CN114249531B - Preparation method of high silica glass melt capable of improving liquid level melting capacity - Google Patents
Preparation method of high silica glass melt capable of improving liquid level melting capacity Download PDFInfo
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- CN114249531B CN114249531B CN202111555539.XA CN202111555539A CN114249531B CN 114249531 B CN114249531 B CN 114249531B CN 202111555539 A CN202111555539 A CN 202111555539A CN 114249531 B CN114249531 B CN 114249531B
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- powder
- glass
- melting
- mirabilite
- silica glass
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002844 melting Methods 0.000 title claims abstract description 34
- 230000008018 melting Effects 0.000 title claims abstract description 34
- 239000007788 liquid Substances 0.000 title claims abstract description 33
- 239000000156 glass melt Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 43
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 30
- 239000010446 mirabilite Substances 0.000 claims abstract description 23
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 22
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 22
- 239000006004 Quartz sand Substances 0.000 claims description 12
- 229910052656 albite Inorganic materials 0.000 claims description 12
- 229910021538 borax Inorganic materials 0.000 claims description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 11
- 239000004327 boric acid Substances 0.000 claims description 11
- 235000010338 boric acid Nutrition 0.000 claims description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- 239000004317 sodium nitrate Substances 0.000 claims description 11
- 235000010344 sodium nitrate Nutrition 0.000 claims description 11
- 239000004328 sodium tetraborate Substances 0.000 claims description 11
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000012163 sequencing technique Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 abstract description 7
- 235000011152 sodium sulphate Nutrition 0.000 abstract description 7
- 229910002651 NO3 Inorganic materials 0.000 abstract description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011449 brick Substances 0.000 abstract description 4
- 239000002344 surface layer Substances 0.000 abstract description 4
- 230000003628 erosive effect Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 230000002950 deficient Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 description 3
- 239000003643 water by type Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/235—Heating the glass
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
Abstract
A preparation method of high silica glass melt capable of improving the melting capacity of a liquid level is characterized in that mirabilite with the mass percentage of 0.10-0.50 is added into high silica glass powder so as to improve the melting capacity of the liquid level of glass. The sodium sulfate in the mirabilite is melted at 884 ℃, and as the melting amount of the sodium sulfate in the high silica glass is only 0.2 percent, the sodium sulfate which is not melted into the glass floats on the melted glass and is positioned below the powder and boils between the glass and the powder, the heat conduction between the glass liquid and the powder is enhanced, and the melting of the powder is accelerated. The invention strictly controls the adding amount of mirabilite, avoids the appearance of surface layer nitrate water on the glass liquid surface, effectively avoids the phenomenon that the surface layer nitrate water is burst when meeting water in a kiln, corrects the safety of the kiln, ensures that the melting performance of the glass liquid surface is improved, thins a raw material layer, does not generate a material covering, reduces the erosion of kiln bricks and improves the quality of the glass under the condition that the performance of the glass is not influenced.
Description
Technical Field
The invention relates to the field of glass manufacturing, in particular to the field of high silica glass electric melting furnaces, and discloses a preparation method of high silica glass with good glass liquid level meltability.
Background
Compared with common glass, the high silica glass has stronger mechanical property and thermal stability, and has higher high temperature resistance after special treatment, thereby being widely applied to the fields of aerospace and military. During the production of this glass, B is contained in the components 2 O 3 The content exceeds 20%, boron volatilizes seriously during high-temperature melting, so that the production does not generally adopt a flame kiln, but the glass melting is realized by heating the inside of the glass by utilizing the conductive characteristic of the glass in a high-temperature state, namely, the production adopts an electric melting cold top kiln technology.
When the electric melting cold top kiln technology is used for production, the kiln glass liquid surface is internally melted, so that the material layer is thicker, the inside is bonded, and the escaping gas cannot be released in time, so that the escaping gas is gathered to form small air holes to prevent heat conduction. Powder is piled up on the glass liquid surface of the kiln to form a crust, and the crust appears to prevent the upper layer powder from melting. At this time, if the internal glass liquid temperature is increased only by increasing the current, not only the intensity of the increase of the melting of the glass liquid surface is not great, but also the internal glass liquid temperature is increased, so that the erosion of the kiln brick material is aggravated, and the glass quality is seriously affected.
The invention of CN102643022A and the invention of CN103864295A respectively disclose a preparation method of high silica glass. The two inventions disclosed in the two inventions do not relate to the problems that the kiln glass liquid surface raw material layer is thicker, powder is piled on the kiln glass liquid surface to form a hard shell, and the material is fluffy, so that the corrosion of kiln brick materials is aggravated, and the quality of glass is affected.
Disclosure of Invention
In order to solve the problems that the high silica glass has thicker raw material layer and is easy to generate the material filling during the production of the electric melting cold top kiln technology, the erosion of kiln bricks is aggravated, and the quality of the glass is affected. The invention provides a preparation method of high silica glass melt capable of improving the liquid level melting capacity.
The specific process of the invention is as follows:
step one, weighing powder:
the glass powder consists of quartz sand, borax, boric acid, albite, sodium carbonate, sodium nitrate and mirabilite, wherein the quartz sand is 45.0-45.6%, the borax is 22.5-22.7%, the boric acid is 21.9-22.5%, the albite is 4.8-5.3%, the sodium carbonate is 2.3-2.6%, the sodium nitrate is 2.0-2.1%, and the mirabilite is 0.10-0.50%. The percentages are mass percentages.
The quartz sand and albite are required to pass through 100 meshes; the borax, boric acid, sodium carbonate, sodium nitrate and mirabilite are required to pass through 10 meshes.
Step two, mixing powder:
and starting the forced mixer. And (3) sequencing the weighed powder according to quartz sand, borax, boric acid, albite, sodium carbonate, sodium nitrate and mirabilite, and sequentially putting the powder into a forced mixer with the rotating speed of 40-50 r/min from a feed inlet. And after the last powder is put into the mixer, continuing stirring for 10-20 min, and stopping stirring to obtain the mixed powder.
Step 3, melting high silica glass melt:
lifting a charging bucket filled with the powder to an upper opening of a charging machine; the feeder feeds the mixed powder into the front end of the glass liquid surface of the kiln at a speed of 5 r/min.
And (3) electrically heating the powder added into the kiln, and melting at high temperature to obtain high-silica glass melt.
The temperature for melting the powder is 1400-1600 ℃.
The method is to add mirabilite into glass powder to improve the melting capacity of the glass liquid level.
The chemical raw material selected by the invention is mirabilite, also known as sodium sulfate decahydrate (Na) 2 SO 4 ·10H 2 O), white fine-grained crystals or powders, are readily soluble in water, hygroscopic, odorless, nontoxic. Because the mass percentage of the introduced mirabilite is only 0.10 to 0.50 percent of that of the batch, and the mirabilite also contains ten structural waters which are decomposed at high temperature, na is introduced 2 SO 4 Only 0.044-0.22% of the batch, and the influence on the glass component is basically negligible.
Natrii sulfas (Na) 2 SO 4 ·10H 2 O) is first to lose ten structural waters (10H) at 32.38 DEG C 2 O), the structural water can stir the upper layer glass liquid during gasification, which is favorable for melting. Sodium sulfate (Na) which lost structural water at 884 ℃ 2 SO 4 ) Because the melting amount of sodium sulfate in the high silica glass is only 0.2%, sodium sulfate which is not melted into the glass floats on the melted glass and is positioned below the powder and boils between the glass and the powder, the heat conduction between the glass liquid and the powder is enhanced, and the melting of the powder is accelerated.
Meanwhile, in order to ensure that the heat of the glass liquid surface is lost as little as possible and no material filling phenomenon occurs, the ratio of the glass liquid surface raw material layer is more than 60 percent. In addition, as the melting amount of sodium sulfate in the high silica glass is only 0.2%, when the melting amount exceeds 0.2%, the glass liquid surface can generate nitrate water, and at the moment, although the glass liquid surface is well melted, the surface layer nitrate water can generate a burst phenomenon when meeting water in a kiln, so that the safety of the kiln is seriously influenced.
The invention comprehensively considers various factors, and only 0.10 to 0.50 percent of mirabilite (Na) is added in the production of the high silica glass 2 SO 4 ·10H 2 O) can achieve the purpose: the thickness of the raw material layer is less than 15cm, the ratio of the glass liquid surface raw material layer is more than 60%, no material filling phenomenon occurs, and the ratio of defective glass is less than 30%.
The comparison of the data for the improvement in glass melting ability after addition of mirabilite is shown in Table 1:
table 1 comparison table
| Test number | 0# | 1# | 2# | 3# |
| Natrii sulfas adding amount | 0 | 0.50％ | 0.30％ | 0.10％ |
| Thickness of raw material layer (cm) | 15 | 10 | 8 | 11 |
| Glass liquid surface layer ratio (%) | 100 | 80 | 70 | 75 |
| Awning material | Has the following components | Without any means for | Without any means for | Without any means for |
| Defective glass ratio (%) | 30 | 5 | 3 | 3.5 |
Note that: the sample # 0 in table 1 is obtained by the prior art, and the samples # 1 to # 3 are obtained according to the present invention.
As can be seen from the experimental data in Table 1, after the mirabilite is added, the thickness of the material layer in the kiln is obviously reduced, the phenomenon of filling is eliminated, and the defective rate of the glass is reduced to be less than one sixth of that when the mirabilite is not added.
Detailed Description
The invention relates to a preparation method of high silica glass with good glass liquid level meltability, which comprises the following specific processes:
step one, weighing powder:
the glass powder consists of quartz sand, borax, boric acid, albite, sodium carbonate, sodium nitrate and mirabilite, wherein the quartz sand is 45.0-45.6%, the borax is 22.5-22.7%, the boric acid is 21.9-22.5%, the albite is 4.8-5.3%, the sodium carbonate is 2.3-2.6%, the sodium nitrate is 2.0-2.1%, and the mirabilite is 0.10-0.50%. The percentages are mass percentages. Wherein, the quartz sand and the albite are required to pass through 100 meshes, and the rest materials are required to pass through 10 meshes.
The proportions of the glass powder materials of the examples in the invention are shown in Table 2
TABLE 2 proportioning of glass powders
Step two, mixing powder:
starting the forced mixer to rotate at a speed of 40-50 r/min. And (3) sequencing the weighed powder according to quartz sand, borax, boric acid, albite, sodium carbonate, sodium nitrate and mirabilite, and sequentially putting the powder into a rotary forced mixer from a feed inlet. And after the last powder is put into the mixer, continuing stirring for 10-20 min, and stopping stirring to obtain the mixed powder.
Step three, melting high silica glass melt:
opening a discharging hole of the forced mixer; and (5) placing the mixed powder into a charging bucket and transporting the powder to a kiln charging platform for standby. And (3) hanging a charging bucket to be used on an upper opening of a charging machine, and feeding the mixed powder into the front end of the glass liquid surface of the kiln at a speed of 5r/min by the charging machine.
And (3) electrically heating the powder added into the kiln to 1400-1600 ℃ and melting to obtain high silica glass melt.
Table 3 process parameters of the examples
| Process for producing a solid-state image sensor | Unit (B) | Example 1 | Example 2 | Example 3 |
| Rotation speed of forced mixer | r/min | 40 | 50 | 45 |
| Stirring time of the mixed powder | min | 16 | 12 | 20 |
| Temperature of the melted powder | ℃ | 1600 | 1500 | 1400 |
The invention tests the melting condition of the liquid level of the high silica glass after adopting each of the examples, and the results are shown in Table 4:
table 4 glass level melting test
Namely, only 0.10 to 0.50 percent of mirabilite (Na) is added in the production of the high silica glass 2 SO 4 ·10H 2 O), namely the purposes that the thickness of the raw material layer is smaller than 15cm, the ratio of the glass liquid surface raw material layer is more than 60 percent, no material is added, and the ratio of the defective glass is smaller than 30 percent are realized.
Claims (2)
1. A preparation method of high silica glass melt capable of improving liquid level melting capacity is characterized by comprising the following specific steps:
step one, weighing powder:
the glass powder consists of quartz sand, borax, boric acid, albite, sodium carbonate, sodium nitrate and mirabilite, wherein the quartz sand is 45.0-45.6%, the borax is 22.5-22.7%, the boric acid is 21.9-22.5%, the albite is 4.8-5.3%, the sodium carbonate is 2.3-2.6%, the sodium nitrate is 2.0-2.1, and the mirabilite is 0.10-0.50%; wherein the percentage is mass percentage;
the quartz sand and albite are required to pass through 100 meshes; the borax, boric acid, sodium carbonate, sodium nitrate and mirabilite are required to pass through 10 meshes;
step two, mixing powder:
starting a forced mixer; sequencing the weighed powder according to quartz sand, borax, boric acid, albite, sodium carbonate, sodium nitrate and mirabilite, and sequentially putting the powder into a forced mixer with the rotating speed of 40-50 r/min from a feed inlet; after the last powder is put into the mixer, stirring is continued for 10-20 min, and stirring is stopped to obtain mixed powder;
step 3, melting high silica glass melt:
lifting a charging bucket filled with the powder to an upper opening of a charging machine; the feeding machine feeds the mixed powder into the front end of the glass liquid surface of the kiln at the speed of 5 r/min;
and (3) electrically heating the powder added into the kiln, and melting at high temperature to obtain high-silica glass melt.
2. The method for producing a high silica glass melt capable of improving the melting ability of a liquid surface according to claim 1, wherein the temperature at which the powder is melted is 1400 to 1600 ℃.
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| CN202111555539.XA CN114249531B (en) | 2021-12-17 | 2021-12-17 | Preparation method of high silica glass melt capable of improving liquid level melting capacity |
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| CN114249531A CN114249531A (en) | 2022-03-29 |
| CN114249531B true CN114249531B (en) | 2024-01-19 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85103433A (en) * | 1985-04-15 | 1986-12-31 | 中国科学院上海硅酸盐研究所 | Recrystallization temperature is higher than the manufacture method of the high temp glass of silica glass |
| CN1618759A (en) * | 2004-11-05 | 2005-05-25 | 中国科学院上海光学精密机械研究所 | Preparation method of low ultraviolet absorption multipore and poreless high silica glass |
| CN102730967A (en) * | 2012-06-29 | 2012-10-17 | 中国科学院上海光学精密机械研究所 | Preparation method for sensitization-enhanced green light-emitting high-silica glass |
| CN103864295A (en) * | 2014-03-07 | 2014-06-18 | 陕西科技大学 | Preparation method of high silica glass |
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2021
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