed alumina prepared in this example 1 was 64 wt%, the particle size distribution D50 was 9.37 μm, and the ignition loss was 7.3 wt%; the method is used for preparing the alumina slurry, the water adding amount is reduced by 65%, and the sintering temperature is reduced by 65 ℃.
Example 2:
65 wt% of alpha-Al having a particle diameter of 2.0 μm2O3The method comprises the following steps of taking micro powder, 30 wt% of manganese dioxide with the particle size of 3 mu m and 5 wt% of polycarboxylate dispersant as raw materials, adding 70 wt% of water into the raw materials, uniformly mixing to prepare slurry, and then carrying out spray drying process to obtain the dispersible alumina micro powder.
Dispersible alumina Al obtained in example 22O3The content is 66 wt%, the particle size distribution D50 is 9.30 μm, and the ignition loss is 5.2 wt%; the method is used for preparing the alumina slurry, the water adding amount is reduced by 60 percent, and the sintering temperature is reduced by 70 ℃.
Example 3:
70 wt% of alpha-Al having a particle size of 3.5 μm2O3The method comprises the following steps of taking micro powder, 20 wt% of titanium oxide with the particle size of 7 mu m and 10 wt% of polysulfonate dispersant as raw materials, adding 60 wt% of water into the raw materials, uniformly mixing to prepare slurry, and then carrying out spray drying process to obtain the dispersible alumina micro powder.
Dispersible alumina Al obtained in example 32O3The content is 73 wt%, the particle size distribution D50 is 10.28 μm, and the ignition loss is 6.2 wt%; the method is used for preparing the alumina slurry, the water adding amount is reduced by 70 percent, and the sintering temperature is reduced by 60 ℃.
Example 4:
75 wt% of alpha-Al having a particle size of 4.0 μm2O3The method comprises the following steps of taking micro powder, 10 wt% of titanium oxide with the particle size of 10 mu m and 15 wt% of polycarboxylic acid dispersant as raw materials, adding 50 wt% of water into the raw materials, uniformly mixing the raw materials to prepare slurry, and then carrying out spray drying process to obtain the dispersible alumina micro powder.
Dispersible alumina Al obtained in example 42O3The content is 77 wt%, the particle size distribution D50 is 10.8 μm, and the ignition loss is 7.5 wt%; the method is used for preparing the alumina slurry, the water adding amount is reduced by 65 percent, and the sintering temperature is reduced by 50 ℃.
Example 5:
80 wt% of alpha-Al having a particle size of 5.0 μm2O3The method comprises the following steps of taking micro powder, 10 wt% of magnesium oxide with the particle size of 5 mu m and 10 wt% of polycarboxylate dispersant as raw materials, adding 60 wt% of water into the raw materials, uniformly mixing to prepare slurry, and then carrying out spray drying process to obtain the dispersible alumina micro powder.
Dispersible alumina Al obtained in example 52O3The content is 82 wt%, the particle size distribution D50 is 11.25 μm, and the ignition loss is 6.5 wt%; the method is used for preparing the alumina slurry, the water adding amount is reduced by 60 percent, and the sintering temperature is reduced by 50 ℃.
Comparative example 1
85 wt% of alpha-Al having a particle size of 6.0 μm2O3The method comprises the following steps of taking micro powder, 15 wt% of magnesium oxide with the particle size of 5 mu m and 0 wt% of polycarboxylate dispersant as raw materials, adding 100 wt% of water into the raw materials, uniformly mixing to prepare slurry, and then carrying out spray drying process to obtain the dispersible alumina micro powder.
Dispersible alumina Al prepared in comparative example 12O3The content is 85 wt%, the particle size distribution D50 is 12.25 μm, and the ignition loss is 0.5 wt%; when the method is used for preparing the alumina slurry, the water adding amount is reduced by 0 percent, and the sintering temperature is reduced by 30 ℃.
Comparative example 2:
70 wt% of alpha-Al having a particle size of 3.0 μm2O3Micro powder, 0 wt% of titanium oxide with the particle size of 5 mu m and 30 wt% of polycarboxylate dispersant are taken as raw materials, and 40 wt% of the raw materials is added% of water is mixed evenly to prepare slurry, and then the dispersive alumina micro powder is obtained through a spray drying process.
Dispersible alumina Al prepared in comparative example 22O3The content is 79 wt%, the particle size distribution D50 is 9.63 μm, and the ignition loss is 15 wt%; the method is used for preparing the alumina slurry, the water adding amount is reduced by 60 percent, and the sintering temperature is reduced by 0 ℃.
Comparative example 3:
85 wt% of alpha-Al having a particle size of 5.0 μm2O3The method comprises the following steps of taking micro powder, 10 wt% of magnesium oxide with the particle size of 5 mu m and 5 wt% of polycarboxylate dispersant as raw materials, adding 50 wt% of water into the raw materials, uniformly mixing to prepare slurry, and then carrying out spray drying process to obtain the dispersible alumina micro powder.
Dispersible alumina Al prepared in comparative example 32O3The content is 88 wt%, the particle size distribution D50 is 10.35 μm, the ignition loss is 2.0 wt%; when the method is used for preparing the alumina slurry, the water adding amount is reduced by 55 percent, and the sintering temperature is reduced by 40 ℃.
Examples of the experiments
The dispersible alumina fine powders obtained in examples 1 to 5 and comparative examples 1 to N were examined and used to prepare alumina slurry to obtain the amount of water added and sintering temperature required for their preparation, and the results are shown in the following table.
The method can be used for preparing the dispersible alumina by using the method provided by the invention, the solid content of the alumina slurry can reach 75%, the sintering temperature of the alumina ceramic is reduced by more than 50 ℃, the dispersible alumina has the functions of reducing water and reducing the sintering temperature, and the dispersible alumina can be obtained by comparing the comparative example data with the embodiment data. If the proportion is not appropriate, the effect is not obvious.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) the dispersible alumina provided by the invention is solid, solves the problems of transportation and addition of the existing liquid ceramic dispersant, and simultaneously achieves the effects of reducing water addition, promoting sintering and reducing sintering temperature when preparing an alumina slurry system;
(2) the method provided by the invention has the advantages that the use performance is superior to that of a liquid dispersant due to pre-dispersion;
(3) the method provided by the invention compounds a plurality of ceramic additives to form functional powder integrating multiple functions;
(4) the dispersible alumina prepared by the method provided by the invention is applied to an alumina slurry system, so that the solid content of the alumina slurry can reach 75%, and the sintering temperature of alumina ceramic is reduced by more than 50 ℃.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A method of preparing a dispersible alumina, the method comprising:
alpha-Al is added2O3Mixing the micro powder, the sintering aid and the dispersing agent to obtain a mixture; the mixture comprises the following components in percentage by mass: alpha-Al2O360% -80% of micro powder, 10% -30% of sintering aid and 5% -15% of dispersing agent;
mixing the mixture with a solvent to obtain a slurry; the solvent accounts for 50% -70% of the mixture;
and carrying out spray drying on the slurry to obtain the dispersive alumina micropowder.
2. The method for preparing dispersible alumina according to claim 1, wherein the composition of the mixture comprises, in mass fraction: alpha-Al2O365 to 75 percent of micro powder, 15 to 25 percent of sintering aid and 7.5 to 12.5 percent of dispersant.
3. The method for preparing dispersible alumina according to claim 2, wherein the solvent is 55-65% of the mixture by mass fraction.
4. The method of producing dispersible alumina according to claim 1, wherein the sintering aid comprises at least one of magnesium oxide, manganese dioxide and titanium oxide.
5. The method of claim 1, wherein the dispersant is at least one of a polycarboxylic acid dispersant, a polycarboxylate dispersant and a polysulfonate dispersant.
6. The method for producing a dispersible alumina according to claim 1, wherein the α -Al is contained in a mass fraction2O3Al in micro powder2O3The content of (A) is 95-99.5%.
7. The method for producing a dispersible alumina according to claim 1, wherein the alumina is a dispersion-type aluminaIn that the alpha-Al2O3The particle size of the micro powder is 0.5-5 μm.
8. The method for producing dispersible alumina according to claim 1, wherein the particle diameter of the sintering aid is 3 μm to 10 μm.
9. A dispersible alumina produced by the method for producing a dispersible alumina according to any one of claims 1 to 8.
10. Use of the dispersible alumina of claim 9, comprising applying the dispersible alumina to prepare an alumina slurry system.
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