CN108503212A - A kind of preparation method of water pearl ash glass - Google Patents
A kind of preparation method of water pearl ash glass Download PDFInfo
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- CN108503212A CN108503212A CN201810496854.1A CN201810496854A CN108503212A CN 108503212 A CN108503212 A CN 108503212A CN 201810496854 A CN201810496854 A CN 201810496854A CN 108503212 A CN108503212 A CN 108503212A
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- water pearl
- ash glass
- pearl ash
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- water
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
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Abstract
A kind of preparation method of water pearl ash glass disclosed by the invention, is specifically implemented according to the following steps：Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, hydrochloric acid and KCl solution is then sequentially added under agitation, obtains mixed liquor；Step 2：Mixed liquor is put into baking oven and carries out 28~30h of constant temperature processing；Step 3：After mixed liquor forms gel, oven temperature is reduced, and carries out constant temperature and handles 50~60h, obtains water pearl ash glass semi-finished product；Step 4：Water pearl ash glass semi-finished product are placed in from taking-up in baking oven in crucible, crucible is placed in the baking oven that temperature is 200~300 DEG C, then oven temperature is risen to 500~600 DEG C, after constant temperature handles 2~3h, baking oven is closed, is taken out after water pearl ash glass semi-finished product are cooled to room temperature in an oven, obtain water pearl ash glass, its purity is high with the uniformity, and preparation method is simple, requires production equipment relatively low.
Description
Technical field
The invention belongs to potash glass preparing technical fields, and in particular to a kind of preparation method of water pearl ash glass.
Background technology
Water pearl ash glass is also known as potash glass, is K2SiO3And SiO2Solid solution.Compared with soda-lime glass, the heat of potash glass is swollen
Swollen coefficient is smaller, it is more difficult to melt, it is more difficult to be corroded by chemicals, can be used for making special chemical apparatuses etc..
For a long time, the preparation of glass and optical fiber glass uses traditional melting-cooling method mostly.Using this method
It is expensive to prepare the required production equipment of glass, and the potash glass purity of preparation and the uniformity are relatively low, are unable to reach requirement.It removes
Except this, special construction and dystectic glass material can not be prepared using melting-cooling method, is greatly limited.
Invention content
The object of the present invention is to provide a kind of preparation methods of water pearl ash glass, solve the potash glass of prior art preparation
Purity and the problem that the uniformity is low and production equipment is of high cost.
The technical solution adopted in the present invention is a kind of preparation method of water pearl ash glass, specifically real according to the following steps
It applies：
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, then under agitation
Hydrochloric acid and KCl solution are sequentially added, mixed liquor is obtained；
Step 2：The mixed liquor that step 1 obtains is put into baking oven and carries out 28~30h of constant temperature processing；
Step 3：Through step 2 processing mixed liquor formed gel after, reduce oven temperature, and carry out constant temperature processing 50~
60h obtains water pearl ash glass semi-finished product；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in
In the baking oven that temperature is 200~300 DEG C, oven temperature is then risen to 500~600 DEG C, after constant temperature handles 2~3h, closes and dries
Case takes out after water pearl ash glass semi-finished product are cooled to room temperature in an oven to get to water pearl ash glass.
The features of the present invention also characterized in that
In step 1, the volume ratio of ethyl orthosilicate, water and ethyl alcohol is 1：6~8：4~5.
In step 1, a concentration of 0.1~0.5mmol/l of hydrochloric acid, a concentration of 0.1~0.5mmol/l of KCl solution.
In step 1, the volume ratio of hydrochloric acid and ethyl orthosilicate is 1：1~2, the KCl solution and ethyl orthosilicate
Volume ratio is 1：100~120.
In step 2, the temperature of baking oven is 60~80 DEG C.
In step 3, oven temperature is 40~50 DEG C.
In step 4, the heating rate of baking oven is 10 DEG C/min.
The invention has the advantages that a kind of preparation method of water pearl ash glass of the present invention, in water and alcohol mixeding liquid
By ethyl orthosilicate, hydrochloric acid, KCl solution by sol-gel method chemically react and generates KSiO by calcining4Glass,
The glass material that high-melting-point and special construction can also be prepared with this method, obtained water pearl ash glass have purity high, uniform
High feature is spent, and preparation method is simple, relatively low to production equipment requirement, cost is relatively low.
Description of the drawings
Fig. 1 is the general figure of infrared light of water pearl ash glass prepared by the method for the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of water pearl ash glass prepared by the method for the present invention.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of water pearl ash glass of the present invention, is specifically implemented according to the following steps：
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, wherein ethyl orthosilicate, water
Volume ratio with ethyl alcohol is 1：6~8：4~5, the salt of a concentration of 0.1~0.5mmol/l is then sequentially added under agitation
The KCl solution of sour and a concentration of 0.1~0.5mmol/l, obtains mixed liquor, mixed liquor in hydrochloric acid and ethyl orthosilicate body
Product is than being 1：The volume ratio of 1~2, KCl solution and ethyl orthosilicate is 1：100~120；
Step 2：By the mixed liquor that step 1 obtains be put into temperature be carried out in 60~80 DEG C of baking oven constant temperature processing 28~
30h；
Step 3：After the mixed liquor of step 2 processing forms gel, oven temperature is reduced to 40~50 DEG C, and carry out constant temperature
50~60h is handled, water pearl ash glass semi-finished product are obtained；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in
In the baking oven that temperature is 200~300 DEG C, oven temperature is then risen to 500~600 DEG C, at constant temperature with the speed of 10 DEG C/min
After managing 2~3h, baking oven is closed, is taken out to get to potassium silicate glass after water pearl ash glass semi-finished product are cooled to room temperature in an oven
Glass.
Embodiment 1
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, wherein ethyl orthosilicate, water
Volume ratio with ethyl alcohol is 1：6：5, the hydrochloric acid of a concentration of 0.1mmol/l and a concentration of is then sequentially added under agitation
The KCl solution of 0.1mmol/l, obtains mixed liquor, mixed liquor in the volume ratio of hydrochloric acid and ethyl orthosilicate be 1：1, KCl is molten
The volume ratio of liquid and ethyl orthosilicate is 1：100；
Step 2：The mixed liquor that step 1 obtains is put into the baking oven that temperature is 80 DEG C and carries out constant temperature processing 28h；
Step 3：After the mixed liquor of step 2 processing forms gel, oven temperature is reduced to 40 DEG C, and carry out constant temperature processing
60h obtains water pearl ash glass semi-finished product；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in
In the baking oven that temperature is 300 DEG C, oven temperature is then risen to 600 DEG C, after constant temperature handles 2h with the speed of 10 DEG C/min, is closed
Baking oven takes out after water pearl ash glass semi-finished product are cooled to room temperature in an oven to get to water pearl ash glass.
Embodiment 2
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, wherein ethyl orthosilicate, water
Volume ratio with ethyl alcohol is 1：8：4, the hydrochloric acid of a concentration of 0.5mmol/l and a concentration of is then sequentially added under agitation
The KCl solution of 0.5mmol/l, obtains mixed liquor, mixed liquor in the volume ratio of hydrochloric acid and ethyl orthosilicate be 1：2, KCl is molten
The volume ratio of liquid and ethyl orthosilicate is 1：120；
Step 2：The mixed liquor that step 1 obtains is put into the baking oven that temperature is 70 DEG C and carries out constant temperature processing 29h；
Step 3：After the mixed liquor of step 2 processing forms gel, oven temperature is reduced to 50 DEG C, and carry out constant temperature processing
50h obtains water pearl ash glass semi-finished product；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in
In the baking oven that temperature is 200 DEG C, oven temperature is then risen to 550 DEG C, after constant temperature handles 2.5h with the speed of 10 DEG C/min, is closed
Baking oven is closed, is taken out to get to water pearl ash glass after water pearl ash glass semi-finished product are cooled to room temperature in an oven.
Embodiment 3
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, wherein ethyl orthosilicate, water
Volume ratio with ethyl alcohol is 1：7：4.5, the hydrochloric acid of a concentration of 0.3mmol/l and a concentration of is then sequentially added under agitation
The KCl solution of 0.3mmol/l, obtains mixed liquor, mixed liquor in the volume ratio of hydrochloric acid and ethyl orthosilicate be 1：1.5, KCl
The volume ratio of solution and ethyl orthosilicate is 1：115；
Step 2：The mixed liquor that step 1 obtains is put into the baking oven that temperature is 60 DEG C and carries out constant temperature processing 30h；
Step 3：After the mixed liquor of step 2 processing forms gel, oven temperature is reduced to 45 DEG C, and carry out constant temperature processing
55h obtains water pearl ash glass semi-finished product；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in
In the baking oven that temperature is 250 DEG C, oven temperature is then risen to 500 DEG C, after constant temperature handles 3h with the speed of 10 DEG C/min, is closed
Baking oven takes out after water pearl ash glass semi-finished product are cooled to room temperature in an oven to get to water pearl ash glass.
Embodiment 4
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, wherein ethyl orthosilicate, water
Volume ratio with ethyl alcohol is 1：6：4, the hydrochloric acid of a concentration of 0.1mmol/l and a concentration of is then sequentially added under agitation
The KCl solution of 0.1mmol/l, obtains mixed liquor, mixed liquor in the volume ratio of hydrochloric acid and ethyl orthosilicate be 1：1, KCl is molten
The volume ratio of liquid and ethyl orthosilicate is 1：100；
Step 2：The mixed liquor that step 1 obtains is put into the baking oven that temperature is 60 DEG C and carries out constant temperature processing 29h；
Step 3：After the mixed liquor of step 2 processing forms gel, oven temperature is reduced to 50 DEG C, and carry out constant temperature processing
50h obtains water pearl ash glass semi-finished product；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in
In the baking oven that temperature is 200 DEG C, oven temperature is then risen to 600 DEG C, after constant temperature handles 2h with the speed of 10 DEG C/min, is closed
Baking oven takes out after water pearl ash glass semi-finished product are cooled to room temperature in an oven to get to water pearl ash glass.
Embodiment 5
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, wherein ethyl orthosilicate, water
Volume ratio with ethyl alcohol is 1：8：5, the hydrochloric acid of a concentration of 0.5mmol/l and a concentration of is then sequentially added under agitation
The KCl solution of 0.5mmol/l, obtains mixed liquor, mixed liquor in the volume ratio of hydrochloric acid and ethyl orthosilicate be 1：2, KCl is molten
The volume ratio of liquid and ethyl orthosilicate is 1：120；
Step 2：The mixed liquor that step 1 obtains is put into the baking oven that temperature is 80 DEG C and carries out constant temperature processing 30h；
Step 3：After the mixed liquor of step 2 processing forms gel, oven temperature is reduced to 40 DEG C, and carry out constant temperature processing
60h obtains water pearl ash glass semi-finished product；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in
In the baking oven that temperature is 300 DEG C, oven temperature is then risen to 500 DEG C, after constant temperature handles 3h with the speed of 10 DEG C/min, is closed
Baking oven takes out after water pearl ash glass semi-finished product are cooled to room temperature in an oven to get to water pearl ash glass.
A kind of principle of the preparation method of water pearl ash glass of the present invention is as follows：
Ethyl orthosilicate is dissolved in water first, and the addition of ethyl alcohol can improve the solubility of ethyl orthosilicate, positive silicic acid second
Ester Si (OC2H5)4It is initial compounds, quartzy silica glass is prepared by sol gel reaction, total reaction is divided into two steps：
The first step, tetraethyl orthosilicate Si (OC2H5)4Silicic acid Si (OH) is generated by hydrolysis4, specific hydrolysis
For：Si(OC2H5)4+4H2O=Si (OH)4+4C2H5OH；
Second step, silicic acid Si (OH)4The three-dimensional net structure to form silica glass is reacted by condensation polymerization, it is specific to polymerize
Reaction is：
Hydrochloric acid is catalyst, and the addition of KCl solution will produce Si-O-K keys under high-temperature calcination, to form potash glass,
Si-O-K keys can be detected in infrared spectrum.
Fig. 1 is the infrared spectrogram of water pearl ash glass, as can be seen from Figure：Positioned at 1050cm-1Spectral peak be due to non-right
Claim, with caused by symmetrical Si-O-Si key chatterings, to vibrate and reinforce with the addition of KCl solution；Positioned at 450cm-1Spectral peak be and O-Si-
O key chatterings are related, and with the addition of KCl solution, its oscillation intensity slightly weakens；Positioned at 790cm-1Spectral peak be that Si-O-K stretches
Caused by contracting vibration, vibrates and reinforce with the addition of KCl solution；In 3000~3800cm-1Region has the OH corresponding to water is flexible to shake
Dynamic spectral peak illustrates that the main component of product is KSiO4。
Fig. 2 is the scanning electron microscope (SEM) photograph of water pearl ash glass, it is seen that using prepared by preparation method of the present invention
Water pearl ash glass surface is smooth, and continuously, flatness is good.
A kind of preparation method of water pearl ash glass of the present invention, by ethyl orthosilicate, hydrochloric acid in water and alcohol mixeding liquid,
KCl solution by sol-gel method chemically react and generates KSiO by calcining4Glass can also be prepared with this method
The glass material of high-melting-point and special construction, obtained water pearl ash glass have the characteristics that purity is high, the uniformity is high, and to production
Equipment requirement is relatively low, and cost is relatively low.
Claims (7)
1. a kind of preparation method of water pearl ash glass, which is characterized in that be specifically implemented according to the following steps：
Step 1：Ethyl orthosilicate, water and ethyl alcohol are placed in container and are mixed into homogeneous phase solution, then under agitation successively
Hydrochloric acid and KCl solution is added, obtains mixed liquor；
Step 2：The mixed liquor that step 1 obtains is put into baking oven and carries out 28~30h of constant temperature processing；
Step 3：After the mixed liquor of step 2 processing forms gel, oven temperature is reduced, and carries out constant temperature and handles 50~60h, is obtained
To water pearl ash glass semi-finished product；
Step 4：The water pearl ash glass semi-finished product that step 3 obtains are placed in from taking-up in baking oven in crucible, crucible is placed in temperature
In 200~300 DEG C of baking oven, oven temperature then to be risen to 500~600 DEG C, after constant temperature handles 2~3h, baking oven is closed, waits for
Water pearl ash glass semi-finished product take out after being cooled to room temperature in an oven to get to water pearl ash glass.
2. a kind of preparation method of water pearl ash glass according to claim 1, which is characterized in that in step 1, it is described just
The volume ratio of silester, water and ethyl alcohol is 1：6~8：4~5.
3. a kind of preparation method of water pearl ash glass according to claim 2, which is characterized in that in step 1, the salt
A concentration of 0.1~the 0.5mmol/l, a concentration of 0.1~0.5mmol/l of KCl solution of acid.
4. a kind of preparation method of water pearl ash glass according to claim 3, which is characterized in that in step 1, the salt
The volume ratio of acid and ethyl orthosilicate is 1：1~2, the volume ratio of the KCl solution and ethyl orthosilicate is 1：100~120.
5. a kind of preparation method of water pearl ash glass according to claim 1, which is characterized in that in step 2, the baking
The temperature of case is 60~80 DEG C.
6. a kind of preparation method of water pearl ash glass according to claim 1, which is characterized in that in step 3, the baking
Box temperature degree is 40~50 DEG C.
7. a kind of preparation method of water pearl ash glass according to claim 1, which is characterized in that in step 4, the baking
The heating rate of case is 10 DEG C/min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810496854.1A CN108503212B (en) | 2018-05-22 | 2018-05-22 | Preparation method of potassium silicate glass |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810496854.1A CN108503212B (en) | 2018-05-22 | 2018-05-22 | Preparation method of potassium silicate glass |
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| CN108503212B CN108503212B (en) | 2021-05-04 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4751202A (en) * | 1985-06-21 | 1988-06-14 | Glaverbel | Manufacturing vitreous beads |
| CN101921061A (en) * | 2010-08-06 | 2010-12-22 | 中国科学院化学研究所 | Method for preparing phosphosilicate based glass |
| US20130210603A1 (en) * | 2011-01-18 | 2013-08-15 | Samsung Electro-Mechanics Co., Ltd. | Glass powder and method of manufacturing the same |
| CN105330134A (en) * | 2015-12-04 | 2016-02-17 | 太仓市建兴石英玻璃厂 | Preparing method for fluorine-high-doped silica glass |
| CN107739153A (en) * | 2017-11-06 | 2018-02-27 | 南昌大学 | A kind of clear glass and preparation method with highly effective green light transmitting |
-
2018
- 2018-05-22 CN CN201810496854.1A patent/CN108503212B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4751202A (en) * | 1985-06-21 | 1988-06-14 | Glaverbel | Manufacturing vitreous beads |
| CN101921061A (en) * | 2010-08-06 | 2010-12-22 | 中国科学院化学研究所 | Method for preparing phosphosilicate based glass |
| US20130210603A1 (en) * | 2011-01-18 | 2013-08-15 | Samsung Electro-Mechanics Co., Ltd. | Glass powder and method of manufacturing the same |
| CN105330134A (en) * | 2015-12-04 | 2016-02-17 | 太仓市建兴石英玻璃厂 | Preparing method for fluorine-high-doped silica glass |
| CN107739153A (en) * | 2017-11-06 | 2018-02-27 | 南昌大学 | A kind of clear glass and preparation method with highly effective green light transmitting |
Non-Patent Citations (2)
| Title |
|---|
| D.M.KROL等: "Raman study of the structure of sodium aluminosilicate gels", 《JOURNAL OF NON-CRYSTALLINE SOLIDS》 * |
| M. SITARZ等: "Rings in the structure of silicate glasses", 《JOURNAL OF MOLECULAR STRUCTURE》 * |
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