CN115448709A - Anti-erosion rotating pipe for glass kiln pipe drawing machine and preparation method thereof - Google Patents
Anti-erosion rotating pipe for glass kiln pipe drawing machine and preparation method thereof Download PDFInfo
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- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
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- C03B17/00—Forming molten glass by flowing-out, pushing-out, extruding or drawing downwardly or laterally from forming slits or by overflowing over lips
- C03B17/04—Forming tubes or rods by drawing from stationary or rotating tools or from forming nozzles
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- 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B2235/3248—Zirconates or hafnates, e.g. zircon
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- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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Abstract
The invention relates to an anti-erosion rotary tube for a tube drawing machine of a glass kiln, which is characterized in that electric melting zirconium mullite and zircon powder are added into components through component design and raw material optimization, so that the service life of the rotary tube is prolonged, and the yield of glass tube products is improved.
Description
Technical Field
The invention relates to the technical field of glass forming and manufacturing, in particular to an anti-corrosion rotary pipe for a glass kiln pipe drawing machine and a preparation method thereof.
Background
The rotary tube is a main component of a glass tube drawing system, and is required to have good erosion resistance in the use process, so that the pollution of stripes, stones, bubbles and the like to glass liquid caused by dissolution of erosion substances is avoided when the glass tube is drawn, and the glass tube has good thermal shock resistance. The rotary tube technology for the glass kiln tube drawing machine is slow in iteration, and the used materials of the rotary tube technology undergo the development process of flint clay, sillimanite, mullite and corundum-mullite complex phase materials. At present, corundum-mullite multiphase material rotating pipes are mainstream products, and the components of the corundum-mullite multiphase material rotating pipes comprise corundum phase, mullite, quartz phase and amorphous phase. In the using process, particularly when special glass with complex components is drawn, the harsh conditions of high alkali content and high working temperature are met, at the moment, amorphous phase in the rotating tube is easy to separate out (the separation temperature is about 1350 ℃) and enters glass liquid, and a cavity is left in the rotating tube; the alkali oxides contained in the molten glass easily corrode the rotary tube, and the corroded substances enter the molten glass to cause pollution. Therefore, when the temperature of the glass liquid is increased or the alkali content is increased, the service life is greatly reduced, the production continuity is influenced by frequently replacing the rotating pipe, and the production efficiency is reduced.
The refractory material for the rotary tube of the glass kiln has small market capacity, and the technical research literature on the rotary tube in China is few. In the early days, a few documents describe that the rotary tube material which takes sillimanite and flint stone as main materials is prepared by adopting methods such as ramming, vacuum casting and the like, and no relevant patent is found. Some patents on the aspect of the rotary tube mainly focus on the structural design, such as a ceramic rotary tube for glass drawing tube (publication number CN 201224706Y), a rotary tube for glass horizontal drawing tube machine (publication number CN 203922982U), and a glass kiln forming rotary tube device (publication number CN 204509099U).
The inventor carries out a series of researches on a rotary tube of a glass kiln tube drawing machine, and partial patents are published in the early period, wherein CN114478038A uses high-purity mullite, sillimanite, andalusite and bonding clay as raw materials, and the rotary tube is prepared by mixing, cold isostatic pressing and high-temperature heat treatment and can resist the corrosion of alkaline oxides in molten glass, but the apparent porosity is slightly high, and the thermal shock resistance and the high-temperature resistance are required to be further improved, CN114988894A uses high-purity sintered mullite with different granularities as a main raw material and introduces a certain content of cordierite pre-synthesis powder, the cordierite pre-synthesis powder is subjected to high-temperature in-situ reaction to form a cordierite phase, and forms micro-scale combination with the original mullite phase, and the multiphase material has the advantages of mullite and cordierite, namely lower volume density, lower thermal expansion coefficient and higher thermal shock resistance, but the performance is required to be improved when the multiphase material is used for special high-alkali glass.
Disclosure of Invention
Aiming at the defects in the prior art, the invention designs the anti-corrosion rotary tube for the tube drawing machine of the glass kiln through component design and raw material optimization, which is beneficial to prolonging the service life of the rotary tube, maintaining the production continuity of the glass tube and improving the yield of glass tube products.
Specifically, the anti-erosion rotary tube for the glass kiln tube drawing machine is composed of the following raw materials in parts by weight:
20 to 50 weight percent of high-purity sintered mullite,
15-30wt% of electric melting mullite,
5-25wt% of fused zirconia mullite,
5-25wt% of zircon,
5-15w% of alumina micro powder,
8-15wt% of bound clay.
Preferably, the anti-corrosion rotating pipe for the glass kiln tube drawing machine is composed of the following raw materials in parts by weight:
20 to 50 weight percent of high-purity sintered mullite,
15-30wt% of electric melting mullite,
10-25wt% of fused zirconia mullite,
10-25wt% of zircon,
5-15w% of alumina micro powder,
8-15wt% of bound clay.
Preferably, the main chemical component of the high-purity mullite is Al 2 O 3 ：65-75wt％，SiO 2 :25 to 30 weight percent, the granularity is respectively 1 to 0.5mm,0.5 to 0.2mm, less than or equal to 0.074mm and less than or equal to 0.044mm.
Preferably, the main chemical component of the electrofused mullite is Al 2 O 3 ：69-71wt％，SiO 2 :26 to 28 weight percent, the granularity is respectively 0.2 to 0mm, less than or equal to 0.074mm and less than or equal to 0.044mm.
Preferably, the main chemical component of the zircon is ZrO 2 ：62-66wt％，SiO 2 :30-34wt% and the granularity is less than or equal to 0.088mm.
It is preferable to useThe main chemical component of the alumina micro powder is Al 2 O 3 More than or equal to 99.5w percent and the granularity is less than or equal to 5 mu m.
Preferably, the main chemical component of the bonding clay is Al 2 O 3 ：30-40wt％，SiO 2 :45-60wt% and the granularity is less than or equal to 0.044mm.
The invention also relates to a preparation method of the anti-corrosion rotary pipe for the glass kiln pipe drawing machine, which comprises the following steps:
1) Weighing the raw materials according to the proportion,
2) Adding the raw materials into a stirring pot for dry mixing, adding a bonding agent accounting for 2-5w% of the total weight of the raw materials, putting the raw materials into a wet mill for wet mixing to obtain a wet mixed material,
3) Carrying out cold isostatic pressing on the wet mixed material to obtain a green body,
4) And drying the blank, and then placing the blank in an electric furnace for heat treatment to obtain the anti-erosion rotating pipe.
Preferably, the dry mixing time in the step 2) is 5 to 10 minutes, and the specific gravity of the binding agent is 1.15 to 1.30g/cm 3 The wet mixing time of the dextrin solution is 10-15 minutes.
Preferably, the cold isostatic compaction pressure in the step 3) is 200MPa, the drying condition in the step 4) is 110 ℃ multiplied by 24h, the heat treatment temperature is 1550-1580 ℃, and the heat treatment time is 6-10h.
The invention relates to an anti-erosion rotary tube for a glass kiln tube drawing machine, which is obtained by taking high-purity mullite with different particle sizes as main aggregate, introducing a certain amount of zirconium-containing fine powder such as electrofused zirconium mullite, zirconite and the like, taking soft clay as a bonding agent, and carrying out mixing, molding and high-temperature heat treatment. The aggregate of the rotating tube is high-purity sintered mullite, the matrix contains composite phases such as fused mullite, fused zirconium mullite and the like, the material of the composite phase material is pure, the dissolution temperature of the contained amorphous phase is high, and the composite phase material has a low thermal expansion coefficient, high thermal shock resistance and excellent erosion resistance. The prepared zirconium mullite rotary tube does not crack in the using process, does not pollute molten glass, has long service life and high production efficiency of the glass tube.
The existing common corundum-mullite rotating tube has the defects of generation of stones, bubbles and the like in molten glass due to dissolution of a low-melting-point amorphous phase contained in the rotating tube in the long-term use process, particularly in the later use stage, and the dissolved rotating tube has a loose structure, is reduced in strength and is easy to damage. The electrofused material introduced into the rotary tube has unique advantages in the aspect of erosion resistance, the electrofused zirconium mullite material is rich in large grains, high in purity and less in intercrystalline vitreous quality, the dissolution temperature of the amorphous phase contained in the electrofused zirconium mullite material is high, the erosion resistance is good, bubbles cannot be brought to molten glass, and the pollution to the molten glass is small. According to the invention, by means of component design and raw material optimization, the fused zirconia-mullite and zircon powder are added into the components to prepare the anti-erosion rotary tube, so that the service life of the rotary tube is prolonged, and the yield of glass tube products is increased.
Through detection, the volume density of the anti-erosion rotating pipe is 2.90-3.30g/cm 3 Within the range of 15% to 20% porosity. After 48h of the insert-method alkaline etching test, no macroscopic etching surface of the sample occurs. The material is suitable for materials for glass kiln rotary tubes.
Detailed Description
Example 1
An anti-erosion rotating pipe for a glass kiln pipe drawing machine is prepared by weighing raw materials according to the proportion of 40wt% of high-purity sintered mullite, 20wt% of fused mullite, 10wt% of fused zirconium mullite, 10wt% of zirconite, 8wt% of alumina micro powder and 12wt% of combined clay, adding the raw materials into a stirring pot for dry mixing for 8 minutes, adding dextrin solution accounting for 3w% of the total weight of the raw materials, wet mixing in a wet mill for 12 minutes to obtain a wet mixed material, carrying out cold isostatic pressing on the wet mixed material under 200MPa to obtain a blank body, drying the blank body, and then placing the blank body in an electric furnace for heat treatment at 1580 ℃ for 6 hours to obtain the anti-erosion rotating pipe. And (3) detecting to obtain: the bulk density is 3.21g/cm 3 The apparent porosity is 17%; after 48h of the embedded part method alkali etching experiment, no macroscopic corrosion damage surface occurs to the sample.
Example 2
An anti-erosion rotary tube for a tube drawing machine of a glass kiln comprises 40wt% of high-purity sintered mullite, 15wt% of fused mullite, 10wt% of fused zirconia mullite, 15wt% of zirconite and 10wt% of aluminaWeighing the raw materials according to the proportion of the micro powder and 10wt% of the combined clay, adding the raw materials into a stirring pot for dry mixing for 9 minutes, adding a dextrin solution accounting for 3w% of the total weight of the raw materials, putting the mixture into a wet mill for wet mixing for 13 minutes to obtain a wet mixed material, carrying out cold isostatic pressing on the wet mixed material under 200MPa to obtain a blank body, drying the blank body, and then placing the blank body into an electric furnace for heat treatment at 1580 ℃ for 6 hours to obtain the anti-erosion rotary pipe. And (3) detecting to obtain: the bulk density is 3.01g/cm 3 The apparent porosity is 18%; after 48h of the embedded part method alkali etching experiment, no macroscopic corrosion damage surface occurs to the sample.
Example 3
An anti-erosion rotating tube for a tube drawing machine of a glass kiln is prepared by weighing raw materials according to the proportion of 30wt% of high-purity sintered mullite, 20wt% of fused mullite, 15wt% of fused zirconium mullite, 15wt% of zircon quartz, 8wt% of alumina micro powder and 12wt% of combined clay, adding the raw materials into a stirring pot for dry mixing for 8 minutes, adding a dextrin solution accounting for 3w% of the total weight of the raw materials, putting the mixture into a wet mill for wet mixing for 11 minutes to obtain a wet mixed material, carrying out cold isostatic pressing on the wet mixed material under 200MPa to obtain a blank body, drying the blank body, and then placing the blank body in an electric furnace for heat treatment at 1580 ℃ for 6 hours to obtain the anti-erosion rotating tube. And (3) detecting to obtain: the bulk density is 3.16g/cm 3 The apparent porosity is 17%; after 48h of the embedded part method alkali etching experiment, no macroscopic corrosion damage surface occurs to the sample.
Comparative example 1
A rotary tube for a glass kiln tube drawing machine is prepared by weighing raw materials according to the proportion of 40wt% of high-purity sintered mullite, 45wt% of alumina micro powder and 15wt% of combined clay, adding the raw materials into a stirring pot for dry mixing for 8 minutes, adding dextrin solution accounting for 3w% of the total weight of the raw materials, putting the mixture into a wet mill for wet mixing for 12 minutes to obtain wet mixed materials, carrying out cold isostatic pressing on the wet mixed materials under 200MPa to obtain a blank body, drying the blank body, and then putting the blank body into an electric furnace for heat treatment at 1580 ℃ for 6 hours to obtain the rotary tube. And (3) detecting to obtain: the bulk density is 2.86g/cm 3 The apparent porosity is 28%; after 48h of the embedded part method alkali etching experiment, the sample generates a macroscopic corrosion damaged surface.
Comparative example 2
The height of the rotating tube for the tube drawing machine of the glass kiln is 40wt%Weighing the raw materials of pure sintered mullite, 15wt% of fused mullite, 10wt% of fused zirconia mullite, 20wt% of alumina micro powder and 15wt% of combined clay, adding the raw materials into a stirring pot for dry mixing for 8 minutes, adding dextrin solution accounting for 3w% of the total weight of the raw materials, putting the mixture into a wet mill for wet mixing for 12 minutes to obtain a wet mixed material, carrying out cold isostatic pressing on the wet mixed material under 200MPa to obtain a blank body, drying the blank body, and then putting the blank body into an electric furnace for heat treatment at 1580 ℃ for 6 hours to obtain the rotary tube. And (3) detecting to obtain: the bulk density is 2.97g/cm 3 The apparent porosity is 24%; after 48h of the embedded part method alkali etching experiment, the sample generates a slight macroscopic erosion damaged surface.
Comparative example 3
A rotary tube for a glass kiln tube drawing machine is prepared by weighing raw materials according to the proportion of 30wt% of high-purity sintered mullite, 20wt% of fused mullite, 15wt% of zircon, 20wt% of alumina micro powder and 15wt% of combined clay, adding the raw materials into a stirring pot for dry mixing for 8 minutes, adding a dextrin solution accounting for 3w% of the total weight of the raw materials, putting the mixture into a wet mill for wet mixing for 12 minutes to obtain a wet mixed material, carrying out cold isostatic pressing on the wet mixed material under 200MPa to obtain a blank body, drying the blank body, and then putting the blank body into an electric furnace for heat treatment at 1580 ℃ for 6 hours to obtain the rotary tube. And (3) detecting to obtain: the bulk density is 3.05g/cm 3 The apparent porosity is 22%; after 48h of the embedded part method alkali etching experiment, the sample generates a slight macroscopic erosion damaged surface.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. An anti-erosion rotary pipe for a glass kiln pipe drawing machine is characterized by comprising the following raw materials in parts by weight:
20 to 50 weight percent of high-purity sintered mullite,
15-30wt% of electric melting mullite,
5-25wt% of electrically fused zirconium mullite,
5-25wt% of zircon,
5-15w% of alumina micro powder,
8-15wt% of bound clay.
2. The erosion-resistant rotary pipe for the glass kiln tube drawing machine according to claim 1, which is characterized by comprising the following raw materials in parts by weight:
20-50wt% of high-purity sintered mullite,
15-30wt% of electric melting mullite,
10-25wt% of electrically fused zirconium mullite,
10-25wt% of zircon,
5-15w% of alumina micro powder,
8-15wt% of bound clay.
3. The erosion resistant rotary tube for a glass furnace tube drawing machine according to claim 1, wherein a main chemical component of the high-purity mullite is Al 2 O 3 ：65-75wt％，SiO 2 :25 to 30 weight percent of the total grain size, the grain size is 1 to 0.5mm,0.5 to 0.2mm, less than or equal to 0.074mm and less than or equal to 0.044mm respectively.
4. The erosion resistant rotary tube for a glass kiln tube drawing machine as defined in claim 1, wherein the fused mullite is made of Al as a main chemical component 2 O 3 ：69-71wt％，SiO 2 :26 to 28 weight percent, the granularity is respectively 0.2 to 0mm, less than or equal to 0.074mm and less than or equal to 0.044mm.
5. The erosion resistant rotary pipe for a glass pulling machine according to claim 1, wherein the main chemical component of zircon is ZrO 2 ：62-66wt％，SiO 2 :30-34wt% and the granularity is less than or equal to 0.088mm.
6. The glass of claim 1The corrosion-resistant rotary pipe for the kiln tube drawing machine is characterized in that the main chemical component of the alumina micro powder is Al 2 O 3 More than or equal to 99.5w percent and the granularity is less than or equal to 5 mu m.
7. The erosion resistant rotary pipe for a glass tube drawing machine according to claim 1, wherein a main chemical component of said bonding clay is Al 2 O 3 ：30-40wt％，SiO 2 :45-60wt% and the granularity is less than or equal to 0.044mm.
8. The method for producing an erosion resistant rotary pipe for a glass-furnace drawing machine according to any one of claims 1 to 7, characterized by comprising the steps of:
1) Weighing the raw materials according to the mixture ratio,
2) Adding the raw materials into a stirring pot for dry mixing, adding a bonding agent accounting for 2-5w% of the total weight of the raw materials, putting the raw materials into a wet mill for wet mixing to obtain a wet mixed material,
3) Carrying out cold isostatic pressing on the wet mixed material to obtain a green body,
4) And drying the blank, and then placing the blank in an electric furnace for heat treatment to obtain the anti-erosion rotating pipe.
9. The method for manufacturing an anti-erosion rotary pipe for a glass kiln pipe drawing machine according to claim 8, wherein the dry-blending time in the step 2) is 5 to 10 minutes, and the specific gravity of the binder is 1.15 to 1.30g/cm 3 The wet mixing time of the dextrin solution is 10-15 minutes.
10. The method for manufacturing an anti-erosion rotary tube for a glass kiln tube drawing machine according to claim 8, wherein the cold isostatic compaction pressure in step 3) is 200MPa, the drying condition in step 4) is 110 ℃ x 24h, the heat treatment temperature is 1550-1580 ℃, and the heat treatment time is 6-10h.
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| CN202211295189.2A CN115448709A (en) | 2022-10-21 | 2022-10-21 | Anti-erosion rotating pipe for glass kiln pipe drawing machine and preparation method thereof |
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| CN202211295189.2A CN115448709A (en) | 2022-10-21 | 2022-10-21 | Anti-erosion rotating pipe for glass kiln pipe drawing machine and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116161862A (en) * | 2023-01-05 | 2023-05-26 | 郑州方铭高温陶瓷新材料有限公司 | Rotary tube for preparing special glass and preparation method thereof |
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| CN109336575A (en) * | 2018-10-26 | 2019-02-15 | 淄博工陶耐火材料有限公司 | One kind re-sintering electric cast mullite brick and preparation method thereof containing zirconium |
| CN112573932A (en) * | 2020-12-16 | 2021-03-30 | 淄博工陶新材料集团有限公司 | Homogeneous body re-sintered fused zirconia mullite brick and preparation method thereof |
| CN114478038A (en) * | 2022-04-02 | 2022-05-13 | 湖南旗滨医药材料科技有限公司 | Alkali-corrosion-resistant refractory material for rotary tube of glass kiln tube drawing machine and preparation method thereof |
| CN114988894A (en) * | 2022-06-07 | 2022-09-02 | 湖南旗滨医药材料科技有限公司 | Light thermal shock-resistant mullite cordierite rotary tube and preparation method thereof |
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| CN112573932A (en) * | 2020-12-16 | 2021-03-30 | 淄博工陶新材料集团有限公司 | Homogeneous body re-sintered fused zirconia mullite brick and preparation method thereof |
| CN114478038A (en) * | 2022-04-02 | 2022-05-13 | 湖南旗滨医药材料科技有限公司 | Alkali-corrosion-resistant refractory material for rotary tube of glass kiln tube drawing machine and preparation method thereof |
| CN114988894A (en) * | 2022-06-07 | 2022-09-02 | 湖南旗滨医药材料科技有限公司 | Light thermal shock-resistant mullite cordierite rotary tube and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116161862A (en) * | 2023-01-05 | 2023-05-26 | 郑州方铭高温陶瓷新材料有限公司 | Rotary tube for preparing special glass and preparation method thereof |
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