CN115159839A - Method for improving melting clarification quality of neutral medicinal glass - Google Patents
Method for improving melting clarification quality of neutral medicinal glass Download PDFInfo
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- CN115159839A CN115159839A CN202210759761.XA CN202210759761A CN115159839A CN 115159839 A CN115159839 A CN 115159839A CN 202210759761 A CN202210759761 A CN 202210759761A CN 115159839 A CN115159839 A CN 115159839A
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- 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
- C03C1/004—Refining agents
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- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention provides a method for improving the melting and clarifying quality of neutral medicinal glass, which achieves the aim of improving the melting and clarifying of the neutral medicinal glass mainly by adding a composite clarifying agent in the preparation process and controlling the ratio of FeO to total iron in the neutral medicinal glass in the melting process. The compound clarifying agent comprises the following components of basic zinc carbonate, sodium chloride, sodium nitrate and cerium dioxide. When the method is adopted to produce the neutral medicinal glass, the viscosity and the surface tension of the glass can be reduced, the bubbles can be quickly eliminated, the discharge and the release of the bubbles during the glass melting are facilitated, the melting temperature is reduced, the generation of defects during the glass melting is avoided, and the product quality of the glass is improved. The method avoids the emission of sulfides in the glass production, does not contain toxic substances, saves energy, has simple process, and is suitable for the actual production of neutral medicinal glass.
Description
Technical Field
The invention relates to the field of glass preparation methods, in particular to a method for improving the melting clarification quality of neutral medicinal glass.
Background
The medicinal glass is glass specially used for medicine packaging, and has international standardISO12775-1997 glass for normal large-scale production classified according to components and test method thereof divides medicinal glass into borosilicate glass, neutral glass and soda-lime glass, wherein the neutral glass is good in chemical stability and does not send chemical reaction with liquid medicine in the long-term contact process of a glass container and the liquid medicine, and neutral glass bottles with expansion coefficient of 5.0 are adopted internationally. In the United states Pharmacopeia USPXXI version, the neutral borosilicate medical glass is strictly regulated, and corresponding standards are established for the anti-aging, water resistance, alkali resistance, acid resistance, corrosion resistance and other performances of glass products. The expansion coefficient of the neutral borosilicate medical glass is 46-58 multiplied by 10 -7 V. (20-300 ℃), also known as "5.0 glass". The product has high specification and size precision and can adapt to advanced filling equipment; the product has stable physical and chemical properties, and the shelf life of the contained medicine is relatively long.
CN101208276B discloses the fining of alumino-borosilicate glasses, suitable for alkali-free glasses, manufactured by the downdraw method, without the use of larger amounts of arsenic or antimony for fining.
CN111499185B discloses a composite clarifier, borosilicate glass and a preparation method thereof, wherein the composite clarifier is used for borosilicate glass, the β -OH value of the borosilicate glass is controlled to (0.1-0.3)/mm, the composite clarifier comprises 30-70 wt% of ammonium chloride and 20-70 wt% of sulfate, in addition, a = sulfate/ammonium chloride, and a is 0.43-2.33.
CN105731786B discloses a composite clarifying agent for medicinal neutral glass, which comprises the following components: sodium chloride, sulfate, variable oxide and zinc oxide, wherein the variable oxide is cerium oxide and/or tin oxide, and the mass ratio of the sodium chloride to the sulfate to the variable oxide to the zinc oxide is (0.15-0.5): 0.1 to 3.0:0.1 to 0.5:1 to 3.
The chemical composition of the neutral glass is as follows: siO 2 2 75% of B 2 O 3 8 to 12% of R 2 O is 4 to 8 percent, RO<5％，Al 2 O 3 2-7%, the neutral medicinal glass has high viscosity and high melting temperature during melting, and the glass has high requirement on the dimensional tolerance of the glass tube during moldingThe requirements on the bubble content of the glass, the chemical uniformity and the temperature uniformity of the glass melt are higher than those of the common glass.
Disclosure of Invention
Therefore, the invention provides a method for improving the melting and clarifying quality of neutral medicinal glass, and solves the problems of high melting difficulty, poor clarifying effect, poor quality of glass products, low yield and the like in the production process of glass.
The technical scheme of the invention is realized as follows:
a method for improving the melting and clarifying quality of neutral medicinal glass is characterized in that a composite clarifying agent is added in the process of preparing the neutral medicinal glass, and the composite clarifying agent comprises the following components: basic zinc carbonate, sodium chloride, sodium nitrate and cerium dioxide.
The compound clarifier is prepared from basic zinc carbonate, sodium chloride, sodium nitrate and cerium dioxide, the basic zinc carbonate can be decomposed at 220 ℃, the decomposition products are water and zinc carbonate, the water can help supplement the surface dehydration phenomenon of the batch after entering a melting furnace, the batch is fully wetted, and the zinc carbonate can be decomposed at about 260 ℃ to produce zinc oxide and carbon dioxide. The carbon dioxide is beneficial to the uniform mixing of the mixture, and the layering phenomenon generated in the conveying process of the mixture is eliminated. Zinc oxide as basic component of neutral medicinal glass and containing zinc oxide tetrahedron [ ZnO ] 4 ]The sodium nitrate is melted at the melting point of 306.8 ℃, so that the batch can be quickly wetted to help melting. The decomposition temperature of the sodium nitrate is low (400 ℃ is started), and oxygen released by the decomposition of the sodium nitrate in the early melting stage ensures the oxidizability of the batch, reduces the decomposition of the cerium dioxide in the early melting stage, and thereby ensures the oxygen amount required by the clarification section. Sodium chloride vaporizes at 1442 ℃, reducing the partial pressure of carbon dioxide and oxygen in the bubbles, promoting the growth and overflow of the bubbles, and clarifying the glass.
Cl introduced by the composite clarifying agent - Can be cleaved from silicon-oxygen tetrahedron [ SiO ] 4 ]The formed glass structure network obviously reduces the viscosity of glass liquidAnd the bubbles in the glass liquid are easy to overcome the surface tension of the glass liquid and escape from the glass liquid, so that the clarification of the glass is realized. The cerium dioxide is used as a strong oxidant, and is heated at high temperature to release oxygen, and simultaneously, the surface tension of the molten glass is reduced at high temperature, so that the discharge of bubbles is facilitated. The purposes of improving the clarification of the neutral medicinal glass and reducing the number of bubbles are achieved through the composite clarifying agent.
Further, the mass ratio of the basic zinc carbonate, the sodium chloride, the sodium nitrate and the cerium dioxide is (0.1-0.3): 0.1 to 0.3: 0.2-0.4.
Furthermore, the addition amount of the composite clarifying agent is 0.7-1.1% of the mass of one batch of the batch.
Further, in the process of melting the neutral medicinal glass, the mass of FeO and total iron in the neutral medicinal glass is controlled to be 0.19-0.22: 1.
further, the neutral medical glass is neutral borosilicate medical glass.
Further, the expansion coefficient of the neutral medicinal glass at 20-300 ℃ is (46-58) multiplied by 10 -7 /℃。
Further, the mass ratio of the basic zinc carbonate, the sodium chloride, the sodium nitrate and the cerium dioxide is 0.3.
Furthermore, the ratio of FeO to total iron can be controlled by adjusting the carbon powder content of the mixture and controlling the atmosphere of the glass melting furnace.
Compared with the prior art, the invention has the beneficial effects that:
(1) The composite clarifier consists of four components of basic zinc carbonate, sodium nitrate, sodium chloride and cerium dioxide, and according to the characteristics of a neutral medicinal glass melting furnace, the components of the composite clarifier have different physical and chemical reactions at different temperatures to release gas, so that bubbles in glass are changed from small to large, and the clarification effect is further exerted in the glass melting process. The composite clarifying agent disclosed by the invention not only improves the glass bubble discharging speed and the bubble discharging efficiency, but also reduces the total using amount of the clarifying agent, reduces the production cost and improves the production efficiency through reasonable proportioning.
(2) The compound clarifying agent used in the invention can obviously reduce the viscosity of the neutral medicinal glass liquid and is beneficial to discharging bubbles in the glass liquid; the composite clarifying agent used in the invention has a wide clarifying temperature range, has good adaptability with the clarification of neutral medicinal glass, and effectively improves the melting and clarifying quality of the neutral medicinal glass.
(3) According to the invention, after the components in the composite clarifying agent are uniformly mixed, the composite clarifying agent is firstly premixed with silica sand, so that the uniformity of glass liquid can be improved, the glass forming is facilitated, the advanced melting of a silicon refractory compound can be facilitated, the generation of inclusions in the glass liquid is reduced, and the melting and clarifying quality of neutral medicinal glass is improved.
(4) The clarifying agent provided by the invention does not contain oxides such as arsenic, antimony and the like, can reduce the content of harmful heavy metals in neutral borosilicate glass, and is beneficial to drug safety.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
The neutral glass of the invention comprises the chemical components of SiO in percentage by weight 2 (silica) 74.5-75.5%, B 2 O 3 (boron oxide) 8-12%, R 2 O is 4 to 8 percent, RO is<5％，Al 2 O 3 (alumina) 2-7%. The R is 2 O is an alkali metal oxide and RO is an alkaline earth metal oxide.
The experimental process comprises the following steps: weighing raw materials, uniformly mixing, melting by using a platinum crucible, simulating a temperature system in the production process, putting the mixture into a high-temperature furnace at 1350 ℃, preserving heat for half an hour, heating to 1620 ℃, preserving heat for 3 hours, controlling the ratio of FeO to total iron, taking out the glass melt, casting and molding, putting the glass melt into an annealing furnace at 600 ℃ for annealing to prepare a glass sample, and observing the bubble clarification condition of the glass.
Example 1
The neutral glass is prepared from SiO by mass percent 2 75.5% of Al 2 O 3 5.5% of R 2 O6%, RO 4%, B 2 O 3 The content was 9%.
0.3% of basic zinc carbonate, 0.2% of sodium chloride, 0.2% of sodium nitrate and 0.2% of cerium dioxide are added according to the mass of the neutral glass raw material.
Example 2
The neutral glass is made from SiO by mass percent 2 74.5% of Al 2 O 3 5.5% of R 2 O5%, RO 4%, B 2 O 3 The content was 11%.
0.3% of basic zinc carbonate, 0.2% of sodium chloride, 0.2% of sodium nitrate and 0.2% of cerium dioxide are added according to the mass of the neutral glass raw material.
Comparative example 1
The components in the composite clarifier are adjusted based on example 1, and see table 1 specifically.
Table 1: comparative example 1 composite clarifying agent combination formula
Comparative example 2
The components in the composite clarifier are adjusted based on example 1, and see table 2 specifically.
Table 2: comparative example 1 composite clarifying agent combination formula
Test example 1
The total iron content and FeO content in the glass were measured according to the determination (8) of total iron and the determination method (16) of ferrous oxide in GB1549-2008, and the values are expressed in wt.%. The melted glass is sampled into a sample with the thickness of 5mm, the melting effect of the glass is observed under a polarizing microscope, the number of air bubbles is counted, and the experimental results of the example 1 and the comparative example 1 are shown in the table 3.
Table 3 experimental results of example 1 and comparative example 1
Table 4 experimental results of example 2 and comparative example 2
As can be seen from the clarification effects of the above examples and comparative examples, the stepped composite clarifier of the invention can be used for controlling the ratio of ferrous iron to total iron in glass, can well improve the clarification quality of neutral medicinal glass, has the bubble elimination effect and the clarification quality of glass superior to those of a single clarifier and other combined clarifiers, has less dosage of clarifiers, does not contain toxic substances, and avoids the harm to human bodies or the pollution to the atmosphere. The invention has the advantages that the viscosity of the neutral medicinal glass liquid can be obviously reduced, and the discharge of bubbles in the glass liquid is facilitated; the clarifying temperature range is wide, the adaptability with the clarification of the neutral medicinal glass is good, and the melting and clarifying quality of the neutral medicinal glass is effectively improved; the uniformity of the glass liquid can be improved, and the glass forming is facilitated; the generation of inclusions in molten glass is reduced, and the melting and clarifying quality of neutral medicinal glass is improved; does not contain oxides such as arsenic, antimony and the like, can reduce the content of harmful heavy metals in a neutral borosilicate glass container, and is beneficial to medicine safety.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The method for improving the melting and clarifying quality of the neutral medicinal glass is characterized in that a composite clarifying agent is added in the process of preparing the neutral medicinal glass, and the composite clarifying agent comprises the following components: basic zinc carbonate, sodium chloride, sodium nitrate and cerium dioxide.
2. The composite clarifying agent for improving the melting and clarifying quality of the neutral medicinal glass is characterized by comprising the following components: the mass ratio of the basic zinc carbonate to the sodium chloride to the sodium nitrate to the cerium dioxide is 0.1-0.3.
3. The method for improving the melting and refining quality of the neutral medicinal glass according to claim 1, wherein the adding amount of the composite refining agent is 0.7-1.1% of the mass of one batch.
4. The method for improving the melting and refining quality of the neutral medicinal glass according to claim 1, wherein the mass ratio of FeO to total iron in the neutral medicinal glass is controlled to be 0.19-0.22.
5. The method of improving the molten fining quality of a neutral medicinal glass according to claim 1, wherein the neutral medicinal glass is a neutral borosilicate medicinal glass.
6. The method of claim 6, wherein the neutral medicinal glass has an expansion coefficient of (46-58) x 10 between 20 ℃ and 300 ℃ -7 /℃。
7. The composite fining agent for improving the melting fining quality of a neutral medicinal glass according to claim 2, wherein the weight ratio of basic zinc carbonate, sodium chloride, sodium nitrate and cerium oxide is 0.3.
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| CN202210759761.XA CN115159839B (en) | 2022-06-30 | 2022-06-30 | Method for improving melting and clarifying quality of neutral medicinal glass |
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| CN202210759761.XA CN115159839B (en) | 2022-06-30 | 2022-06-30 | Method for improving melting and clarifying quality of neutral medicinal glass |
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| CN115159839B CN115159839B (en) | 2023-08-18 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116161853A (en) * | 2023-02-14 | 2023-05-26 | 湖南洪康新材料科技有限公司 | Clarification method of medium borosilicate glass, medium borosilicate glass and application thereof |
| CN116199422A (en) * | 2023-03-29 | 2023-06-02 | 海南海控特玻科技有限公司 | Preparation method of neutral medicinal glass tube for improving tube diameter uniformity |
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| DE102009021116A1 (en) * | 2009-05-13 | 2010-11-18 | Schott Ag | Manufacturing borosilicate glass, preferably borosilicate glass of hydrolytic class I, comprises preparing glass batch with addition of refining agent, inserting glass batch, melting glass batch and manufacturing glass articles e.g. pipe |
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| CN107445471A (en) * | 2017-08-08 | 2017-12-08 | 中国洛阳浮法玻璃集团有限责任公司 | A kind of float process leaded light glass sheet compound clarifier |
| CN109133612A (en) * | 2018-10-31 | 2019-01-04 | 浙江大学 | A kind of high alumina silicate glass compound clarifier |
| CN112624607A (en) * | 2021-01-05 | 2021-04-09 | 河北光兴半导体技术有限公司 | Composite clarifying agent, composition for neutral borosilicate medicinal glass, glass prepared from composition and application of glass |
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2022
- 2022-06-30 CN CN202210759761.XA patent/CN115159839B/en active Active
Patent Citations (9)
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| US20090266111A1 (en) * | 2005-11-15 | 2009-10-29 | Nippon Sheet Glass Company, Limited | Method of Producing Glass |
| US20110263410A1 (en) * | 2008-11-10 | 2011-10-27 | Tomoaki Negishi | Method for producing glass, optical glass, glass material for press molding, optical element and methods for producing same |
| DE102009021116A1 (en) * | 2009-05-13 | 2010-11-18 | Schott Ag | Manufacturing borosilicate glass, preferably borosilicate glass of hydrolytic class I, comprises preparing glass batch with addition of refining agent, inserting glass batch, melting glass batch and manufacturing glass articles e.g. pipe |
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| CN112624607A (en) * | 2021-01-05 | 2021-04-09 | 河北光兴半导体技术有限公司 | Composite clarifying agent, composition for neutral borosilicate medicinal glass, glass prepared from composition and application of glass |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116161853A (en) * | 2023-02-14 | 2023-05-26 | 湖南洪康新材料科技有限公司 | Clarification method of medium borosilicate glass, medium borosilicate glass and application thereof |
| CN116199422A (en) * | 2023-03-29 | 2023-06-02 | 海南海控特玻科技有限公司 | Preparation method of neutral medicinal glass tube for improving tube diameter uniformity |
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