CN114394820B - Magnesia-alumina spinel sintered by waste magnesia-alumina brick powder and preparation method thereof - Google Patents
Magnesia-alumina spinel sintered by waste magnesia-alumina brick powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a magnesia-alumina spinel sintered by waste magnesia-alumina brick powder and a preparation method thereof. To produce Al 2 O 3 The magnesia-alumina spinel with the mass percentage content of 60-70 percent is taken as a reference, and the magnesia-alumina spinel consists of 30-50 percent of raw material waste magnesia-alumina brick powder, 50-65 percent of industrial alumina powder and 0-5 percent of raw alumina powder. Firstly, weighing various raw materials according to the raw material proportion of the magnesium aluminate spinel, and then mixing and co-grinding the raw materials to obtain a mixed and ground fine material; putting the obtained mixed and ground fine powder into a mould to be molded into a mixed blank; finally, sintering is carried out, and cooling is carried out after sintering to obtain the solid magnesia-alumina spinel. According to the invention, by regulating and controlling the proportion and the firing temperature of different waste magnesia-alumina brick powder, industrial alumina and raw alumina powder, the production cost is reduced while the thermal shock stability, erosion resistance and other performances are ensured, an efficient method is provided for recycling waste magnesia-alumina bricks, and the method is beneficial to environmental protection. Therefore, the method has remarkable economic benefit and social benefit.
Description
1. The technical field is as follows:
the invention belongs to the technical field of refractory materials, and particularly relates to magnesia-alumina spinel sintered by waste magnesia-alumina brick powder and a preparation method thereof.
2. The background art comprises the following steps:
the magnesia-alumina spinel has the characteristics of high temperature resistance, small thermal expansion coefficient, good thermal stability, strong slag resistance and the like, is a high-quality refractory raw material, and is widely applied to the fields of steel smelting, cement rotary kilns, glass industrial kilns and the like. However, the natural magnesium aluminate spinel has limited resources and generally meets the industrial requirements through a manual synthesis method, and the synthesis method of the magnesium aluminate spinel mainly comprises a solid-phase sintering method, a melting method, a coprecipitation method, a drying and washing method, a high-temperature atomization method and the like. Wherein the solid-phase sintering method is a method for synthesizing powder in a solid-state mode, and has the characteristics of simple and easy process and easy large-scale production; the synthetic raw materials are generally selected from high-quality magnesite, high-alumina bauxite and industrial alumina, and the production cost is high. The invention researches a method for synthesizing high-added-value magnesia-alumina spinel raw material by using low-cost waste magnesia-alumina brick powder as raw material.
3. The invention content is as follows:
the technical problem to be solved by the invention is as follows: in order to overcome the technical problems of high power consumption and high cost of the existing synthesis process of magnesia-alumina spinel, the invention provides magnesia-alumina spinel sintered by waste magnesia-alumina brick powder and a preparation method thereof.
In order to solve the problems, the invention adopts the technical scheme that:
the invention provides a magnesia-alumina spinel sintered by waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesium aluminate spinel with the mass percentage of 60-70 percent is taken as a reference, and the magnesium aluminate spinel is prepared from raw materials30 to 50 weight percent of waste magnesia-alumina brick powder, 50 to 65 weight percent of industrial alumina powder and 0 to 5 weight percent of raw alumina powder.
According to the magnesia-alumina spinel sintered by the waste magnesia-alumina brick powder, in the waste magnesia-alumina brick powder, the mass percentage of MgO is 79-89%, and Al is 2 O 3 The mass percentage content of the compound is 10-20%.
According to the magnesia-alumina spinel sintered by using the waste magnesia-alumina brick powder, al in the industrial alumina powder 2 O 3 The mass percentage content of the compound is more than or equal to 96 percent.
According to the magnesia-alumina spinel sintered by the waste magnesia-alumina brick powder, al in the raw bauxite powder 2 O 3 70-80% of Fe 2 O 3 The mass percentage of SiO is less than or equal to 1 percent 2 The mass percentage content is less than or equal to 6 percent, and the ignition loss is 15 percent.
According to the magnesia-alumina spinel sintered and combined by the waste magnesia-alumina brick powder, the particle size of the waste magnesia-alumina brick powder is less than or equal to 1mm, the particle size of the industrial alumina powder is 325 meshes, and the particle size of the raw bauxite powder is 325 meshes.
In addition, a preparation method of the magnesium aluminate spinel is provided, and the preparation method comprises the following steps:
a. firstly, weighing various raw materials according to the raw material proportion of the magnesia-alumina spinel;
b. mixing and co-grinding the weighed raw materials by a ball mill, wherein the rotating speed of the ball mill is 1000-1200 r/min, the co-grinding time is 8-12 h, and the mixed-ground fine materials with the granularity of less than or equal to 325 meshes are obtained after co-grinding;
c. and c, placing the mixed and ground fine powder obtained in the step b into a mold, slightly pressing the mixed and ground fine powder into a mixed blank, then sintering the mixed blank by adopting a tunnel kiln at the sintering temperature of 1500-1600 ℃ for 6 hours, and cooling the sintered mixed blank to obtain the solid magnesia-alumina spinel.
According to the preparation method of the magnesium aluminate spinel, in the step c, the pressure is controlled to be 50-75 MPa in the light pressure forming process;
according to the preparation method of the magnesia-alumina spinel, al in the solid magnesia-alumina spinel is obtained 2 O 3 60-70 wt%, mgO 28-38 wt%, siO 2 The content of the compound is less than or equal to 1wt percent, and the content of other impurities is less than or equal to 1 percent; the water absorption rate of the obtained product solid magnesium aluminate spinel is less than or equal to 3 percent, and the volume density is more than or equal to 2.80g/cm 3 。
The invention has the following positive beneficial effects:
1. the solid magnesium aluminate spinel is prepared by using waste magnesium aluminate brick powder, industrial alumina and raw alumina powder as raw materials, co-grinding the waste magnesium aluminate brick, the industrial alumina and the raw alumina powder, forming and then sintering in a tunnel kiln. The magnesia-alumina spinel in the waste magnesia-alumina brick powder provides a growth source for the growth of magnesia-alumina spinel crystals in the sintering process, and can enable magnesium oxide and aluminum oxide to be adhered and reacted on spinel to form magnesia-alumina spinel. In addition, the introduction of the raw alumina plays a good role in promoting sintering and ensures the higher volume density of the prepared magnesia-alumina spinel. According to the technical scheme, the proportion and the firing temperature of different waste magnesia-alumina brick powder, industrial alumina and raw alumina powder are regulated, so that the production cost is reduced while the performances such as thermal shock stability, erosion resistance and the like are ensured, an efficient method is provided for secondary recycling of waste magnesia-alumina bricks, and the method is beneficial to environmental protection.
2. In the solid magnesia-alumina spinel prepared by the technical scheme of the invention, al 2 O 3 60-70% of (A), 28-38% of MgO and SiO 2 The content of (A) is less than or equal to 1 percent; the content of other impurities is less than or equal to 1 percent, the water absorption rate of the obtained product solid magnesium aluminate spinel is less than or equal to 3 percent, and the volume density is more than or equal to 2.80g/cm 3 。
In conclusion, the invention has obvious economic benefit and social benefit.
4. The specific implementation mode is as follows:
the invention is further illustrated by the following examples, which do not limit the scope of the invention.
In the following examples, the particle size of the used waste magnesia-alumina brick powder is less than or equal to 1mm, the particle size of the industrial alumina powder is 325 meshes, and the particle size of the raw bauxite powder is 325 meshes.
In the adopted waste magnesia-alumina brick powder, the mass percentage of MgO is79 to 89 percent of Al 2 O 3 The mass percentage content of the compound is 10 to 20 percent; al in the industrial alumina powder 2 O 3 The mass percentage content of the compound is more than or equal to 96 percent; in the raw bauxite powder, al 2 O 3 70-80% of Fe 2 O 3 Mass percent of less than or equal to 1 percent, siO 2 The mass percentage content is less than or equal to 6 percent, and the ignition loss is 15 percent.
Example 1:
the invention utilizes the magnesia-alumina spinel formed by burning and combining waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesia-alumina spinel with the mass percentage of 60 percent is taken as a reference, and the magnesia-alumina spinel is composed of 30 percent by weight of raw material waste magnesia-alumina brick powder (the mass percentage of alumina in the waste magnesia-alumina brick powder is 10 percent) and 57 percent by weight of industrial alumina powder.
Example 2:
the preparation method of the magnesium aluminate spinel disclosed by the embodiment 1 of the invention comprises the following detailed steps:
a. firstly, weighing various raw materials according to the raw material proportion of the magnesium aluminate spinel in the embodiment 1;
b. mixing and co-grinding the weighed raw materials by a ball mill, wherein the rotating speed of the ball mill is 1200r/min, the co-grinding time is 12h, and the mixed and ground fine material with the granularity of less than or equal to 325 meshes is obtained after co-grinding;
c. and c, placing the mixed and ground fine powder obtained in the step b into a mold, slightly pressing the mixed and ground fine powder under 65MPa to form a mixed blank, then sintering the mixed blank by adopting a tunnel kiln, keeping the temperature for 6 hours at 1550 ℃, and cooling the sintered mixed and ground fine powder to obtain the solid magnesium aluminate spinel.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 1.
TABLE 1 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption Rate% |
| 2.93 | 61.47 | 37.74 | 1.15 | 2.8 |
Example 3:
the invention utilizes the magnesia-alumina spinel formed by burning and combining waste magnesia-alumina brick powder to prepare Al 2 O 3 On the basis of the magnesia-alumina spinel with the mass percentage of 60 percent, the magnesia-alumina spinel consists of 40 percent by weight of raw material waste magnesia-alumina brick powder (the mass percentage of alumina in the waste magnesia-alumina brick powder is 10 percent) and 56 percent by weight of industrial alumina powder.
Example 4:
the preparation method of the magnesium aluminate spinel disclosed in the embodiment 3 of the invention is the same as that of the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 2.
TABLE 2 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 2.92 | 60.57 | 38 | 0.45 | 2.7 |
Example 5:
the invention utilizes the magnesia-alumina spinel sintered by waste magnesia-alumina brick powder to prepare Al 2 O 3 On the basis of the magnesia-alumina spinel with the mass percentage of 60 percent, the magnesia-alumina spinel consists of 50 weight percent of raw material waste magnesia-alumina brick powder (the mass percentage of alumina in the waste magnesia-alumina brick powder is 10 percent) and 55 weight percent of industrial alumina powder.
Example 6:
the preparation method of the magnesium aluminate spinel disclosed by the invention in the embodiment 5 is the same as that in the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment on the detection of the relevant properties are detailed in table 3.
TABLE 3 data of the solid magnesium aluminate spinel prepared in this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption Rate% |
| 2.8 | 61.83 | 37.01 | 0.39 | 2.7 |
Example 7:
the invention utilizes the magnesia-alumina spinel formed by burning and combining waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesia-alumina spinel with the mass percentage of 60 percent is taken as a reference, and the magnesia-alumina spinel is composed of 35 percent by weight of raw material waste magnesia-alumina brick powder (the mass percentage of alumina in the waste magnesia-alumina brick powder is 15 percent) and 55 percent by weight of industrial alumina powder.
Example 8:
the preparation method of the magnesium aluminate spinel disclosed in the embodiment 7 of the invention is the same as that of the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment on the detection of the relevant properties are detailed in table 4.
TABLE 4 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 2.96 | 60.88 | 37.68 | 0.66 | 2.9 |
Example 9:
the invention utilizes the magnesia-alumina spinel sintered by waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesium aluminate spinel with the mass percentage of 65 percent is taken as a reference, and the magnesium aluminate spinel is composed of 40wt percent of raw material waste magnesium aluminate brick powder (the mass percentage of alumina in the waste magnesium aluminate brick powder is 15 percent) and 59wt percent of industrial alumina powder.
Example 10:
the preparation method of the magnesium aluminate spinel disclosed by the embodiment 9 of the invention is the same as that of the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 5.
TABLE 5 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption Rate% |
| 2.93 | 65.24 | 34.06 | 0.51 | 3.0 |
Example 11:
the invention utilizes the magnesia-alumina spinel sintered by waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesium aluminate spinel with the mass percentage of 65 percent is taken as a reference, and the magnesium aluminate spinel is composed of 50 percent by weight of raw material waste magnesium aluminate brick powder (the mass percentage of alumina in the waste magnesium aluminate brick powder is 10 percent) and 60 percent by weight of industrial alumina powder.
Example 12:
the preparation method of the magnesium aluminate spinel disclosed by the invention in the embodiment 11 is the same as that in the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment on the detection of the relevant properties are detailed in table 6.
TABLE 6 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 2.80 | 65.23 | 33.29 | 0.51 | 2.8 |
Example 13:
the invention utilizes the magnesia-alumina spinel sintered by waste magnesia-alumina brick powder to prepare Al 2 O 3 Based on 70% of magnesia-alumina spinel by mass, the magnesia-alumina spinel is composed of 50wt% of raw material waste magnesia-alumina brick powder (the mass percentage of alumina in the waste magnesia-alumina brick powder is 10%) and 65wt% of industrial alumina powder.
Example 14:
the preparation method of the magnesium aluminate spinel disclosed by the invention in the embodiment 13 is the same as that of the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 7.
TABLE 7 data of the solid magnesium aluminate spinel prepared by this example
| Bulk densityg/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 2.96 | 69.59 | 28.85 | 0.68 | 2.7 |
Example 15:
the invention utilizes the magnesia-alumina spinel formed by burning and combining waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesia-alumina spinel with the mass percentage of 70 percent is taken as a reference, and the magnesia-alumina spinel is composed of 50 percent by weight of raw material waste magnesia-alumina brick powder (the mass percentage of alumina in the waste magnesia-alumina brick powder is 20 percent) and 50 percent by weight of industrial alumina powder.
Example 16:
the preparation method of the magnesium aluminate spinel disclosed by the invention in the embodiment 15 is the same as that of the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 8.
TABLE 8 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 2.97 | 70.02 | 28.00 | 1.00 | 2.9 |
Example 17:
the invention utilizes the magnesia-alumina spinel formed by burning and combining waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesia-alumina spinel with the mass percentage of 70 percent is taken as a reference, and the magnesia-alumina spinel comprises 30 weight percent of raw material waste magnesia-alumina brick powder (the mass percentage of alumina in the waste magnesia-alumina brick powder is 10 percent), 63 weight percent of industrial alumina powder and 5 weight percent of raw alumina powder (the mass percentage of alumina in the raw alumina powder is 80 percent).
Example 18:
the preparation method of the magnesium aluminate spinel disclosed by the invention in the embodiment 17 is the same as that in the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 9.
TABLE 9 data of the solid magnesium aluminate spinel prepared in this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption Rate% |
| 3.03 | 70.10 | 28.06 | 1.09 | 2.9 |
Example 19:
the invention utilizes the magnesia-alumina spinel formed by burning and combining waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesium aluminate spinel with the mass percentage of 65% is taken as a reference, and the magnesium aluminate spinel is composed of 30wt% of raw material waste magnesium aluminate brick powder (the mass percentage of alumina in the waste magnesium aluminate brick powder is 15%), 60wt% of industrial alumina powder and 1wt% of raw alumina powder (the mass percentage of alumina in the raw alumina powder is 70%).
Example 20:
the preparation method of the magnesium aluminate spinel used in the embodiment 19 of the invention is the same as that of the embodiment 2.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 10.
TABLE 10 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 3.01 | 64.59 | 34.11 | 0.47 | 2.8 |
Example 21:
the invention utilizes the magnesia-alumina spinel sintered by waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesium aluminate spinel with the mass percentage of 65 percent is taken as a reference, and the magnesium aluminate spinel is composed of 35wt percent of raw material waste magnesium aluminate brick powder (the mass percentage of alumina in the waste magnesium aluminate brick powder is 20 percent) and 58wt percent of industrial alumina powder.
Example 22:
the preparation method of the magnesium aluminate spinel of the embodiment 21 of the invention is basically the same as the embodiment 2, except that:
in the step c: the sintering temperature is 1500 ℃, and the heat preservation time is 6h.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 11.
TABLE 11 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 2.80 | 65.23 | 33.29 | 0.51 | 2.8 |
Example 23:
the invention utilizes the magnesia-alumina spinel formed by burning and combining waste magnesia-alumina brick powder to prepare Al 2 O 3 The magnesium aluminate spinel with the mass percentage of 65 percent is taken as a reference, and the magnesium aluminate spinel is composed of 40wt percent of raw material waste magnesium aluminate brick powder (the mass percentage of alumina in the waste magnesium aluminate brick powder is 15 percent) and 59wt percent of industrial alumina powder.
Example 24:
the preparation method of the magnesium aluminate spinel disclosed in the embodiment 23 of the invention is basically the same as the preparation method of the embodiment 2, except that:
in the step c: the firing temperature is 1600 ℃, and the heat preservation time is 6h.
The data of the solid magnesium aluminate spinel prepared by the embodiment for detecting the relevant properties are detailed in table 12.
TABLE 12 data of the solid magnesium aluminate spinel prepared by this example
| Bulk density g/cm 3 | Al 2 O 3 ％ | MgO％ | SiO 2 ％ | Water absorption% |
| 3.01 | 65.56 | 32.71 | 0.82 | 2.7 |
。
Claims (4)
1. A method for synthesizing magnesia-alumina spinel by sintering waste magnesia-alumina brick powder is characterized in that: to produce Al 2 O 3 Taking magnesium aluminate spinel with the mass percentage content of 60-70% as a reference, wherein the magnesium aluminate spinel consists of 30-50 wt% of raw material waste magnesium aluminum brick powder, 50-65 wt% of industrial alumina powder and 0-5 wt% of raw alumina powder;
in the waste magnesium aluminum brick powder, the mass percentage of MgO is 79-89%, and Al is 2 O 3 The mass percentage content of the compound is 10 to 20 percent; in the raw bauxite powder, al 2 O 3 70-80% of Fe 2 O 3 The mass percentage of SiO is less than or equal to 1 percent 2 The mass percentage content is less than or equal to 6 percent, and the ignition loss is 15 percent; the granularity of the waste magnesia-alumina brick powder is less than or equal to 1mm, the granularity of the industrial alumina powder is 325 meshes, and the granularity of the raw bauxite powder is 325 meshes;
the synthesis method comprises the following steps:
a. firstly, weighing various raw materials according to the raw material proportion of the magnesium aluminate spinel;
b. mixing and co-grinding the weighed raw materials by a ball mill, wherein the rotating speed of the ball mill is 1000-1200 r/min, the co-grinding time is 8-12 h, and the mixed-ground fine materials with the granularity of less than or equal to 325 meshes are obtained after co-grinding;
c. and c, placing the mixed and ground fine powder obtained in the step b into a mold, slightly pressing the mixed and ground fine powder into a mixed blank, then sintering the mixed blank by adopting a tunnel kiln at the sintering temperature of 1500-1600 ℃ for 6 hours, and cooling the sintered mixed blank to obtain the solid magnesia-alumina spinel.
2. The method for synthesizing magnesia-alumina spinel by sintering waste magnesia-alumina brick powder according to claim 1, is characterized in that: al in the industrial alumina powder 2 O 3 The mass percentage content of the compound is more than or equal to 96 percent.
3. The method for synthesizing magnesia-alumina spinel by sintering waste magnesia-alumina brick powder according to claim 1, is characterized in that: c, controlling the pressure to be 50-75 MPa in the light pressure forming process;
4. the method for synthesizing magnesia-alumina spinel by sintering waste magnesia-alumina brick powder according to claim 1, which is characterized in that: in the solid magnesium aluminate spinel, al is contained in the product 2 O 3 60-70 wt%, mgO 28-38 wt%, siO 2 The content of the compound is less than or equal to 1wt percent, and the content of other impurities is less than or equal to 1 percent; the water absorption rate of the obtained solid magnesia-alumina spinel is less than or equal to 3 percent, and the volume density is more than or equal to 2.80g/cm 3 。
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