CN112194473B - Chrome corundum brick with high erosion resistance and thermal shock resistance prepared by secondary mixed grinding and drying and process thereof - Google Patents

Chrome corundum brick with high erosion resistance and thermal shock resistance prepared by secondary mixed grinding and drying and process thereof Download PDF

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CN112194473B
CN112194473B CN202010602427.4A CN202010602427A CN112194473B CN 112194473 B CN112194473 B CN 112194473B CN 202010602427 A CN202010602427 A CN 202010602427A CN 112194473 B CN112194473 B CN 112194473B
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powder
drying
grinding
granularity
chromium
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CN112194473A (en
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陈松林
王俊涛
吴跃峰
袁林
钱蛇大
俞永平
吴忠阳
张伯南
闫昕
孙旭东
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Ruitai Technology Co ltd
Yixing Ruitai Refractory Material Co ltd
China Building Materials Academy CBMA
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Ruitai Technology Co ltd
Yixing Ruitai Refractory Material Co ltd
China Building Materials Academy CBMA
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Abstract

The invention relates to a method for preparing high erosion resistance and high thermal shock resistance chromium corundum brick by secondary mixed grinding and drying and a process thereof2And (3) coating the pretreated granular material with a chromium sand granular structure with powder. And then carrying out secondary mixing and grinding on the modified particle material, the modified powder material and the binding agent, ageing the mixture, forming and drying the mixture for the second time, oxidizing the thermosetting resin into gas to escape during sintering, leaving a coated particle structure with various hole defects, and toughening the mixture through the pore defects and the zirconia phase change to obtain the refractory material with high erosion resistance and high thermal shock resistance. Compared with the original high-chromium brick, the chromium corundum brick has equivalent erosion resistance, and the water quenching cycle times of the thermal shock resistance at 1100 ℃ are improved to more than 6 times from the original 1-2 times.

Description

Chrome corundum brick with high erosion resistance and thermal shock resistance prepared by secondary mixed grinding and drying and process thereof
Technical Field
The invention relates to a chrome corundum brick with high erosion resistance and high thermal shock resistance prepared by secondary mixed grinding and drying and a process thereof, belonging to the field of inorganic non-metallic material subject high-temperature ceramics and refractory materials.
Background
China is a country with oil shortage, less gas and more coal, the proportion of energy consumption of coal in China is 64% in 2015, 74% of electric power comes from coal, and the proportion of energy consumption is predicted to be over 50% even in 2050. The Texaco coal gasification technology with great popularization strength in China is a gasification technology which takes coal water slurry as a raw material and is operated at high temperature (1300 plus 1500 ℃) and high pressure (2.7-6.5 MPa). Because the operating temperature must be higher than the melting point of the coal ash, Fe must be introduced into the coal water slurry2O3CaO, etc. reduce the melting point of the fly ash, but the fly ash aggravates the erosion and scouring of the lining material. Over 85wt% high Cr2O3Content of Cr2O3-Al2O3-ZrO2The series material has excellent compatibility with coal slag, and is a key refractory material commonly used in the existing coal water slurry gasification furnace. Although the erosion resistance of the high-chromium brick to the coal slurry slag is good, the service life of the high-chromium brick in a coal slurry gasification furnace is still short and can only be generally operated for about 5000 hours, the fundamental reason is that the thermal shock resistance of the high-chromium brick is extremely poor, and the water quenching cycle is only 1-2 times at 1100 ℃.
Therefore, the improvement of the thermal shock resistance of the high-chromium brick becomes the key for solving the service life of the coal water slurry gasification furnace. Generally, the structure of a refractory material is composed of aggregates, matrix and pores. The powder matrix has more apparent porosity, weaker erosion resistance and stronger thermal shock resistance; on the contrary, the granular aggregate has a compact and complete single crystal or polycrystalline structure, and has strong erosion resistance and weak thermal shock resistance. The method for improving the erosion resistance of the material is to prepare the matrix more compact, and the method for improving the thermal shock resistance of the material is to destroy the particle structure of a complete single crystal or polycrystalline structure, introduce more defects and effectively release the thermal stress when the material is subjected to uneven temperature. Reducing the size of the particulate aggregate reduces thermal stress concentrations in the same volume, but sacrifices the erosion resistance of the material. The invention adopts a method for modifying the particles, and the obtained pseudo particles with the coating structure artificially introduce more structural defects, thereby achieving the effects of reducing the thermal stress concentration in the same volume, improving the thermal shock resistance and not sacrificing the erosion resistance of the material.
Disclosure of Invention
The invention prepares ZrO by mixing and grinding large-particle chromium sand aggregate, submicron zirconia micro powder and thermosetting resin at one time, drying, heating and thermosetting2Powder coated pretreated granules of chrome sand grain structure (see figure 1). And then carrying out secondary mixing and grinding on the modified particle material, the modified powder material and the binding agent, ageing, forming and secondary drying, wherein the thermosetting resin is oxidized and ablated to escape and leave micropores and microporous holes and a coating particle structure of zirconium oxide (shown in figure 2) during firing, and the heat stress concentration is relieved through the pore defect and a zirconium oxide phase change toughening mechanism, so that the refractory material with high erosion resistance and high thermal shock resistance is obtained.
The technical characteristics of the secondary mixing grinding and drying process have 4 aspects: (1) ZrO coating around chromium sand particles by using thermosetting resin2The powder is prepared by heating thermosetting resin to obtain high strength, so that the chromium sand and the coating powder are formed into a compact pseudo particle. Compared with other physical adsorption methods, the chromium sand and nano zirconia pseudo particles can bear high mechanical grinding force of secondary mixing grinding without ZrO2The powder falls off to destroy the coating structure. The thermosetting resin acts as a binder during primary mixing and milling. (2) Adding a trace amount of additive into the fine powder by strong premixing, wherein the additive comprises a dispersant and a mineralizer, and the dispersant has the functions of ensuring that the fine powder has good flowing property and reducing deltaPotential, reducing or eliminating electrostatic repulsion of the press forming; the mineralizer has the functions of reducing the sintering temperature, promoting the sintering of the material, enabling the particles and the matrix to be combined more tightly and the matrix to be more compact, and improving the strength, the wear resistance, the slag penetration resistance and the erosion resistance of the refractory material. (3) The aluminum sol is used as a bonding agent to carry out secondary mixing and grinding on the granules and the powder, because the aluminum sol has better wettability on the resin-bonded pseudo granules than that of phosphate, and the influence of phosphate decomposition during the sintering of aluminum dihydrogen phosphate is avoided. (4) In the sintering process of the refractory material, the thermosetting resin in the pseudo particles is oxidized and ablated to escape and leave fine air holes, so that a micro-structure with the particles wrapped by the micro-holes is formed, a buffer space is provided for the particles when the particles expand with heat and contract with cold, and the concentration of thermal stress is reduced. The granule material is modified to achieve the effect of toughening and improve the thermal shock resistance of the material. The thermosetting resin plays a role of a pore-forming agent when the material is sintered after secondary mixing, grinding and drying.
The raw materials of the invention comprise the following components and the preparation process:
1. and (3) carrying out primary mixing and grinding and drying on large granules with the granularity of more than 1mm to obtain the pretreated granules A. The composition and treatment method of the pretreated granule A were as follows:
(1) 10-23 wt% of chromium sand with the granularity of 6-4 mm;
(2) 5-10 wt% of chromium sand with the granularity of 4-2 mm;
(3) 16-25 wt% of chromium sand with the granularity of 2-1 mm;
(4) 3-8 wt% of zirconia powder with the particle size of 0.1-0.5 mu m;
(5) thermosetting resin, plus, + 1-2 wt%;
and (3) sequentially mixing the granules (1), (2) and (3), adding (5) thermosetting resin and 1-2 wt%, then adding (4) powder, mixing and grinding for 5-10 minutes, and drying at 220-260 ℃ for 3-5 hours to obtain the pretreated granules A with the zirconia-coated chromium sand granule structure.
2. Meanwhile, the powder of the fine powder is strongly premixed to prepare premixed powder B, and the composition and the premixing method of the premixed powder B are as follows:
(6) 10-20 wt% of chromium sand powder with the particle size less than or equal to 88 mu m;
(7) 5-15 wt% of chromium green powder with the particle size less than or equal to 5 mu m;
(8) alpha-Al with particle size of 2-1 mu m2O310-18 wt% of powder;
(9) dextrin powder, plus + 0.5-1 wt%;
(10) high-dispersion hydroxypropyl methyl cellulose, plus, + 0.05-0.1 wt%;
and (3) mixing the three powder materials of (6), (7) and (8), adding (9) dextrin powder and 0.5-1 wt% and adding (10) high-dispersion hydroxypropyl methyl cellulose and 0.05-0.1 wt%, and strongly premixing at high speed for 10-20 minutes to prepare premixed powder material B.
3. Secondary mixing and grinding
(11) 5-10 wt% of chromium sand with the granularity of 1-0 mm;
(12) 2-5 wt% of mullite with the granularity of 1-0 mm;
(13) aluminum sol with the pH value of 3.5-4.0 and the particle size of colloidal particles of 10-20 nanometers, and + 3-5 wt%;
sequentially adding pretreated particle material A, (11) 5-10 wt% of chromium sand with the granularity of 1-0 mm, (12) 2-5 wt% of mullite with the granularity of 1-0 mm, and (13) 3.5-4.0 additional alumina sol with the pH value of 3.5-20 nm and the particle size of colloidal particles plus 3-5 wt%, mixing and grinding for 1-2 minutes, adding premixed powder material B, and strongly mixing and grinding for 10-20 minutes.
4. Ageing mixture
After the secondary mixing and grinding, ageing the mixture for 24-48 hours.
5. Shaping of
And (5) performing pressure forming according to the required drawing.
6. Secondary drying
And naturally drying the formed biscuit for 24 hours, and then drying the biscuit for 12 to 36 hours at the temperature of more than or equal to 150 ℃.
7. Firing into
And after drying, firing at 1550-1650 ℃ for 5-8 hours.
The invention has the advantages that: compared with the original high-chromium brick, the chrome corundum brick with high erosion resistance and high thermal shock resistance prepared by secondary mixed grinding and drying has equivalent erosion resistance; but compared with the high-chromium brick which is only subjected to water quenching circulation for 1-2 times at 1100 ℃, the circulation frequency is more than 5 times, the thermal shock resistance is obviously improved, the service life of the high-chromium brick applied to the coal water slurry gasification furnace is prolonged to more than 10000 hours, and the service life is prolonged by more than one time compared with the service life of the original high-chromium brick which is 5000 hours. Due to the excellent erosion resistance and thermal shock resistance, the material is suitable for a coal water slurry gasification furnace, a plasma melting furnace, an ultrahigh temperature gasification furnace and the like.
Drawings
FIG. 1 shows ZrO produced by primary mulling, drying and thermosetting2The powder-coated chromium sand particles are structurally schematic, wherein 1 is chromium sand, 2 is zirconium oxide and 3 is resin.
Fig. 2 is a schematic view of the structure of the microporous holes and zirconia-coated chromium sand particles formed after secondary mixing, grinding, drying, forming and firing, wherein 1 is chromium sand, 2 is zirconia, and 4 is pores.
Detailed Description
Example one
1. The preparation method comprises the following steps of (1) carrying out primary mixing and grinding and drying on large granules with the granularity of more than 1mm to obtain pretreated granules A1, wherein the composition and the treatment method of the pretreated granules A1 are as follows:
(1) 10wt% of chromium sand with the granularity of 6-4 mm;
(2) 10wt% of chromium sand with the granularity of 4-2 mm;
(3) 25wt% of chromium sand with the granularity of 2-1 mm;
(4) 8wt% of zirconia powder with the granularity of 0.1-0.5 mu m;
(5) thermosetting resin, plus, +2 wt%;
and (3) sequentially mixing the granules (1), (2) and (3), adding (5) thermosetting resin and 2wt%, then adding (4) powder, mixing and grinding for 5 minutes, and drying for 5 hours at 220 ℃ to obtain the pretreated granule A1 with the zirconia coated chromium sand granule structure.
2. Meanwhile, the powder of the fine powder is strongly premixed to prepare premixed powder B1, and the premixed powder B1 comprises the following components in parts by weight:
(6) 20wt% of chromium sand powder with the granularity less than or equal to 88 mu m;
(7) 5wt% of chromium green powder with the granularity less than or equal to 5 mu m;
(8) alpha-Al with particle size of 2-1 mu m2O3Powder, 10 wt%;
(9) dextrin powder, plus, +0.5 wt%;
(10) high-dispersion hydroxypropyl methyl cellulose, plus, +0.05 wt%;
and (3) mixing the powder materials of the (6), (7) and (8), adding (9) dextrin powder and 0.5wt% and adding (10) high-dispersion hydroxypropyl methyl cellulose and 0.05wt%, and performing powerful high-speed premixing for 20 minutes to obtain premixed powder material B1.
3. Secondary mixing and grinding
(11) 10wt% of chromium sand with the granularity of 1-0 mm;
(12) 2wt% of mullite with the granularity of 1-0 mm;
(13) adding 3wt% of alumina sol with the pH value of 3.5 and the particle size of colloidal particles of 10-20 nanometers;
sequentially adding pretreated particle material A1, (11) 10wt% of chrome sand with the granularity of 1-0 mm, (12) 2wt% of mullite with the granularity of 1-0 mm, (13) adding 3wt% of aluminum sol with the pH value of 3.5 and the particle size of colloidal particles of 10-20 nanometers, mixing and grinding for 2 minutes, adding premixed powder material B1, and strongly mixing and grinding for 10 minutes.
4. Ageing mixture
After the secondary mixing and grinding, the material is aged for 24 hours.
5. Shaping of
And (5) performing pressure forming according to the required drawing.
6. Secondary drying
The shaped biscuit was dried naturally for 24 hours and then dried at 150 ℃ for 12 hours.
7. Firing into
After drying, the mixture was fired at 1550 ℃ for 8 hours.
Compared with the original high-chromium brick, the chromium corundum brick with high erosion resistance and high thermal shock resistance prepared in the embodiment I has equivalent erosion resistance, and the water quenching cycle times of the thermal shock resistance at 1100 ℃ are improved to 7 times from the original 1-2 times. The water-coal-slurry gasification furnace is applied to a water-coal-slurry gasification furnace of Hua certain company, is replaced after being actually used for 10200 hours, and can be used for 1 month according to the conjecture of the length of the replaced residual brick. The average service life of the actual service life 10200 hours is more than doubled compared with the 5000 hours of the original high chrome brick.
Example two
1. The preparation method comprises the following steps of (1) carrying out primary mixing and grinding and drying on large granules with the granularity of more than 1mm to obtain pretreated granules A2, wherein the composition and the treatment method of the pretreated granules A2 are as follows:
(1) 17wt% of chromium sand with the granularity of 6-4 mm;
(2) 7wt% of chromium sand with the granularity of 4-2 mm;
(3) 20wt% of chromium sand with the granularity of 2-1 mm;
(4) 6wt% of zirconia powder with the granularity of 0.1-0.5 mu m;
(5) thermosetting resin, plus, +1.5 wt%;
and (3) sequentially mixing the granules (1), (2) and (3), adding (5) thermosetting resin and 1.5wt%, then adding the powder (4), mixing and grinding for 10 minutes, and drying at 260 ℃ for 3 hours to obtain the pretreated granule A2 with the zirconia-coated chromium sand granule structure.
2. Meanwhile, the powder of the fine powder is strongly premixed to prepare premixed powder B2, and the premixed powder B2 comprises the following components by a premixing method:
(6) 15wt% of chromium sand powder with the granularity less than or equal to 88 mu m;
(7) 10wt% of chromium green powder with the granularity less than or equal to 5 mu m;
(8) alpha-Al with particle size of 2-1 mu m2O3Powder, 13 wt%;
(9) dextrin powder, plus, +0.8 wt%;
(10) high-dispersion hydroxypropyl methyl cellulose, plus, +0.08 wt%;
mixing the above powders (6), (7) and (8), adding (9) dextrin powder and 0.8wt% and (10) high-dispersion hydroxypropyl methylcellulose and 0.08wt%, and strongly premixing at high speed for 15 min to obtain premixed powder B2.
3. Secondary mixing and grinding
(11) 8wt% of chromium sand with the granularity of 1-0 mm;
(12) 4wt% of mullite with the granularity of 1-0 mm;
(13) adding 4wt% of alumina sol with the pH value of 3.5 and the particle size of colloidal particles of 10-20 nanometers;
sequentially adding pretreated particle material A2, (11) 8wt% of chrome sand with the granularity of 1-0 mm, (12) 4wt% of mullite with the granularity of 1-0 mm, (13) adding 4wt% of aluminum sol with the pH value of 3.5 and the particle size of colloidal particles of 10-20 nanometers, mixing and grinding for 2 minutes, adding premixed powder material B2, and strongly mixing and grinding for 15 minutes.
4. Ageing mixture
After the secondary mixing and grinding, the material is aged for 24 hours.
5. Shaping of
And (5) performing pressure forming according to the required drawing.
6. Secondary drying
The formed biscuit is naturally dried for 24 hours and then dried for 24 hours at the temperature of more than or equal to 150 ℃.
7. Firing into
After drying, the mixture was fired at 1590 ℃ for 7 hours.
Compared with the original high-chromium brick, the chromium corundum brick with high erosion resistance and high thermal shock resistance prepared in the second embodiment has equivalent erosion resistance, and the water quenching cycle times of the thermal shock resistance at 1100 ℃ are improved to 6 times from the original 1-2 times. The water-coal-slurry gasification furnace is applied to a water-coal-slurry gasification furnace of Hua certain company, is replaced after being actually used for 10200 hours, and can be used for 1 month according to the conjecture of the length of the replaced residual brick. The service life of the brick is 10200 hours, which is more than doubled compared with the average service life of 5000 hours of the original high chrome brick.
EXAMPLE III
1. The preparation method comprises the following steps of (1) carrying out primary mixing and grinding and drying on large granules with the granularity of more than 1mm to obtain pretreated granules A3, wherein the composition and the treatment method of the pretreated granules A3 are as follows:
(1) 23wt% of chromium sand with the granularity of 6-4 mm;
(2) 5wt% of chromium sand with the granularity of 4-2 mm;
(3) 16wt% of chrome sand with the granularity of 2-1 mm;
(4) 3wt% of zirconia powder with the granularity of 0.1-0.5 mu m;
(5) thermosetting resin, plus, +1 wt%;
and (3) sequentially mixing the granules (1), (2) and (3), adding (5) thermosetting resin and 1wt%, then adding (4) powder, mixing and grinding for 5 minutes, and drying at 260 ℃ for 3 hours to obtain the pretreated granule A3 with the zirconia coated chromium sand granule structure.
2. Meanwhile, the powder of the fine powder is strongly premixed to prepare premixed powder B3, and the premixed powder B3 comprises the following components in parts by weight:
(6) 10wt% of chromium sand powder with the granularity less than or equal to 88 mu m;
(7) 15wt% of chromium green powder with the granularity less than or equal to 5 mu m;
(8) alpha-Al with particle size of 2-1 μm2O3Powder, 18 wt%;
(9) dextrin powder, plus, +1 wt%;
(10) high-dispersion hydroxypropyl methyl cellulose, plus, +0.1 wt%;
and (3) mixing the powder materials of the (6), (7) and (8), adding (9) dextrin powder and 0.1wt% of high-dispersion hydroxypropyl methyl cellulose, and adding (10), and performing powerful high-speed premixing for 10 minutes to obtain premixed powder material B3.
3. Secondary mixing and grinding
(11) 5wt% of chromium sand with the granularity of 1-0 mm;
(12) 5wt% of mullite with the granularity of 1-0 mm;
(13) adding 5wt% of alumina sol with the pH value of 4.0 and the particle size of colloidal particles of 10-20 nanometers;
sequentially adding pretreated particle material A3, (11) 5wt% of chromium sand with the granularity of 1-0 mm, (12) 5wt% of mullite with the granularity of 1-0 mm, (13) 5wt% of aluminum sol with the pH value of 4.0 and the particle size of colloidal particles of 10-20 nanometers, mixing and grinding for 1 minute, adding premixed powder material B3, and strongly mixing and grinding for 20 minutes.
4. Ageing mixture
After the secondary mixing and grinding, the material is aged for 48 hours.
5. Shaping of
And (5) performing pressure forming according to the required drawing.
6. Secondary drying
The formed biscuit is naturally dried for 24 hours and then dried for 36 hours at the temperature of more than or equal to 150 ℃.
7. Firing into
After drying, the mixture was fired at 1650 ℃ for 5 hours.
Compared with the original high-chromium brick, the chromium corundum brick with high erosion resistance and high thermal shock resistance prepared in the third embodiment has equivalent erosion resistance, and the water quenching cycle times of the thermal shock resistance at 1100 ℃ are improved to 6 times from the original 1-2 times. The water-coal-slurry gasification furnace is applied to a water-coal-slurry gasification furnace of Hua certain company, is replaced after being actually used for 10200 hours, and can be continuously used for about half a month according to the conjecture of the length of the replaced residual bricks. The service life of the brick is 10200 hours, which is more than doubled compared with the average service life of 5000 hours of the original high chrome brick.

Claims (1)

1. A preparation method for preparing a high erosion resistance and high thermal shock resistance chromium corundum brick by secondary mixed grinding and drying is characterized by comprising the following raw material components and preparation processes of a secondary mixed grinding process:
step 1: the preparation method comprises the following steps of (1) carrying out primary mixing and grinding and drying on large granules with the granularity of more than 1mm to obtain pretreated granules A, wherein the composition and the treatment method of the pretreated granules A are as follows:
(1) 10-23 wt% of chromium sand with the granularity of 6-4 mm;
(2) 5-10 wt% of chromium sand with the granularity of 4-2 mm;
(3) 16-25 wt% of chromium sand with the granularity of 2-1 mm;
(4) 3-8 wt% of zirconia powder with the particle size of 0.1-0.5 mu m;
(5) thermosetting resin, plus, + 1-2 wt%;
sequentially mixing the three granular materials (1), (2) and (3), adding (5) thermosetting resin and 1-2 wt%, and then adding (4) powder; mixing and grinding for 5-10 minutes; drying for 3-5 hours at 220-260 ℃ to obtain a pretreated granule material A with a zirconia-coated chromium sand granule structure, wherein thermosetting resin is used as a bonding agent through primary mixing and grinding and drying, and is subjected to secondary mixing and grinding, drying and firing, and the thermosetting resin is oxidized and ablated to escape and leave micropores during firing to form a pore-forming agent;
step 2: and (2) strongly premixing the fine powder to prepare premixed powder B, wherein the premixed powder B comprises the following components in parts by weight:
(6) 10-20 wt% of chromium sand powder with the particle size less than or equal to 88 mu m;
(7) 5-15 wt% of chromium green powder with the particle size less than or equal to 5 mu m;
(8) alpha-Al with particle size of 2-1 mu m2O310-18 wt% of powder;
(9) dextrin powder, plus + 0.5-1 wt%;
(10) high-dispersion hydroxypropyl methyl cellulose, plus, + 0.05-0.1 wt%;
mixing the three powder materials of (6), (7) and (8), adding (9) dextrin powder and 0.5-1 wt% and adding (10) high-dispersion hydroxypropyl methyl cellulose and 0.05-0.1 wt%, and strongly premixing at high speed for 10-20 minutes to prepare premixed powder material B;
and step 3: secondary mixing and grinding
(11) 5-10 wt% of chromium sand with the granularity of 1-0 mm;
(12) 2-5 wt% of mullite with the granularity of 1-0 mm;
(13) aluminum sol with the pH value of 3.5-4.0 and the particle size of colloidal particles of 10-20 nanometers, and + 3-5 wt%;
sequentially adding pretreated particle material A, (11) 5-10 wt% of chromium sand with the granularity of 1-0 mm, (12) 2-5 wt% of mullite with the granularity of 1-0 mm, (13) adding alumina sol with the pH value of 3.5-4.0 and the particle size of colloidal particles of 10-20 nanometers and 3-5 wt%, mixing and grinding for 1-2 minutes, adding premixed powder material B, and strongly mixing and grinding for 10-20 minutes;
and 4, step 4: ageing mixture
After secondary mixing and grinding, ageing for 24-48 hours;
and 5: shaping of
Molding according to the required drawing pressure;
step 6: secondary drying
Naturally drying the formed biscuit for 24 hours, and then drying the biscuit for 12 to 36 hours at the temperature of more than or equal to 150 ℃;
and 7: firing into
And after drying, firing at 1550-1650 ℃ for 5-8 hours.
CN202010602427.4A 2020-06-30 2020-06-30 Chrome corundum brick with high erosion resistance and thermal shock resistance prepared by secondary mixed grinding and drying and process thereof Active CN112194473B (en)

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