CN113264544A - Method for reducing oil absorption value and viscosity of aluminum oxide - Google Patents
Method for reducing oil absorption value and viscosity of aluminum oxide Download PDFInfo
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- CN113264544A CN113264544A CN202110454778.XA CN202110454778A CN113264544A CN 113264544 A CN113264544 A CN 113264544A CN 202110454778 A CN202110454778 A CN 202110454778A CN 113264544 A CN113264544 A CN 113264544A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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Abstract
The invention discloses a method for reducing oil absorption value and viscosity of alumina, which comprises the following steps: s1, mixing alumina and a mineralizer, and then calcining to obtain alumina powder A; s2, mixing the aluminum oxide powder A with a dispersant, niobium oxide and organic alcohol, uniformly stirring, and performing freeze drying and calcination to obtain aluminum oxide powder B; and S3, adding the alumina powder B into organic alcohol, and carrying out jet milling treatment to obtain the finished product alumina micropowder. The method for reducing the oil absorption value and viscosity of the alumina can effectively reduce the oil absorption value and viscosity of the alumina, can reduce the oil absorption value to 16.3g/100g, and can reduce the viscosity to 2210mPa & s.
Description
Technical Field
The invention relates to the technical field of alumina, in particular to a method for reducing oil absorption value and viscosity of alumina.
Background
After high-temperature calcination and grinding classification, the alumina is widely applied to the fields of ceramics, refractory materials, fillers for glass insulators, resin casting fillers and the like.
The dispersive alumina is a special alumina product, can be well dispersed in the amorphous refractory material, and has the effects of good water reducing effect, bleeding prevention, casting material strength improvement and the like. In the prior art, in order to meet the requirement that the castable can achieve more excellent construction and setting properties, an additive is usually added into alumina for treatment, or the adding proportion of dispersible alumina is regulated, but if the alumina obtained by the method is directly used for refractory materials, the filling rate is low due to high oil absorption value, high viscosity and poor dispersion of the alumina, and the refractory properties of the materials are still influenced. Therefore, there is a need to develop a method for reducing the oil absorption value and viscosity of alumina to improve the dispersibility and agglomeration resistance of alumina, so as to improve the filling rate of the refractory material and improve the refractory performance.
Disclosure of Invention
Aiming at the defects of the background art, the invention provides a method for reducing the oil absorption value and viscosity of alumina, which can effectively reduce the oil absorption value and viscosity of the alumina, reduce the oil absorption value to 16.3g/100g and reduce the viscosity to 2210 mPa.
In order to achieve the above purpose, the invention provides the following technical scheme: a method of reducing the oil absorption and viscosity of alumina comprising the steps of:
s1, mixing alumina and a mineralizer, and then calcining to obtain alumina powder A;
s2, mixing the aluminum oxide powder A with a dispersant, niobium oxide and organic alcohol, uniformly stirring, and performing freeze drying and calcination to obtain aluminum oxide powder B;
and S3, adding the alumina powder B into organic alcohol, and carrying out jet milling treatment to obtain the finished product alumina micropowder.
By adopting the scheme, the step S1 adds the mineralizer into the alumina, which is beneficial to reducing the calcining temperature and promoting the alpha-Al2O3Crystal form conversion, promoting the increase of original grain size; step S2, mixing the aluminum oxide powder A with a dispersant, niobium oxide and organic alcohol, uniformly stirring, improving the dispersibility of the aluminum oxide powder A, the dispersant and the niobium oxide after freeze drying, wherein the doped niobium oxide can further promote the growth of aluminum oxide grains to form aluminum oxide with larger original crystal size in the calcining process of the freeze-dried material, and the added dispersant can further improve the dispersibility of the aluminum oxide; and step S3, dispersing the alumina powder B by using an air flow mill, wherein the added organic alcohol can wrap the surface of the alumina powder B to prevent the structure of the alumina powder B from being damaged in the air flow mill process, so that the finished product alumina micropowder which is not easy to agglomerate and has high-efficiency dispersibility is formed by using the air flow mill and the organic alcohol.
Preferably, step S1 is specifically to mix alumina with a mineralizer, and calcine the mixture for 2 to 4 hours at 1200-1400 ℃, so as to obtain alumina powder a, wherein the mineralizer accounts for 0.5 to 1.5% of the mass of the alumina.
Preferably, in step S1, the temperature increase rate during the calcination of the alumina and the mineralizer is 5-10 ℃/min.
By adopting the scheme, the temperature rise rate of the alumina and the mineralizer during calcination is improved, so that the growth of the primary crystal size is promoted.
Preferably, in step S1, the mineralizer is aluminum fluoride, ammonium chloride or a mixture of the two.
Preferably, in step S2, the alumina powder A is 80-85 wt%, the dispersant is 2-10 wt%, the niobium oxide is 0.5-3 wt%, and the organic alcohol is 5-10 wt%.
Preferably, in step S2, the freeze-drying process includes: firstly, pre-freezing at-20 to 0 ℃ for 5 to 10 hours, and then freezing at-60 to-30 ℃ for 5 to 48 hours.
Preferably, in step S2, the dispersant is one or more of sodium pyrophosphate, sodium tripolyphosphate, and sodium hexametaphosphate.
Preferably, in step S2 and step S3, the organic alcohol is one or more of tert-butyl alcohol, propanol and ethanol.
Preferably, in step S3, the temperature of the jet mill is 80-120 ℃, and the treatment time of the jet mill is 1-3 h.
Preferably, in step S3, the organic alcohol is added in an amount of 60 to 80 wt% based on the weight of the alumina powder B.
Compared with the prior art, the invention has the following beneficial effects:
(1) the mineralizer is added into the alumina for calcination, which is beneficial to reducing the calcination temperature and promoting the alpha-Al2O3And crystal form conversion promotes the increase of the original grain size.
(2) The aluminum oxide powder A, the dispersant, the niobium oxide and the organic alcohol are mixed and then uniformly stirred, the dispersibility of the aluminum oxide powder A, the dispersant and the niobium oxide is improved after freeze drying, the doped niobium oxide can further promote the growth of aluminum oxide grains to form aluminum oxide with larger primary crystal size in the calcining process of the freeze-dried material, and the added dispersant can further improve the dispersibility of the aluminum oxide.
(3) The alumina powder B is dispersed by the jet mill, and the added organic alcohol can wrap the surface of the alumina powder B to prevent the structure of the alumina powder B from being damaged in the jet mill process, so that finished alumina micropowder which is not easy to agglomerate and has high-efficiency dispersibility is formed by the jet mill and the organic alcohol.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The invention provides a method for reducing oil absorption value and viscosity of alumina, which comprises the following steps:
s1, mixing alumina and a mineralizer, and then calcining to obtain alumina powder A;
s2, mixing the aluminum oxide powder A with a dispersant, niobium oxide and organic alcohol, uniformly stirring, and performing freeze drying and calcination to obtain aluminum oxide powder B;
and S3, adding the alumina powder B into organic alcohol, and carrying out jet milling treatment to obtain the finished product alumina micropowder.
Step S1 is specifically to mix alumina and a mineralizer and calcine the mixture for 2 to 4 hours at the temperature of 1200 ℃ and 1400 ℃ to obtain alumina powder A, wherein the mineralizer accounts for 0.5 to 1.5 percent of the mass of the alumina.
In step S1, the temperature rise rate during the calcination of the alumina and the mineralizer is 5-10 ℃/min.
In step S1, the mineralizer is aluminum fluoride, ammonium chloride, or a mixture of both.
In step S2, the alumina powder A accounts for 80-85 wt%, the dispersant accounts for 2-10 wt%, the niobium oxide accounts for 0.5-3 wt%, and the organic alcohol accounts for 5-10 wt%.
In step S2, the freeze-drying process includes: firstly, pre-freezing at-20 to 0 ℃ for 5 to 10 hours, and then freezing at-60 to-30 ℃ for 5 to 48 hours.
In step S2, the dispersant is one or more of sodium pyrophosphate, sodium tripolyphosphate, and sodium hexametaphosphate.
In step S2 and step S3, the organic alcohol is one or more of tert-butyl alcohol, propanol, and ethanol.
In step S3, the temperature of the jet mill is 80-120 ℃, and the processing time of the jet mill is 1-3 h.
In step S3, the organic alcohol is added in an amount of 60 to 80 wt% based on the weight of the alumina powder B.
Example 1
The invention provides a method for reducing oil absorption value and viscosity of alumina, which comprises the following steps:
s1, mixing alumina and a mineralizer, and then calcining to obtain alumina powder A;
s2, mixing the aluminum oxide powder A with a dispersant, niobium oxide and organic alcohol, uniformly stirring, and performing freeze drying and calcination to obtain aluminum oxide powder B;
and S3, adding the alumina powder B into organic alcohol, and carrying out jet milling treatment to obtain the finished product alumina micropowder.
In this embodiment, step S1 specifically includes mixing alumina and a mineralizer, and calcining at 1200 ℃ for 4h to obtain alumina powder a, where the mineralizer is 0.5% of the mass of the alumina, the mineralizer is aluminum fluoride, the amount of alumina added is 100g, and the amount of aluminum fluoride added is 0.5 g.
In this example, in step S1, the temperature increase rate at the time of calcining alumina and mineralizer is 5 ℃/min.
In this example, in step S2, the alumina powder a was 80 wt%, the dispersant was 10 wt%, the niobium oxide was 3 wt%, the organic alcohol was 7 wt%, the dispersant was sodium pyrophosphate, the organic alcohol was t-butanol, the amount of alumina powder a added was 80g, the amount of sodium pyrophosphate added was 10g, the amount of niobium oxide added was 3g, and the amount of t-butanol added was 7 g.
In this embodiment, in step S2, the freeze-drying process includes: firstly, pre-freezing at-20 ℃ for 5h, and then freezing at-60 ℃ for 5 h.
In this embodiment, in step S3, the temperature of the jet mill is 80 ℃, and the processing time of the jet mill is 3 h.
In this example, in step S3, the organic alcohol was added in an amount of 60 wt% based on the weight of alumina powder B, the organic alcohol was t-butanol, the alumina powder B was added in an amount of 50g, and the t-butanol was added in an amount of 30 g.
Example 2
The procedure is as in example 1, except that:
in this embodiment, step S1 specifically includes mixing alumina and a mineralizer, and calcining at 1300 ℃ for 3h to obtain alumina powder a, where the mineralizer is 1.0% of the mass of the alumina, the mineralizer is ammonium chloride, the amount of alumina added is 100g, and the amount of mineralizer added is 1.0 g.
In this example, in step S1, the temperature increase rate at the time of calcining alumina and mineralizer was 7 ℃/min.
In this example, in step S2, the alumina powder a was 85 wt%, the dispersant was 8 wt%, the niobium oxide was 2 wt%, the organic alcohol was 5 wt%, the dispersant was sodium tripolyphosphate, the organic alcohol was propanol, the alumina powder a was 85g, the sodium tripolyphosphate was 8g, the niobium oxide was 2g, and the propanol was 5 g.
In this embodiment, in step S2, the freeze-drying process includes: firstly, pre-freezing at-10 ℃ for 7h, and then freezing at-30 ℃ for 48 h.
In this embodiment, in step S3, the temperature of the jet mill is 100 ℃, and the processing time of the jet mill is 2 h.
In this example, in step S3, the organic alcohol was added in an amount of 70 wt% based on the weight of alumina powder B, the organic alcohol was propanol, the alumina powder B was added in an amount of 50g, and the propanol was added in an amount of 35 g.
Example 3
The procedure is as in example 1, except that:
in this embodiment, step S1 specifically includes mixing alumina and a mineralizer, and calcining at 1300 ℃ for 3h to obtain alumina powder a, where the mineralizer accounts for 1.5% of the mass of the alumina, the mineralizer is a mixture of ammonium fluoride and ammonium chloride, the addition amount of the alumina is 100g, and the addition amounts of the ammonium fluoride and the ammonium chloride are both 0.75 g.
In this example, in step S1, the temperature increase rate at the time of calcining alumina and mineralizer was 8 ℃/min.
In this example, in step S2, alumina powder a was 80 wt%, dispersant was 8 wt%, niobium oxide was 2 wt%, organic alcohol was 10 wt%, dispersant was sodium hexametaphosphate, organic alcohol was ethanol and propanol, alumina powder a was added in an amount of 80g, sodium hexametaphosphate was added in an amount of 8g, niobium oxide was added in an amount of 2g, and organic alcohol was added in an amount of 10 g.
In this embodiment, in step S2, the freeze-drying process includes: the method comprises the steps of pre-freezing at 0 ℃ for 10 hours, and then freezing at-50 ℃ for 48 hours.
In this embodiment, in step S3, the temperature of the jet mill is 120 ℃, and the processing time of the jet mill is 3 h.
In this example, in step S3, the organic alcohol was added in an amount of 70 wt% based on the alumina powder B, the organic alcohol was a mixture of ethanol and propanol, the alumina powder B was added in an amount of 50g, the ethanol was added in an amount of 17.5g, and the propanol was added in an amount of 17.5 g.
Example 4
The procedure is as in example 1, except that:
in this embodiment, step S1 specifically includes mixing alumina and a mineralizer, and calcining at 1400 ℃ for 2h to obtain alumina powder a, where the mineralizer is 1.2% of the mass of the alumina, the mineralizer is ammonium chloride, the amount of alumina added is 100g, and the amount of ammonium chloride added is 1.2 g.
In this example, in step S1, the temperature increase rate at the time of calcining alumina and mineralizer is 10 ℃/min.
In this example, in step S2, alumina powder a was 85 wt%, dispersant was 5 wt%, niobium oxide was 0.5 wt%, organic alcohol was 9.5 wt%, dispersant was a mixture of sodium tripolyphosphate and sodium hexametaphosphate, organic alcohol was ethanol, alumina powder a was added in an amount of 85g, sodium tripolyphosphate and sodium hexametaphosphate were each added in an amount of 2.5g, niobium oxide was added in an amount of 0.5g, and ethanol was added in an amount of 9.5 g.
In this embodiment, in step S2, the freeze-drying process includes: the method comprises the steps of pre-freezing at 0 ℃ for 10 hours, and then freezing at-40 ℃ for 24 hours.
In this embodiment, in step S3, the temperature of the jet mill is 120 ℃, and the processing time of the jet mill is 1 h.
In this example, in step S3, the organic alcohol was added in an amount of 80 wt% based on the weight of alumina powder B, the organic alcohol was ethanol, the alumina powder B was added in an amount of 50g, and the ethanol was added in an amount of 40 g.
Comparative example 1
Specifically, the only difference from example 1 is that in step S2, alumina powder a was mixed with a dispersant, niobium oxide, and an organic alcohol, and then uniformly stirred, dried at 120 ℃ for 3 hours, and calcined to obtain alumina powder B.
Comparative example 2
Specifically, the only difference from example 2 is that in step S2, alumina powder a was mixed with a dispersant, niobium oxide, and an organic alcohol, and then uniformly stirred, dried at 120 ℃ for 3 hours, and calcined to obtain alumina powder B.
Comparative example 3
Specifically, the only difference from example 3 is that in step S2, alumina powder a was mixed with a dispersant, niobium oxide, and an organic alcohol, and then stirred uniformly, dried at 120 ℃ for 3 hours, and calcined to obtain alumina powder B.
Comparative example 4
Specifically, the only difference from example 4 is that in step S2, alumina powder a was mixed with a dispersant, niobium oxide, and an organic alcohol, and then uniformly stirred, dried at 120 ℃ for 3 hours, and calcined to obtain alumina powder B.
Comparative example 5
Specifically, the present embodiment is different from embodiment 1 only in that the processing of step S1 is not performed.
Comparative example 6
Specifically, the present embodiment is different from embodiment 2 only in that the processing of step S1 is not performed.
Comparative example 7
Specifically, the present embodiment is different from embodiment 3 only in that the processing of step S1 is not performed.
Comparative example 8
Specifically, the present embodiment is different from embodiment 4 only in that the processing of step S1 is not performed.
Comparative example 9
Alumina without any treatment.
And (3) testing an oil absorption value: weighing 5g of sample to be detected, placing the sample in a porcelain plate, dropwise adding dioctyl phthalate (DOP) by using a micro burette, continuously turning and grinding by using a scraper, wherein the sample to be detected is in a dispersion state before the DOP is dropwise added, and then is gradually wetted by the DOP, and the DOP consumption is calculated according to the following formula (1):
X＝(m1/m)×100 (1)
in the formula (1), X represents the mass of DOP absorbed per 100g of the sample to be tested, and m1Represents the mass of DOP consumed, and m represents the mass of the sample to be tested.
And (3) viscosity testing: mixing vinyl silicone oil, hydrogen-containing silicone oil and a sample to be detected, fully stirring, defoaming, and measuring by using a rotational viscometer at 25 ℃, wherein 100 parts of the vinyl silicone oil, 5.5 parts of the hydrogen-containing silicone oil and a proper amount of the sample to be detected are taken.
Test example 1
The samples prepared in examples 1 to 4 and comparative examples 1 to 9 were subjected to the oil absorption value test and the viscosity test, and the specific results are shown in table 1.
TABLE 1 oil absorption and viscosity of samples prepared in examples 1-4 and comparative examples 1-9
| Test examples | Oil absorption number (g/100g) | Viscosity (mPa. s) |
| Example 1 | 19.2 | 3700 |
| Comparative example 1 | 22.3 | 6420 |
| Comparative example 5 | 19.7 | 5610 |
| Example 2 | 17.9 | 3260 |
| Comparative example 2 | 20.5 | 6300 |
| Comparative example 6 | 18.8 | 5030 |
| Example 3 | 16.3 | 2210 |
| Comparative example 3 | 19.2 | 5300 |
| Comparative example 7 | 17.5 | 4410 |
| Example 4 | 18.1 | 3550 |
| Comparative example 4 | 20.8 | 6460 |
| Comparative example 8 | 19.3 | 5410 |
| Comparative example 9 | 23.9 | 7200 |
As can be seen from table 1, the oil absorption value and viscosity of the finished alumina micro powders prepared in examples 1 to 4 are significantly lower than those of the finished alumina micro powders prepared in corresponding comparative examples 1 to 4, because in step S2, the dispersibility of the alumina powder a, the dispersant and the niobium oxide is improved by freeze-drying, and in the process of calcining the freeze-dried material, the doped niobium oxide can promote the growth of alumina grains to form alumina with a larger primary crystal size, and the dispersant added can effectively improve the dispersibility of the alumina, so that the finished alumina micro powders prepared in examples 1 to 4 are not easy to agglomerate and have a good dispersing effect.
The finished alumina fine powders prepared in examples 1 to 4 had significantly lower oil absorption values and viscosities than those of comparative examples 5 to 6, because the finished alumina fine powders prepared in examples 1 to 4 were calcined after mixing alumina with a mineralizer, which was added to facilitate lowering the calcination temperature and promoting the promotion of α -Al, in step S12O3The crystal transformation promotes the increase of the original grain size, thereby reducing the oil absorption value and the viscosity of the finished product of the alumina micro powder prepared in the examples 1 to 4.
Compared with comparative example 9, the oil absorption value and viscosity of the finished alumina micro powder prepared in examples 1 to 4 are lower, which shows that the oil absorption value and viscosity of the alumina can be effectively reduced by using the treatment method of the invention. Wherein the finished alumina micropowder prepared in example 3 had the smallest oil absorption and viscosity, the oil absorption was 16.3g/100g, and the viscosity was 2210mPa · s.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A method for reducing oil absorption and viscosity of alumina, comprising the steps of:
s1, mixing alumina and a mineralizer, and then calcining to obtain alumina powder A;
s2, mixing the aluminum oxide powder A with a dispersant, niobium oxide and organic alcohol, uniformly stirring, and performing freeze drying and calcination to obtain aluminum oxide powder B;
and S3, adding the alumina powder B into organic alcohol, and carrying out jet milling treatment to obtain the finished product alumina micropowder.
2. The method as claimed in claim 1, wherein the step S1 is specifically that the alumina is mixed with a mineralizer and then calcined at 1200-1400 ℃ for 2-4h to obtain the alumina powder a, wherein the mineralizer is 0.5-1.5% of the mass of the alumina.
3. The method of claim 2, wherein the heating rate of the alumina and mineralizer calcination in step S1 is 5-10 ℃/min.
4. The method of claim 2, wherein in step S1, the mineralizer is aluminum fluoride, ammonium chloride, or a mixture thereof.
5. The method of claim 1, wherein in step S2, the alumina powder a is 80-85 wt%, the dispersant is 2-10 wt%, the niobium oxide is 0.5-3 wt%, and the organic alcohol is 5-10 wt%.
6. The method of claim 1, wherein the step of freeze-drying in step S2 comprises: firstly, pre-freezing at-20 to 0 ℃ for 5 to 10 hours, and then freezing at-60 to-30 ℃ for 5 to 48 hours.
7. The method of claim 1, wherein in step S2, the dispersant is one or more selected from sodium pyrophosphate, sodium tripolyphosphate and sodium hexametaphosphate.
8. The method for reducing the oil absorption value and viscosity of the alumina according to claim 1, wherein in the step S2 and the step S3, the organic alcohol is one or more of tert-butyl alcohol, propanol and ethanol.
9. The method of claim 1, wherein the jet mill temperature is 80-120 ℃ and the jet mill treatment time is 1-3h in step S3.
10. The method of claim 1, wherein the organic alcohol is added in an amount of 60-80 wt% based on the weight of the alumina powder B in step S3.
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