CN115894018A - Glass kiln material flowing nozzle brick and preparation method thereof - Google Patents
Glass kiln material flowing nozzle brick and preparation method thereof Download PDFInfo
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- CN115894018A CN115894018A CN202310010406.7A CN202310010406A CN115894018A CN 115894018 A CN115894018 A CN 115894018A CN 202310010406 A CN202310010406 A CN 202310010406A CN 115894018 A CN115894018 A CN 115894018A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention relates to a high-temperature material, in particular to a material flow nozzle brick of a glass kiln and a preparation method thereof, wherein the material of a working layer does not have a low-melting-point glass phase, the content of zirconium dioxide is high, and the sintering temperature is high, so that the anti-erosion performance is far better than that of an electric melting AZS protective layer, the protective layer is a non-working part of the material flow nozzle brick, is not contacted with glass liquid, plays the roles of supporting and protecting the working layer, and is lower in manufacturing cost, so that the overall cost of the composite material flow nozzle brick is slightly higher than that of the electric melting AZS.
Description
Technical Field
The invention relates to a high-temperature material, in particular to a glass kiln material flow nozzle brick and a preparation method thereof.
Background
The special glass tubular product is an important inorganic material and is widely applied to various fields of medical treatment, electronics, national defense, military industry, civil use and the like. The material flow nozzle bricks used in the glass kiln for manufacturing special glass tubular products are all made of fused zirconia corundum materials, and are called AZS by English abbreviation, and the brands of the material flow nozzle bricks are AZS-33#, AZS-36#, and AZS-41#. The meaning of the brand: A-AI2O3, Z-ZrO2, S-SiO2, numbers (33 #, 36#, 41 #) represent the percent content of zirconium dioxide of each brand. At present, the material of the nozzle brick which is applied more is AZS-33#.
The fused zirconia corundum nozzle brick is prepared by melting and casting industrial alumina, zircon sand (containing about 65% of ZrO2 and about 34% of SiO 2) and a part of soda Na2CO3 in an electric arc furnace. The phase composition of the brick is as follows: corundum, baddeleyite, corundum baddeleyite eutectic and glass phase. Because about 15% of low-melting-point glass phase exists in the brick, under the high-temperature working condition environment, the glass phase in the brick is continuously separated out towards the surface of the brick and is subjected to uninterrupted physical scouring with flowing high-temperature glass liquid, the internal structure of the brick body is hollow, and then the high-temperature glass liquid gradually permeates and erodes from the surface of the brick body to the inside, and the high-temperature glass liquid gradually becomes a deteriorated layer from the permeable layer and then falls off and runs off in the glass liquid, under the double effects of the physical scouring and the chemical erosion of the glass liquid on the brick, the width size of a glass liquid channel of the brick body is increased, when the width size is increased by about 10 millimeters, the glass liquid flow is out of control, the brick body is scrapped, a new material nozzle brick needs to be replaced, the maintenance and production stopping loss is caused, and the production cost of a glass enterprise is increased.
In order to reduce the dissolution of the glass phase, those skilled in the art have studied prior art 1, a fused cast zirconia-corundum refractory brick (202010659684.1) with zero exudation of the glass phase, specifically disclosing Al 2 O 3 59.6 to 65.9 percent of ZrO 2 15.1 to 17.7 percent of SiO 2 16.4 to 17.2 percent of Na 2 2.2 to 2.5 percent of O and Fe 2 O 3 With TiO 2 The total content of SiO in the fused cast zirconia corundum is 0.2 percent 2 Constituting the bulk of the glassy phase, directly determining the amount of glassy phase, and Na 2 O affects the viscosity of the glass phase and reduces SiO in the chemical composition 2 And Na 2 The content of O can reduce the quantity of the glass phase in the material and improve the quality of the glass phase, thereby reducing the exudation quantity of the glass phase, but the material still belongs to the fused cast zirconia-corundum brick, the content of sodium silicate is as high as 17.3% -20.2%, and the glass phase in the system still stays high.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a glass kiln material nozzle brick which has no low-melting-point glass phase in the material of a working layer, high zirconium dioxide content and high sintering temperature and a preparation method thereof.
The invention is realized by the following technical scheme: a glass kiln material flowing nozzle brick comprises an inner working layer and an outer protective layer, wherein the thickness of the working layer accounts for 30% -40%, and the thickness of the protective layer accounts for 60% -70%;
the working layer is made of ZrO from the following raw materials in percentage by weight 2 70-90wt%、α-Al 2 O 3 4-20wt%、Al 2 O 3 2-5wt%、SiO 2 1-3wt%、Y 2 O 3 1-3wt%、MgO 1-3wt%；
The protective layer is made of the following raw materials in percentage by weight, alpha-Al 2 O 3 10-20wt%、 Al 2 O 3 5-8wt%、SiO 2 2-4wt% and 70-80wt% of mullite crystal.
Further, the ZrO 2 Is stable zirconium powder with purity not lower than 95% and granularity of 2-74 um.
Further, the alpha-Al 2 O 3 The purity is not lower than 98 percent, and the granularity is 2um-74um.
Further, the Al 2 O 3 The purity is not lower than 98 percent, and the granularity is 2um-10um.
Further, the SiO 2 The purity is not less than 95 percent, and the granularity is 2um-10um.
Further, said Y 2 O 3 The purity is not lower than 98 percent, and the granularity is 2um-10um.
Furthermore, the purity of the MgO is not lower than 98%, and the granularity is 2um-10um.
Further, al in the mullite crystal 2 O 3 、SiO 2 、K 2 The total content of 0, not less than 98wt%, and the granularity of 2-74 um.
A preparation method of a glass kiln material flowing nozzle brick comprises the following steps:
step one, making a working layer blank, and preparing ZrO from the working layer blank 2 70-95wt%、α-Al 2 O 3 15-20wt%、Al 2 O 3 3-5wt%、SiO 2 2-4wt%、Y 2 O 3 3-5wt% and 2-4wt% of MgO are mixed, injected into a working layer die cavity and compacted to obtain a working layer blank;
step two, shaping the working layer, namely naturally drying the blank of the working layer, then heating to 120 ℃, and keeping the constant temperature for 24 hours to obtain a shaping material of the working layer;
step three, sintering the working layer, heating to 1550-1590 ℃, and sintering for 15-20h to obtain a working layer prefabricated member;
step four, making a blank by using the whole brick, putting the working layer prefabricated part into a whole brick mould, and putting alpha-Al 2 O 3 10-15wt%、Al 2 O 3 5-8wt%、SiO 2 2-4wt% of mullite crystal and 70-80wt% of mullite crystal are injected into a die cavity of the whole brick die and are compacted to obtain a whole brick blank;
step five, shaping the whole brick, naturally drying the blank of the whole brick, heating to 120 ℃, and keeping the constant temperature for 24 hours to obtain a shaping material of the whole brick;
and sixthly, firing the whole brick, heating to 1200-1300 ℃, and sintering for 10-15h to obtain the material flowing nozzle brick of the glass kiln.
The invention has the beneficial effects that: the working layer has no low-melting-point glass phase, the zirconium dioxide content is high, the sintering temperature is high, the erosion resistance is far better than that of the fused AZS, the glass phase source of the fused cast zirconia-corundum brick is SiO 2 、Na 2 O reaction product at certain temperature, so that the fused cast zirconia-corundum brick contains about 20wt% of glass phase, and the measures for preventing the product from cracking in the brick making process are taken 2 、Na 2 The content of O component is very low, the product is produced by a sintering method, and almost no glass phase exists in the product, so that a working layer of the product has excellent molten glass corrosion resistance, zirconium dioxide is a main body for resisting molten glass corrosion, the strength of the molten glass corrosion resistance of the product is determined by the content of the zirconium dioxide in the product, the content of the zirconium dioxide in the fused cast zirconia corundum brick is 33wt%, the content of the zirconium dioxide in the working layer is 70-90wt%, the sintering temperature is a power source for promoting the solid phase reaction and the growth and growth of a crystalline phase of the working layer, the working layer is a suitable sintering temperature of 1550-1590 ℃ determined by multiple tests according to the components and properties of various materials, so that the optimal index and performance of the product are ensured, and a protective layer is a non-working part of the nozzle brick, is not in contact with molten glass, plays a role in supporting and protecting the working layer, is low in manufacturing cost, so that the overall cost of the composite nozzle brick is slightly higher than that the AZS based on the unique performance of the composite nozzle brick, compared with an AZS nozzle brick, the fused brick, the service life is long, and plays an important role in reducing the cost of glass enterprise, saving resources and improving social benefits of the glass enterprises.
Drawings
Fig. 1 is a schematic view of a spout brick structure.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In each of the following examples,
ZrO 2 the zirconium powder is stable zirconium powder with the purity of not less than 95 percent and the granularity of 2um-74um;
α-Al 2 O 3 the purity is not lower than 98 percent, and the granularity is 2um-74um;
Al 2 O 3 the purity is not lower than 98 percent, and the granularity is 2um-10um;
SiO 2 the purity is not lower than 95 percent, and the granularity is 2um-10um;
Y 2 O 3 the purity is not lower than 98 percent, and the granularity is 2um-10um;
the purity of MgO is not lower than 98%, and the granularity is 2um-10um;
al in mullite crystals 2 O 3 、SiO 2 、K 2 The total content of the three components 0 is not less than 98wt%, the granularity is 2um-74um;
preparing the working layer raw material and the protective layer raw material according to the designed weight proportion, respectively putting the working layer raw material and the protective layer raw material into a three-dimensional mixer, respectively, mixing for not less than 15h, taking out for later use,
the preparation method comprises the following steps of,
step one, preparing a working layer blank, namely putting the mixed raw materials of the working layer with the designed weight into a stirrer, stirring for more than 15 hours, injecting the mixture into a working layer mold cavity, and performing vibration molding by adopting a three-dimensional variable frequency vibrator for 10-15 minutes to obtain a working layer blank;
step two, shaping the working layer, namely naturally drying the blank of the working layer for 24-36h, then uniformly heating the blank from room temperature to 120 ℃ for 20h, keeping the temperature at 120 ℃ for 24h, and obtaining a shaping material of the working layer;
step three, sintering the working layer, namely putting the working layer sizing material into an electric heating furnace or a gas furnace for high-temperature calcination, heating the working layer sizing material to 1550-1590 ℃ from room temperature at a heating rate of 20-30 ℃/h, then sintering the working layer sizing material at a constant temperature for 15-20h, and naturally cooling the working layer sizing material to room temperature to obtain a working layer prefabricated member;
step four, making a blank by using a whole brick, namely putting the working layer prefabricated part into a whole brick mould, taking the mixed working layer raw materials with the designed weight, putting the mixed working layer raw materials into a stirrer, stirring for more than 15 hours, injecting the mixed raw materials into the whole brick mould, and performing vibration forming by using a three-dimensional variable frequency vibrator for 10-15 minutes to obtain a blank of the whole brick;
step five, shaping the whole brick, naturally drying the whole brick blank for 24-36h, then uniformly heating the whole brick blank to 120 ℃ from room temperature through 20h, keeping the temperature at 120 ℃ for 24h, and obtaining a shaping material of the whole brick;
and sixthly, firing the whole brick, putting the shaped material of the whole brick into an electric heating furnace or a gas furnace for high-temperature calcination, heating the shaped material of the whole brick to 1200-1300 ℃ from the room temperature at the heating rate of 15-20 ℃/h, then sintering the shaped material at the constant temperature for 10-15h, and naturally cooling the shaped material of the whole brick to the room temperature to obtain the material nozzle brick of the glass furnace.
Example 1
A glass kiln material flowing nozzle brick comprises an inner working layer and an outer protective layer, wherein the thickness of the working layer accounts for 30-40%, and the thickness of the protective layer accounts for 60-70%;
the working layer is made of the following raw materials in percentage by weight,
ZrO 2 70wt%；
α-Al 2 O 3 16wt%；
Al 2 O 3 5wt%；
SiO 2 4wt%；
Y 2 O 3 3wt%；
MgO 2wt%；
the protective layer is made of the following raw materials in percentage by weight,
α-Al 2 O 3 15wt%；
Al 2 O 3 5wt%；
SiO 2 5wt%；
75wt% of mullite crystals.
The detection structure is shown in attached table 1.
Example 2
A glass kiln material flowing nozzle brick comprises an inner working layer and an outer protective layer, wherein the thickness of the working layer accounts for 30-40%, and the thickness of the protective layer accounts for 60-70%;
the working layer is made of the following raw materials in percentage by weight,
ZrO 2 85wt%；
α-Al 2 O 3 5wt%；
Al 2 O 3 4wt%；
SiO 2 2wt%；
Y 2 O 3 3wt%；
MgO 1wt%；
the protective layer is made of the following raw materials in percentage by weight,
α-Al 2 O 3 14wt%；
Al 2 O 3 3wt%；
SiO 2 3wt%；
80wt% of mullite crystals.
The results are shown in the attached Table 1.
Attached table 1
The attached table 1 shows the performance test results of the present application,
wherein the apparent porosity detection execution standard is GB/T2997-2000;
the volume density detection execution standard is GB/T2997-2000;
the compression strength detection execution standard is GB/T5072.2-2004;
the thermal shock stability detection execution standard is YB/T376.1-1995.
The flow nozzle brick can be obtained from the attached table 1, and the rapid cooling and rapid heating performance and the molten glass erosion resistance of the flow nozzle brick are superior to those of a No. 33 electric melting zirconia-corundum brick.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (9)
1. The material flowing nozzle brick of the glass kiln is characterized by comprising an inner working layer and an outer protective layer, wherein the thickness of the working layer accounts for 30-40%, and the thickness of the protective layer accounts for 60-70%;
the working layer is made of ZrO from the following raw materials in percentage by weight 2 70-90wt%、α-Al 2 O 3 4-20wt%、Al 2 O 3 2-5wt%、SiO 2 1-3wt%、Y 2 O 3 1-3wt%、MgO 1-3wt%；
The protective layer is made of alpha-Al raw material in percentage by weight 2 O 3 10-20wt%、 Al 2 O 3 5-8wt%、SiO 2 2-4wt% and 70-80wt% of mullite crystal.
2. The glass kiln flow nozzle brick as defined in claim 1, wherein the ZrO2 2 Is stable zirconium powder with purity not lower than 95% and granularity of 2-74 um.
3. The glass kiln nozzle brick as defined in claim 1, wherein the α -Al is present in the form of a powder 2 O 3 The purity is not lower than 98 percent, and the granularity is 2um-74um.
4. The glass kiln nozzle brick as claimed in claim 1, characterized in that the Al is present in the form of a block 2 O 3 The purity is not lower than 98 percent, and the granularity is 2um-10um.
5. The glass kiln nozzle brick as claimed in claim 1, characterized in that the SiO 2 The purity is not less than 95 percent, and the granularity is 2um-10um.
6. The glass kiln nozzle brick as defined in claim 1, wherein the Y is 2 O 3 The purity is not less than 98 percent, and the granularity is 2um-10um.
7. The glass kiln flow nozzle brick according to claim 1, characterized in that the MgO purity is not less than 98% and the particle size is 2um-10um.
8. The glass kiln spout brick as defined in claim 1, wherein Al in the mullite crystal is present 2 O 3 、SiO 2 、K 2 The total content of 0, not less than 98wt%, and the granularity of 2-74 um.
9. The preparation method of the glass kiln material flowing nozzle brick is characterized by comprising the following steps:
step one, making a working layer blank, and preparing ZrO from the working layer blank 2 70-95wt%、α-Al 2 O 3 15-20wt%、Al 2 O 3 3-5wt%、SiO 2 2-4wt%、Y 2 O 3 3-5wt% and 2-4wt% of MgO, injecting into a working layer die cavity, and compacting to obtain a working layer blank;
step two, shaping the working layer, namely naturally drying the blank of the working layer, then heating to 120 ℃, and keeping the constant temperature for 24 hours to obtain a shaping material of the working layer;
step three, sintering the working layer, heating to 1550-1590 ℃, and sintering for 15-20h to obtain a working layer prefabricated member;
step four, making a blank by using the whole brick, putting the working layer prefabricated part into a whole brick mould, and putting alpha-Al 2 O 3 10-15wt%、Al 2 O 3 5-8wt%、SiO 2 2-4wt% of mullite crystal and 70-80wt% of mullite crystal are injected into a die cavity of the whole brick die and are compacted to obtain a whole brick blank;
step five, shaping the whole brick, naturally drying the blank of the whole brick, heating to 120 ℃, and keeping the constant temperature for 24 hours to obtain a shaping material of the whole brick;
and sixthly, firing the whole brick, heating to 1200-1300 ℃, and sintering for 10-15h to obtain the material flowing nozzle brick of the glass kiln.
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| 谢金莉;李坤明;李春燕;李丽萍;薛飞;潘传才;林国伟;张林林;: "熔铸AZS耐火材料的组成、性能与结构", 硅酸盐通报, no. 09, pages 2432 - 2435 * |
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