CN113213513A - Preparation method of large primary crystal alpha-alumina - Google Patents
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- CN113213513A CN113213513A CN202110398630.9A CN202110398630A CN113213513A CN 113213513 A CN113213513 A CN 113213513A CN 202110398630 A CN202110398630 A CN 202110398630A CN 113213513 A CN113213513 A CN 113213513A
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Abstract
The invention discloses a preparation method of large primary crystal alpha-alumina for overcoming the problem that a fluorine-containing additive in the prior art has large corrosion to kiln equipment for producing alumina powder, which comprises the following steps of 1, mixing boric acid and a calcium carbonate reagent for 5-40 min according to the weight ratio of 10: 0.1-2 to obtain M1; step 2, adding M1 into gamma-alumina, and mixing for 5-120 min to obtain M2, wherein the using amount of M1 is 0.2-3% of the weight of the gamma-alumina; step 3, calcining M2 at 1300-1500 ℃ for 2-8 h to obtain M3; and 4, grinding by using M3 for 1-3 h to obtain the large primary crystal alpha-alumina. The invention provides a preparation method of large primary crystal alpha-alumina, which reduces the corrosion damage to high-temperature kiln equipment and reduces the maintenance cost because the raw materials do not adopt fluorine-containing additives.
Description
Technical Field
The invention relates to the technical field of preparation of alumina powder, in particular to a preparation method of large primary crystal alpha-alumina.
Background
In the field of electronic devices, a large amount of alumina with the median particle size D50 of 2-5 mu m is used as a heat-conducting filler, or an alumina raw material with the median particle size D50 of 2-5 mu m is used for preparing spherical alumina, so that the market demand is high. In the prior art, a fluorine-containing additive is often added in the preparation process of alumina powder to promote the grain growth.
However, in the preparation process of the alumina powder, the fluorine-containing additive has great corrosion to the kiln equipment, so that the kiln equipment needs to be stopped for maintenance for many times, and the maintenance cost is high. On the other hand, due to the mass difference of the alumina powder raw materials, the performance of the prepared alpha-alumina is unstable.
Disclosure of Invention
The invention provides a preparation method of large primary crystal alpha-alumina for overcoming the problem that the fluorine-containing additive has larger corrosion to kiln equipment for producing alumina powder in the prior art, and the fluorine-containing additive is not adopted in the raw materials, so that the corrosion damage to high-temperature kiln equipment is reduced, and the maintenance cost is reduced.
The technical scheme adopted by the invention is as follows:
the preparation method of the large primary crystal alpha-alumina comprises the following steps
Step 1, mixing boric acid and a calcium carbonate reagent for 5-40 min according to a weight ratio of 10: 0.1-2 to obtain M1;
and 4, grinding by using M3 for 1-3 h to obtain the large primary crystal alpha-alumina.
Further, in the step 1, the purity of the boric acid is more than or equal to 99%.
Further, in the step 1, the purity of the calcium carbonate is more than or equal to 99 percent.
Furthermore, in the step 2, the moisture content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
Further, in the step 4, an airflow mill is adopted during grinding, and a sorting machine is matched with the grading powder.
Furthermore, the grinding pressure is 0.1-0.5 MPa when the jet mill is used for grinding.
Further, in step 3, the M2 is washed before calcination.
Further, when the furnace is washed, the temperature in the furnace is gradually increased to 1000 ℃, the temperature increasing time is 1.5-2 h, nitrogen and air are alternately injected into the furnace in the temperature increasing process, the time for injecting nitrogen or air once is 0.5h,the flow rate is 1-10 m3/min。
The invention has the beneficial effects that:
1. in order to solve the problem that the fluorine-containing additive has large corrosion to kiln equipment for producing alumina powder in the prior art, the invention provides a preparation method of large primary crystal alpha-alumina. The method has simple process and convenient operation. Because the raw materials do not adopt the additive containing fluorine, the corrosion damage to high-temperature kiln equipment is reduced, and the maintenance cost is reduced.
2. The invention adopts single gamma-alumina as the main raw material, and avoids the influence of the quality fluctuation of the raw material on the quality of the large primary crystal alpha-alumina from the source.
3. In the invention, the furnace washing operation is carried out in the furnace before the alumina is calcined, so that impurities in the furnace are removed as much as possible, the influence on the alumina calcination is avoided, and the production stability of the alumina among different batches is ensured.
4. The median particle size D50 of the large primary crystal alpha-alumina prepared by the method is 2-6 μm.
Drawings
FIG. 1 shows the results of laser particle size measurement of the gamma-alumina raw material before calcination in example 2.
FIG. 2 shows the results of laser particle size measurement of large primary-crystal alpha-alumina after calcination and grinding in example 2.
FIG. 3 shows the results of X-ray diffraction measurements of the gamma-alumina starting material before calcination in example 3.
FIG. 4 shows the X-ray diffraction results of the large primary crystal α -alumina after calcination and grinding in example 3.
Detailed Description
Example 1
A preparation method of large primary crystal alpha-alumina comprises the following steps,
step 1: mixing boric acid and calcium carbonate reagent at a ratio of 10:1 for 20min to obtain M1. Wherein, the purity of the boric acid and the calcium carbonate is more than 99 percent.
Step 2: m1 was added to the gamma-alumina feedstock at 1% wt and mixed using a blender for 120min to give M2. Wherein the water content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
And step 3: and calcining the M2 in a high-temperature furnace at 1500 ℃ for 5 hours to obtain M3. Before M2 is placed in a high-temperature furnace, the temperature in the furnace is gradually increased to 1000 ℃, the temperature increasing time is 1.5-2 hours, nitrogen and air are alternately injected into the furnace in the temperature increasing process, the time for single injection of nitrogen or air is 0.5 hour, and the flow is 1-10M3/min。
And 4, step 4: and (3) grinding the M3 in an airflow mill, and matching grading and powder selection with a classifier to obtain the product of large primary crystal alpha-alumina with the median particle size of D504.0 microns. Wherein the grinding pressure of the jet mill is 0.50 MPa.
Example 2
A preparation method of large primary crystal alpha-alumina comprises the following steps,
step 1: mixing boric acid and calcium carbonate reagent at a ratio of 10:2 for 20min to obtain M1. Wherein, the purity of the boric acid and the calcium carbonate is more than 99 percent.
Step 2: m1 was added to the gamma-alumina raw material at 2% wt and mixed using a mixer for 120min to give M2. Wherein the water content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
And step 3: and calcining the M2 in a high-temperature furnace at 1500 ℃ for 5 hours to obtain M3. Before M2 is placed in a high-temperature furnace, the temperature in the furnace is gradually increased to 1000 ℃, the temperature increasing time is 1.5-2 hours, nitrogen and air are alternately injected into the furnace in the temperature increasing process, the time for single injection of nitrogen or air is 0.5 hour, and the flow is 1-10M3/min。
And 4, step 4: and (3) grinding the M3 in an airflow mill, and matching grading and powder selection with a classifier to obtain the product of large primary crystal alpha-alumina with the median particle size of D505.0 microns. Wherein the grinding pressure of the jet mill is 0.50 MPa.
The particle size detection of the gamma-alumina raw material before calcination and the large primary crystal alpha-alumina after calcination and grinding is carried out, and the results are shown in the attached figures 1 and 2. As can be seen from the figure, the particle size of the gamma-alumina raw material D50 before calcination was 83 μm, and the particle size of the large primary crystal alpha-alumina D50 after calcination and grinding was 5.0. mu.m. Namely, the particle size of the large primary crystal alpha-alumina prepared by the method in the embodiment meets the application requirements in the field of electronic devices.
Example 3
A preparation method of large primary crystal alpha-alumina comprises the following steps,
step 1: mixing boric acid and calcium carbonate reagent at a ratio of 10:2 for 20min to obtain M1, wherein the purity of boric acid and calcium carbonate is more than 99%.
Step 2: m1 was added to the gamma-alumina raw material at 2% wt and mixed using a mixer for 120min to give M2. Wherein the water content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
And step 3: and calcining the M2 in a high-temperature furnace at 1300 ℃ for 5h to obtain M3.
And 4, step 4: and (3) grinding the M3 in an airflow mill, and matching grading and powder selection with a classifier to obtain the product of large primary crystal alpha-alumina with the median particle size of D504.0 microns. Wherein the grinding pressure of the jet mill is 0.50 MPa.
The gamma-alumina raw material before calcination and the large primary crystal alpha-alumina after calcination and grinding are taken to carry out X-ray diffraction detection, and the results are shown in the attached figures 3 and 4. It can be seen from fig. 3 that the diffraction peaks are broad, and the diffraction peaks exist at 67.00, 45.84, 37.59, 39.47 and 19.44 of 2 theta, and are characteristic peaks of gamma-alumina. As can be seen from fig. 4, the diffraction peaks are relatively sharp, and the diffraction peaks exist at 43.36, 35.15, 57.50, 25.58 and 37.78 of 2 θ, and are characteristic peaks of α -alumina. That is, the method in this example will be described as the method in which alumina is changed from the γ phase to the α phase.
Example 4
A preparation method of large primary crystal alpha-alumina comprises the following steps,
step 1: mixing boric acid and calcium carbonate reagent at a ratio of 10:2 for 20min to obtain M1, wherein the purity of boric acid and calcium carbonate is more than 99%.
Step 2: m1 was added at 0.2% wt to the gamma-alumina feedstock and mixed using a blender for 120min to give M2. Wherein the water content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
And step 3: and calcining the M2 in a high-temperature furnace at 1300 ℃ for 5h to obtain M3. Wherein, before M2 is put into a high-temperature furnace, the temperature in the furnace is gradually increased to 1000 ℃ for 1.5-2 hAlternately injecting nitrogen and air into the furnace in the temperature rising process, wherein the time for injecting nitrogen or air once is 0.5h, and the flow is 1-10 m3/min。
And 4, step 4: and (3) grinding the M3 in an airflow mill, and matching grading and powder selection with a classifier to obtain the product large primary crystal alpha-alumina with the median particle size D502.0 mu M. Wherein the grinding pressure of the jet mill is 0.50 MPa.
Example 5
A preparation method of large primary crystal alpha-alumina comprises the following steps,
step 1: mixing boric acid and calcium carbonate reagent at a ratio of 10:1 for 20min to obtain M1, wherein the purity of boric acid and calcium carbonate is more than 99%.
Step 2: m1 was added at 0.2% wt to the gamma-alumina feedstock and mixed using a blender for 120min to give M2. Wherein the water content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
And step 3: and calcining the M2 in a high-temperature furnace at 1500 ℃ for 5 hours to obtain M3. Before M2 is placed in a high-temperature furnace, the temperature in the furnace is gradually increased to 1000 ℃, the temperature increasing time is 1.5-2 hours, nitrogen and air are alternately injected into the furnace in the temperature increasing process, the time for single injection of nitrogen or air is 0.5 hour, and the flow is 1-10M3/min。
And 4, step 4: and (3) grinding the M3 in an airflow mill, and matching grading and powder selection with a classifier to obtain the product large primary crystal alpha-alumina with the median particle size D503.1 mu M. Wherein the grinding pressure of the jet mill is 0.50 MPa.
Example 6
A preparation method of large primary crystal alpha-alumina comprises the following steps,
step 1: mixing boric acid and calcium carbonate reagent at a ratio of 10:2 for 20min to obtain M1. Wherein, the purity of the boric acid and the calcium carbonate is more than 99 percent;
step 2: m1 was added to the gamma-alumina feedstock at 3% wt and mixed using a blender for 120min to give M2. Wherein the water content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
And step 3: and calcining the M2 in a high-temperature furnace at 1500 ℃ for 5 hours to obtain M3. Wherein, before M2 is put into a high-temperature furnace, the temperature in the furnace is gradually increased to 1000 ℃ for a heating time1.5-2 h, alternately injecting nitrogen and air into the furnace in the temperature rising process, wherein the time for injecting nitrogen or air once is 0.5h, and the flow is 1-10 m3/min。
And 4, step 4: and (3) grinding the M3 in an airflow mill, and matching grading and powder selection with a classifier to obtain the product large primary crystal alpha-alumina with the median particle size D505.8 mu M. Wherein the grinding pressure of the jet mill is 0.50 MPa.
Example 7
A preparation method of large primary crystal alpha-alumina comprises the following steps,
step 1: mixing boric acid and calcium carbonate reagent at a ratio of 10:0.1 for 20min to obtain M1. Wherein, the purity of the boric acid and the calcium carbonate is more than 99 percent;
step 2: m1 was added to the gamma-alumina feedstock at 3% wt and mixed using a blender for 100min to give M2. Wherein the water content of the gamma-alumina is less than 3 wt%, and the median particle size is 50-100 μm.
And step 3: and calcining the M2 in a high-temperature furnace at 1500 ℃ for 5 hours to obtain M3. Before M2 is placed in a high-temperature furnace, the temperature in the furnace is gradually increased to 1000 ℃, the temperature increasing time is 1.5-2 hours, nitrogen and air are alternately injected into the furnace in the temperature increasing process, the time for single injection of nitrogen or air is 0.5 hour, and the flow is 1-10M3/min。
And 4, step 4: and (3) grinding the M3 in an airflow mill, and matching grading and powder selection with a classifier to obtain the product large primary crystal alpha-alumina with the median particle size of D505.5 microns. Wherein the grinding pressure of the jet mill is 0.50 MPa.
Claims (8)
1. The preparation method of the large primary crystal alpha-alumina is characterized by comprising the following steps
Step 1, mixing boric acid and a calcium carbonate reagent for 5-40 min according to a weight ratio of 10: 0.1-2 to obtain M1;
step 2, adding M1 into gamma-alumina, and mixing for 5-120 min to obtain M2; wherein the using amount of M1 is 0.2-3% of the weight of gamma-alumina;
step 3, calcining M2 at 1300-1500 ℃ for 2-8 h to obtain M3;
and 4, grinding by using M3 for 1-3 h to obtain the large primary crystal alpha-alumina.
2. The method for preparing large primary crystal alpha-alumina according to claim 1, wherein the purity of boric acid in step 1 is not less than 99%.
3. The method for preparing large primary crystal alpha-alumina according to claim 1, wherein the purity of calcium carbonate in step 1 is not less than 99%.
4. The method for preparing large primary crystal alpha-alumina according to claim 1, wherein in the step 2, the moisture content of the gamma-alumina is less than 3 wt%, and the median particle size is 50 to 100 μm.
5. The method for preparing large primary crystal alpha-alumina according to claim 1, wherein in the step 4, a jet mill is adopted during grinding, and a classifier is matched with the classification powder.
6. The method for preparing large primary crystal alpha-alumina according to claim 5, wherein the pressure of the jet mill is 0.1 to 0.5 MPa.
7. The method of claim 1, wherein in step 3, M2 is washed before calcination.
8. The method for preparing large primary crystal alpha-alumina according to claim 7, wherein the temperature in the furnace is gradually raised to 1000 ℃ for 1.5-2 h during washing, nitrogen and air are alternately injected into the furnace during the temperature raising process, the time for single injection of nitrogen or air is 0.5h, and the flow rate is 1-10 m3/min。
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