CN106946556B - Preparation method of low-creep anti-crack silica brick - Google Patents
Preparation method of low-creep anti-crack silica brick Download PDFInfo
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- CN106946556B CN106946556B CN201710162107.XA CN201710162107A CN106946556B CN 106946556 B CN106946556 B CN 106946556B CN 201710162107 A CN201710162107 A CN 201710162107A CN 106946556 B CN106946556 B CN 106946556B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 75
- 239000011449 brick Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 239000011268 mixed slurry Substances 0.000 claims abstract description 22
- 238000007710 freezing Methods 0.000 claims abstract description 20
- 230000008014 freezing Effects 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 17
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical class [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 14
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 241000736285 Sphagnum Species 0.000 claims abstract description 10
- 235000006040 Prunus persica var persica Nutrition 0.000 claims abstract description 9
- 240000006413 Prunus persica var. persica Species 0.000 claims abstract 2
- 239000012065 filter cake Substances 0.000 claims description 51
- 239000000463 material Substances 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 13
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 10
- 238000012258 culturing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 7
- 239000004575 stone Substances 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 abstract description 8
- 239000002002 slurry Substances 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 abstract 1
- 230000003628 erosive effect Effects 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000010257 thawing Methods 0.000 abstract 1
- 244000144730 Amygdalus persica Species 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- 239000002344 surface layer Substances 0.000 description 4
- 239000000571 coke Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000009628 steelmaking Methods 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000011044 quartzite Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/608—Green bodies or pre-forms with well-defined density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention relates to a preparation method of a low-creep anti-crack silica brick, belonging to the technical field of silica brick preparation. The present invention prepares the mixed slurry of sphagnum and lichen through soaking in silica pores during constant temperature culture, freezing with liquid nitrogen to freeze the liquid in the pores and increase the volume to produce pressure, widening and deepening the silica pores, microwave thawing to make the slurry enter the silica pores deeply, eroding silica, re-freezing and crushing to break up silica, absorbing saturated calcium hydroxide solution in silica at relatively low temperature, ultrasonic dispersing, lowering the solubility of calcium hydroxide at relatively high temperature, depositing on the surface of silica, drying, mixing with peach gum, etc. and high temperature burning. The low-creep anti-crack silica brick prepared by the invention has excellent creep resistance under high temperature conditions, the refractoriness under load reaches 1700-1800 ℃, the refractoriness reaches over 1750 ℃, and the low-creep anti-crack silica brick has wide application prospect.
Description
Technical Field
The invention relates to a preparation method of a low-creep anti-crack silica brick, belonging to the technical field of silica brick preparation.
Background
The silica brick is made of SiO
2The traditional refractory product as main component belongs to acid refractory material, and has the features of high volume stability at high temperature, high heat conductivity, high acid slag corrosion resistance, high refractoriness under load (30-50 deg.c different from refractoriness), etc. The main raw material for manufacturing the silica brick is silica (quartzite), and the silica brick is produced in China from 30 s in the 20 th century to the beginning of 50 s in large quantities for steelmaking open-hearth furnaces and coke ovens. For half a century, with the elimination of open-hearth furnaces for steel making, the use of silica bricks has currently been mainly concentrated on coke ovens, blast furnaces and hot blast stoves, however, the manufacturing processes and techniques of silica bricks have not changed greatly over a considerable period of time.
Currently used silica brick (SiO)
2Content is more than or equal to 95 percent), the phase change of the contained quartz at medium temperature and the volume effect of the phase change very severely limit the heating and cooling operation of the hot blast stove, and in the periodic combustion-air supply circulating work of the stove, the silicon brick body of the hot blast stove is gradually softened under certain pressure to generate plastic deformation and greatly reduce the strength because of working at high temperature for a long time, and even the brick body can be seriously damaged, thereby causing the damage of the stove body.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the problems that the traditional silica brick works at high temperature for a long time in the using process, the traditional silica brick generates plastic deformation after being pressed, the strength is greatly reduced, and even the brick body is cracked and damaged, the method for preparing the low-creep anti-crack silica brick by mixing and burning the silica stone after being pretreated and modified with peach gum and the like is provided. The present invention prepares mixed slurry with sphagnum tenue and cupulate lichen, the mixed slurry is made to penetrate into the pores of silica during constant temperature culture, and then frozen with liquid nitrogen to freeze the liquid in the pores and increase the volume to produce pressure, so as to widen and deepen the pores of silica, and then defreeze with microwave to make the slurry enter into the silica deeply along the enlarged pores to erode the silica, so that the silica is cracked after being frozen and crushed again, and the silica absorbs saturated calcium hydroxide solution at lower temperature, and after ultrasonic dispersion, the solubility of calcium hydroxide is reduced at higher temperature and precipitated on the surface of silica to achieve the purpose of full mixing, and after drying, the silica is mixed with peach gum, etc. and fired at high temperature to prepare the low creep crack resistant silica brick. In the firing process of the silica brick, the silica has uniform conversion rate, less residual quartz content and excellent creep resistance under the high-temperature condition, and the problem that the traditional silica is easy to plastically deform when working at a high-temperature state for a long time is effectively solved.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) weighing 150-200 g of sphagnum gracile and 160-280 g of cupulate moss in sequence, pouring the materials into a stone mill, grinding for 10-15 min, mixing 2200-2800 mL of water in the grinding process to obtain mixed slurry, adding 1000-1200 mL of the obtained mixed slurry and 400-500 g of 40-60-mesh silica into a beaker in sequence, stirring and mixing for 10-15 min by using a glass rod, transferring the beaker into a constant temperature incubator, and culturing for 5-7 days at a constant temperature of 20-25 ℃; the silica has a silicon dioxide content of greater than 99%;
(2) after the culture is finished, filtering materials in the beaker, collecting a filter cake, freezing the obtained filter cake for 2-4 min by using liquid nitrogen, transferring the frozen filter cake into a microwave heater, unfreezing for 3-5 min under the condition that the power is 400-600W, putting the unfrozen filter cake into the beaker filled with 900-1100 mL of the obtained mixed slurry, placing the beaker into a constant-temperature incubator, culturing for 3-5 days at the constant temperature of 20-25 ℃, filtering the materials in the beaker, collecting filter residues, washing the filter residues for 3-5 times by using deionized water, transferring the washed filter residues into a freezing crusher, freezing for 2-4 min by using liquid nitrogen, and crushing for 20-30 min to obtain a wet crushed filter residue material;
(3) weighing 800-1000 mL of deionized water, pouring the deionized water into a beaker, placing the beaker in an ice-water bath at the temperature of 2-4 ℃, adding calcium hydroxide into the beaker until the calcium hydroxide is not dissolved, weighing 300-400 g of the obtained wet crushed filter residue, pouring the wet crushed filter residue into the beaker, stirring and mixing the mixture for 3-5 min by using a glass rod, ultrasonically dispersing the mixture for 15-20 min at the frequency of 35-40 kHz, then transferring the beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 45-60 min at the constant temperature of 90-95 ℃ and the rotating speed of 600-800 r/min, filtering the material in the beaker while the material is hot, collecting filter cakes, transferring the obtained filter cakes into a drying oven, and drying the filter cakes at the temperature of 105-110 ℃ until the water content is 0.6-0.8% to obtain dried filter cakes;
(4) sequentially adding 100-120 parts by weight of the obtained dry filter cake, 2-4 parts by weight of peach gum, 0.3-0.5 part by weight of nano iron oxide, 0.2-0.8 part by weight of nano silicon dioxide and 10-15 parts by weight of water into a wet mill, mixing for 40-60 min, transferring the materials in the wet mill into a friction press, and pressing to obtain the product with the bulk density of 2.2-2.5 g/cm
3And (3) placing the brick in an oven, drying the brick to constant weight at the temperature of 105-110 ℃, transferring the dried brick into a tunnel kiln, carrying out heat preservation firing at the temperature of 1400-1450 ℃ for 24-36 h, and discharging to obtain the low-creep anti-crack silica brick.
The application method of the invention comprises the following steps: the low-creep anti-crack silica brick surface layer prepared by the method is uniformly coated with a cementing material, the silica brick coated with the binding material is built on the wall of a hot blast stove by adopting a stacking and stacking mode, the thickness of a brick joint of the building body is controlled to be 1.0-2.0 mm, and after the building is finished, the building body is plastered and maintained at normal temperature for 7-10 days. Through detection, the low-creep anti-crack silica brick masonry wall body prepared by the invention has the advantages that the refractoriness under load reaches 1700-1800 ℃, the refractoriness reaches over 1750 ℃, the wall body works for 25 hours under the conditions that the pressure is 0.2MPa and the temperature is 1500 ℃, and the creep rate is lower than 0.06%.
Compared with other methods, the method has the beneficial technical effects that:
(1) the low-creep anti-crack silica brick prepared by the invention works for 25 hours under the conditions that the pressure is 0.2MPa and the temperature is 1500 ℃, the creep rate is lower than 0.06 percent, and the creep resistance is excellent under the high-temperature condition;
(2) the low-creep anti-crack silica brick prepared by the invention has the refractoriness under load of 1700-1800 ℃ and the refractoriness of over 1750 ℃, can be widely applied to coke ovens, blast furnaces and hot blast furnaces, and has wide application prospect.
Detailed Description
Firstly, 150-200 g of sphagnum gracile and 160-280 g of cupulate moss are sequentially weighed, poured into a stone mill, ground for 10-15 min, mixed with 2200-2800 mL of water in the grinding process to obtain mixed slurry, then 1000-1200 mL of the mixed slurry and 400-500 g of 40-60-mesh silica are sequentially added into a beaker, stirred and mixed by a glass rod for 10-15 min, and then the beaker is transferred into a constant temperature incubator and cultured for 5-7 days at a constant temperature of 20-25 ℃; the silica has a silicon dioxide content of greater than 99%; after the culture is finished, filtering materials in the beaker, collecting a filter cake, freezing the obtained filter cake for 2-4 min by using liquid nitrogen, transferring the frozen filter cake into a microwave heater, unfreezing for 3-5 min under the condition that the power is 400-600W, putting the unfrozen filter cake into the beaker filled with 900-1100 mL of the obtained mixed slurry, placing the beaker into a constant-temperature incubator, culturing for 3-5 days at the constant temperature of 20-25 ℃, filtering the materials in the beaker, collecting filter residues, washing the filter residues for 3-5 times by using deionized water, transferring the washed filter residues into a freezing crusher, freezing for 2-4 min by using liquid nitrogen, and crushing for 20-30 min to obtain a wet crushed filter residue material; measuring 800-1000 mL of deionized water, pouring the deionized water into a beaker, placing the beaker in an ice-water bath at the temperature of 2-4 ℃, adding calcium hydroxide into the beaker until the calcium hydroxide is not dissolved, then weighing 300-400 g of the obtained wet crushed filter residue, pouring the wet crushed filter residue into the beaker, stirring and mixing the materials for 3-5 min by using a glass rod, ultrasonically dispersing the materials for 15-20 min at the frequency of 35-40 kHz, then transferring the beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the materials for 45-60 min at the constant temperature of 90-95 ℃ and the rotating speed of 600-800 r/min, filtering the materials in the beaker while the materials are hot, collecting filter cakes, and filtering the obtained filter cakesTransferring the cake into an oven, and drying at 105-110 ℃ until the water content is 0.6-0.8% to obtain a dry filter cake; sequentially adding 100-120 parts by weight of the obtained dry filter cake, 2-4 parts by weight of peach gum, 0.3-0.5 part by weight of nano iron oxide, 0.2-0.8 part by weight of nano silicon dioxide and 10-15 parts by weight of water into a wet mill, mixing for 40-60 min, transferring the materials in the wet mill into a friction press, and pressing to obtain the product with the bulk density of 2.2-2.5 g/cm
3And (3) placing the brick in an oven, drying the brick to constant weight at the temperature of 105-110 ℃, transferring the dried brick into a tunnel kiln, carrying out heat preservation firing at the temperature of 1400-1450 ℃ for 24-36 h, and discharging to obtain the low-creep anti-crack silica brick.
Example 1
Firstly, sequentially weighing 200g of sphagnum gracile and 280g of cupulate moss, pouring the sphagnum gracile and the cupulate moss into a stone mill, grinding the sphagnum gracile and the cupulate moss for 15min, mixing 2800mL of water in the grinding process to obtain mixed slurry, sequentially adding 1200mL of the mixed slurry and 500g of 60-mesh silica into a beaker, stirring and mixing the mixed slurry and 500g of the 60-mesh silica for 15min by using a glass rod, transferring the beaker into a constant-temperature incubator, and culturing the beaker at the constant temperature of 25 ℃ for 7; the silica has a silicon dioxide content of greater than 99%; after the culture is finished, filtering materials in the beaker, collecting filter cakes, freezing the obtained filter cakes for 4min by using liquid nitrogen, transferring the frozen filter cakes into a microwave heater, unfreezing for 5min under the condition that the power is 600W, putting the unfrozen filter cakes into the beaker filled with 1100mL of the obtained mixed slurry, placing the beaker into a constant-temperature incubator, culturing for 5 days at the constant temperature of 25 ℃, filtering the materials in the beaker, collecting filter residues, washing the filter residues for 5 times by using deionized water, transferring the washed filter residues into a freezing and crushing machine, freezing for 4min by using liquid nitrogen, and crushing for 30min to obtain crushed wet filter residues; weighing 1000mL of deionized water, pouring the deionized water into a beaker, placing the beaker in an ice-water bath at 4 ℃, adding calcium hydroxide into the beaker until the calcium hydroxide is not dissolved, weighing 400g of the obtained crushed filter residue wet material, pouring the crushed filter residue wet material into the beaker, stirring and mixing the crushed filter residue wet material for 5min by a glass rod, ultrasonically dispersing the crushed filter residue wet material for 20min at the frequency of 40kHz, then transferring the beaker into a digital display speed measurement constant-temperature magnetic stirrer, and carrying out ultrasonic dispersion at the temperature of 95 ℃ and the rotating speed of 80 ℃ for 20minStirring and mixing at constant temperature of 0r/min for 60min, filtering the materials in the beaker while the materials are hot, collecting a filter cake, transferring the obtained filter cake into an oven, and drying at the temperature of 110 ℃ until the water content is 0.8% to obtain a dried filter cake; adding 120 parts by weight of the obtained dry filter cake, 4 parts by weight of peach gum, 0.5 part by weight of nano iron oxide, 0.8 part by weight of nano silicon dioxide and 15 parts by weight of water into a wet mill in sequence, mixing for 60min, transferring the materials in the wet mill into a friction press, and pressing to obtain the product with the volume density of 2.5g/cm
3And (3) placing the bricks in an oven, drying the bricks to constant weight at the temperature of 110 ℃, transferring the dried bricks into a tunnel kiln, carrying out heat preservation firing at the temperature of 1450 ℃ for 36 hours, and discharging to obtain the low-creep anti-crack silicon brick.
The low-creep anti-crack silica brick surface layer prepared by the invention is uniformly coated with cementing materials, the silica brick coated with the binding materials is built on the wall of a hot blast stove by adopting a stacking and stacking mode, the thickness of the brick joint of the masonry is controlled to be 2.0mm, and after the building is finished, the masonry is plastered and maintained at normal temperature for 10 days. Tests show that the low-creep anti-crack silica brick masonry wall body prepared by the method has the refractoriness under load of 1800 ℃, the refractoriness of 1755 ℃, works for 25 hours under the conditions of 0.2MPa of pressure and 1500 ℃, and has the creep rate of 0.05 percent.
Example 2
Firstly, 150g of sphagnum tenue and 160g of cupulate moss are weighed in sequence, poured into a stone mill, ground for 10min, 2200mL of water is mixed in the grinding process to obtain mixed slurry, 1000mL of the mixed slurry and 400g of 40-mesh silica are sequentially added into a beaker, stirred and mixed for 10min by a glass rod, and then the beaker is transferred into a constant-temperature incubator and cultured for 5 days at the constant temperature of 20 ℃; the silica has a silicon dioxide content of greater than 99%; after the culture is finished, filtering the materials in the beaker, collecting filter cakes, freezing the obtained filter cakes for 2min by using liquid nitrogen, transferring the frozen filter cakes into a microwave heater, unfreezing for 3min under the condition that the power is 400W, putting the unfrozen filter cakes into the beaker filled with 900mL of the mixed slurry, putting the beaker into a constant-temperature incubator, and culturing for 3 days at the constant temperature of 20 DEG CFiltering the materials in the beaker, collecting the filter residue, washing the filter residue for 3 times by using deionized water, transferring the washed filter residue into a freezing grinder, freezing for 2min by using liquid nitrogen, and then grinding for 20min to obtain wet ground filter residue; weighing 800mL of deionized water, pouring the deionized water into a beaker, placing the beaker in an ice-water bath at 2 ℃, adding calcium hydroxide into the beaker until the calcium hydroxide is not dissolved, weighing 300g of the obtained wet crushed filter residue, pouring the wet crushed filter residue into the beaker, stirring and mixing the wet crushed filter residue for 3min by using a glass rod, ultrasonically dispersing the mixture for 15min at the frequency of 35kHz, then transferring the beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 45min at the constant temperature of 90 ℃ and the rotating speed of 600r/min, filtering the material in the beaker while the material is hot, collecting a filter cake, transferring the obtained filter cake into a baking oven, and drying the filter cake at the temperature of 105 ℃ until the water content is 0.6% to obtain a dried filter cake; adding 100 parts by weight of the obtained dry filter cake, 2 parts by weight of peach gum, 0.3 part by weight of nano iron oxide, 0.2 part by weight of nano silicon dioxide and 10 parts by weight of water into a wet mill in sequence, mixing for 40min, transferring the materials in the wet mill into a friction press, and pressing to obtain the product with the volume density of 2.2g/cm
3And (3) placing the bricks in an oven, drying the bricks to constant weight at the temperature of 105 ℃, transferring the dried bricks into a tunnel kiln, carrying out heat preservation firing for 24 hours at the temperature of 1400 ℃, and discharging to obtain the low-creep anti-crack silicon brick.
The low-creep anti-crack silica brick surface layer prepared by the invention is uniformly coated with cementing materials, the silica brick coated with the binding materials is built on the wall of a hot blast stove by adopting a stacking and stacking mode, the thickness of the brick joint of the masonry is controlled to be 1.0mm, and after the building is finished, the masonry is plastered and maintained at normal temperature for 7 days. Through detection, the refractoriness under load of the wall body built by the low-creep anti-crack silica brick prepared by the invention reaches 1700 ℃, the refractoriness reaches 1760 ℃, the wall body works for 25 hours under the conditions that the pressure is 0.2MPa and the temperature is 1500 ℃, and the creep rate is 0.04%.
Example 3
Firstly, 170g of sphagnum tenue and 200g of cupulate moss are weighed in turn, poured into a stone mill, ground for 12min, mixed with 2400mL of water in the grinding process to obtain mixed slurry, and 1100mL of the mixed slurry is added into a beaker in turnMixing the slurry and 450g of 50-mesh silica, stirring and mixing for 12min by using a glass rod, transferring the beaker into a constant-temperature incubator, and carrying out constant-temperature culture for 6 days at the temperature of 22 ℃; the silica has a silicon dioxide content of greater than 99%; after the culture is finished, filtering materials in the beaker, collecting filter cakes, freezing the obtained filter cakes for 3min by using liquid nitrogen, transferring the frozen filter cakes into a microwave heater, unfreezing for 4min under the condition that the power is 500W, putting the unfrozen filter cakes into the beaker filled with 1000mL of the obtained mixed slurry, placing the beaker into a constant-temperature incubator, culturing for 4 days at a constant temperature under the condition that the temperature is 22 ℃, filtering the materials in the beaker, collecting filter residues, washing the filter residues for 4 times by using deionized water, transferring the washed filter residues into a freezing and crushing machine, freezing for 3min by using liquid nitrogen, and crushing for 25min to obtain crushed wet filter residues; measuring 900mL of deionized water, pouring the deionized water into a beaker, placing the beaker in an ice-water bath at 3 ℃, adding calcium hydroxide into the beaker until the calcium hydroxide is not dissolved, weighing 350g of the obtained wet crushed filter residue, pouring the wet crushed filter residue into the beaker, stirring and mixing the wet crushed filter residue for 4min by using a glass rod, ultrasonically dispersing the wet crushed filter residue for 17min at the frequency of 37kHz, then transferring the beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 50min at the constant temperature of 92 ℃ and the rotation speed of 700r/min, filtering the material in the beaker while the material is hot, collecting a filter cake, transferring the obtained filter cake into a baking oven, and drying the filter cake at the temperature of 107 ℃ until the water content is 0.7% to obtain a dried filter cake; according to the weight portion, 110 portions of the obtained dry filter cake, 3 portions of peach gum, 0.4 portion of nano iron oxide, 0.6 portion of nano silicon dioxide and 12 portions of water are sequentially added into a wet mill, after mixing for 50min, the materials in the wet mill are transferred into a friction press machine, and are pressed into the material with the volume density of 2.3g/cm
3And (3) placing the brick in an oven, drying the brick to constant weight at the temperature of 107 ℃, transferring the dried brick into a tunnel kiln, carrying out heat preservation firing for 30 hours at the temperature of 1420 ℃, and discharging to obtain the low-creep anti-crack silicon brick.
The low-creep anti-crack silica brick surface layer prepared by the invention is uniformly coated with cementing materials, the silica brick coated with the binding materials is built on the wall of a hot blast stove by adopting a stacking and stacking mode, the thickness of the brick joint of the masonry is controlled to be 1.5mm, and after the building is finished, the masonry is plastered and maintained at normal temperature for 8 days. Through detection, the refractoriness under load of the wall body built by the low-creep anti-crack silica brick prepared by the invention reaches 1730 ℃, the refractoriness reaches 1780 ℃, the wall body works for 25 hours under the conditions that the pressure is 0.2MPa and the temperature is 1500 ℃, and the creep rate is 0.03%.
Claims (1)
1. A preparation method of a low-creep anti-crack silica brick is characterized by comprising the following specific preparation steps:
(1) weighing 150-200 g of sphagnum gracile and 160-280 g of cupulate moss in sequence, pouring the materials into a stone mill, grinding for 10-15 min, mixing 2200-2800 mL of water in the grinding process to obtain mixed slurry, adding 1000-1200 mL of the obtained mixed slurry and 400-500 g of 40-60-mesh silica into a beaker in sequence, stirring and mixing for 10-15 min by using a glass rod, transferring the beaker into a constant temperature incubator, and culturing for 5-7 days at a constant temperature of 20-25 ℃; the silica has a silicon dioxide content of greater than 99%;
(2) after the culture is finished, filtering materials in the beaker, collecting a filter cake, freezing the obtained filter cake for 2-4 min by using liquid nitrogen, transferring the frozen filter cake into a microwave heater, unfreezing for 3-5 min under the condition that the power is 400-600W, putting the unfrozen filter cake into the beaker filled with 900-1100 mL of the obtained mixed slurry, placing the beaker into a constant-temperature incubator, culturing for 3-5 days at the constant temperature of 20-25 ℃, filtering the materials in the beaker, collecting filter residues, washing the filter residues for 3-5 times by using deionized water, transferring the washed filter residues into a freezing crusher, freezing for 2-4 min by using liquid nitrogen, and crushing for 20-30 min to obtain a wet crushed filter residue material;
(3) weighing 800-1000 mL of deionized water, pouring the deionized water into a beaker, placing the beaker in an ice-water bath at the temperature of 2-4 ℃, adding calcium hydroxide into the beaker until the calcium hydroxide is not dissolved, weighing 300-400 g of the obtained wet crushed filter residue, pouring the wet crushed filter residue into the beaker, stirring and mixing the mixture for 3-5 min by using a glass rod, ultrasonically dispersing the mixture for 15-20 min at the frequency of 35-40 kHz, then transferring the beaker into a digital display speed measurement constant-temperature magnetic stirrer, stirring and mixing the mixture for 45-60 min at the constant temperature of 90-95 ℃ and the rotating speed of 600-800 r/min, filtering the material in the beaker while the material is hot, collecting filter cakes, transferring the obtained filter cakes into a drying oven, and drying the filter cakes at the temperature of 105-110 ℃ until the water content is 0.6-0.8% to obtain dried filter cakes;
(4) sequentially adding 100-120 parts by weight of the obtained dried filter cake, 2-4 parts by weight of peach gum, 0.3-0.5 part by weight of nano iron oxide, 0.2-0.8 part by weight of nano silicon dioxide and 10-15 parts by weight of water into a wet mill, mulling for 40-60 min, transferring the materials in the wet mill into a friction press, pressing to obtain 3 bricks with the volume density of 2.2-2.5 g/cm, placing the bricks in a drying oven, drying at the temperature of 105-110 ℃ to constant weight, transferring the dried bricks into a tunnel kiln, carrying out heat preservation firing at the temperature of 1400-1450 ℃ for 24-36 h, and discharging to obtain the low-creep anti-crack silicon brick;
the low creep crack resistant silica brick works for 25 hours under the conditions that the pressure is 0.2Mpa and the temperature is 1500 ℃, and the creep rate is lower than 0.06 percent.
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