CN109942207A - A kind of preparation method of hydrophilic glass product - Google Patents
A kind of preparation method of hydrophilic glass product Download PDFInfo
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- CN109942207A CN109942207A CN201910301426.3A CN201910301426A CN109942207A CN 109942207 A CN109942207 A CN 109942207A CN 201910301426 A CN201910301426 A CN 201910301426A CN 109942207 A CN109942207 A CN 109942207A
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Abstract
The present invention provides a kind of preparation method of hydrophilic glass product, it is the following steps are included: glass is immersed in the mixed liquor of tributyl tin organic acid esters, silica, acetic anhydride and butanol, pulling film forming, pull rate is 1-10mm/s, after drying, 2-3h is roasted at 520-600 DEG C, it is cooling, obtain counterdie;Glassware is placed in tempering case, is heated to 650-710 DEG C, while being passed through N simultaneously from all directions2And hydrophilic agent, after 20-30 minutes, stop ventilation, after glassware is cooled to room temperature rapidly, tempering terminates, and glassware is taken out from tempering case, obtains hydrophilic glass product.The present invention is using tributyl tin organic acid esters and silica as mixed liquor, and through pulling film forming, dry roasting, tributyl tin organic acid esters is pyrolyzed to obtain stannum oxide nano-crystal body film, then by being passed through N2Secondary film is coated with the mode of hydrophilic agent, improves the hydrophily of glass.
Description
Technical field
The present invention relates to glass technology fields, specifically disclose a kind of preparation method of hydrophilic glass product.
Background technique
The wetability of material surface is always the hot spot of academic and industrial circle concern, super hydrophilic and super-hydrophobic as two kinds of poles
Special wetting phenomena is held, has attracted the extensive research of domestic and foreign scholars in recent years.In general, super hydrophobic surface refers to solid-liquid
Contact angle is greater than 150 ° of surface.On the contrary, ultra-hydrophilic surface refers to that liquid can be spread completely, and cause contact angle be equal to or
Close to 0 ° of surface.Compared with super-hydrophobic research, super hydrophilic aspect research it is less, but due to the unique wetting of ultra-hydrophilic surface
Feature, so that ultra-hydrophilic surface has many advantages, such as automatically cleaning, high heat transfer.Earliest it is found out that super hydrophilic characteristic is based on two
The photocatalysis characteristic of titanium oxide, after by ultraviolet light, water and titanium dioxide semiconductor film contacts, contact angle be reduced rapidly to
0±1°.Its principle is that the bridge location oxygen of titanium dioxide surface generates active oxygen radical after by ultraviolet excitation, and life is reacted with hole
At oxygroup hole, water, which is adsorbed in oxygroup hole, becomes chemical absorbed water, to form equally distributed nanoscale on surface
Hydrophilic microcell.This super hydrophilic property has important application in terms of antifog glass, self-cleaning glass.However, titanium dioxide is thin
Film for the significant drawback of self-cleaning glass is restricted by illumination condition, that is, must have under conditions of light irradiates could send out
Wave super hydrophilic characteristic.In view of the above problems, special to propose this invention.
Summary of the invention
It is an object of the invention to overcome existing defect, a kind of preparation method of hydrophilic glass product is provided, the present invention
The hydrophilic glass product sample of acquisition has water-wet behavior, and has good translucency.
In order to achieve the goal above, the present invention is by including what following technical scheme was realized: a kind of hydrophilic glass product
Preparation method, comprising the following steps:
1) it is sent into microwave processing equipment by glass raw material and carries out interval microwave treatment;
Preferably, in step 1), the glass raw material includes following raw material and parts by weight: nano silica 70-
80 parts, 20-30 parts of carbon nanotube dust, 10-18 parts of borax, 5-12 parts of zirconium oxide, 6-15 parts of potassium carbonate, 0.5-2 parts of lithium carbonate,
5-12 parts of niobium pentaoxide, 8-16 parts of antimony oxide, 4-12 parts of boron oxide, 2-7 parts of titanium dioxide.
Preferably, in step 1), it is spaced the condition of microwave treatment are as follows: microwave frequency 1800-2000MHz, power are
250-300W, interval time are 2-5 minutes, each microwave treatment 20-25 minutes, are carried out continuously 20-30 times.
2) raw material after microwave treatment is melted in pot furnace, obtains glass metal;
Preferably, in step 2), melting temperature is 1425~1500 DEG C, and the melting time is 5~8 hours.
3) glass metal melted is cooled to 850~910 DEG C, is subsequently placed in molding machine and forms, then Temperature fall
To 420-510 DEG C;
4) product after molding is sent into annealing kiln and is annealed, kept the temperature, naturally cool to room temperature;
Preferably, in step 4), annealing temperature is 480~500 DEG C, keeps the temperature 4~6 hours.
5) it coats counterdie: glass being immersed in the mixed liquor of tributyl tin organic acid esters, silica, acetic anhydride and butanol,
Pulling film forming, pull rate 1-10mm/s roast 2-3h after dry at 520-600 DEG C, cooling, obtain counterdie;
Preferably, in step 5), tributyl tin organic acid esters, silica, acetic anhydride and butanol weight proportion be (2-
20):(10-20):(5-17):(27-40)。
6) secondary film, tempering are coated: glassware is placed in tempering case, is heated to 650-710 DEG C, while from each side
To being passed through N simultaneously2And hydrophilic agent, after 20-30 minutes, stop ventilation, after glassware is cooled to room temperature rapidly, tempering knot
Glassware is taken out from tempering case, obtains hydrophilic glass product by beam.
Preferably, in step 6), while N is passed through2With the specific steps of hydrophilic agent are as follows: by N2It is first passed through in hydrophilic agent bottle,
Then hydrophilic agent is carried and is realized in tempering case while is passed through N2And hydrophilic agent;
Preferably, in step 6), the hydrophilic agent is by butyl acetate and ethyl alcohol according to the group of weight ratio 1:(15-20)
At.
In conclusion the present invention provides a kind of preparation method of hydrophilic glass product, beneficial effects of the present invention:
The present invention is using tributyl tin organic acid esters and silica as mixed liquor, through pulling film forming, dry roasting, and three
Butyl tin organic acid esters is pyrolyzed to obtain stannum oxide nano-crystal body film, then by being passed through N2It is coated with the mode of hydrophilic agent secondary
Film further increases the hydrophily of glass, and glassware is made equally to have water-wet behavior, while glass system under non-illumination condition
Product have good mechanical strength.
The present invention obtains the surface of hydrophilic glass product, and steam is uniformly distributed according to the position of nano tin dioxide, hydrophilic glass
Product has good visible light transmittance, and light transmittance may be up to 93%;Also there is good infrared absorption, corrosion-resistant, resistance toization
Learn performance;The manufacture craft of this hydrophilic glass product is simple, can scale processing, have in future feature type glass art wide
Wealthy application prospect.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.It should be understood that embodiment is merely to illustrate the present invention, rather than limit
The scope of the present invention.
Embodiment 1
A kind of preparation method of hydrophilic glass product, comprising the following steps:
1) it is mixed by glass raw material according to following weight proportion: 70 parts of nano silica, carbon nanotube dust 30
Part, 11 parts of borax, 12 parts of zirconium oxide, 6 parts of potassium carbonate, 0.5 part of lithium carbonate, 12 parts of niobium pentaoxide, 8 parts of antimony oxide, oxygen
5 parts of boron oxide, 7 parts of titanium dioxide.
Mixed glass raw material is sent into microwave processing equipment and carries out interval microwave treatment;It is spaced the item of microwave treatment
Part are as follows: microwave frequency 1800MHz, power 250W, interval time are 5 minutes, and each microwave treatment 20 minutes is carried out continuously
30 times.
2) raw material after microwave treatment being melted in pot furnace, melting temperature is 1500 DEG C, and the melting time is 6 hours,
Obtain glass metal;
3) glass metal melted is cooled to 900 DEG C, is subsequently placed in molding machine and forms, be then naturally cooling to 420
℃;
4) product after molding is sent into annealing kiln and is annealed, annealing temperature is 480 DEG C, keeps the temperature 5 hours, naturally cools to
Room temperature.
5) counterdie is coated: by tributyl tin organic acid esters, silica, acetic anhydride and butanol 5:10:10 according to the weight ratio:
32 mixing, are configured to mixed liquor, then immerse glass in mixed liquor, pulling film forming, pull rate 5mm/s, after dry,
2.5h is roasted at 550 DEG C, it is cooling, obtain counterdie;
6) coat secondary film, tempering: butyl acetate and ethyl alcohol are configured to hydrophilic agent according to weight ratio 1:17, by glassware
It is placed in tempering case, is heated to 700 DEG C, by N2It is first passed through in hydrophilic agent bottle, then N2Hydrophilic agent is carried into tempering case from each
It realizes while being passed through N in direction2And hydrophilic agent stops ventilation, after glassware is cooled to room temperature rapidly, tempering after twenty minutes
Terminate, glassware is taken out from tempering case, obtains hydrophilic glass product.The contact angle of water droplet on the hydrophilic glass product
It is 5.5 °, light transmittance 90%.
Embodiment 2
A kind of preparation method of hydrophilic glass product, comprising the following steps:
1) it is mixed by glass raw material according to following weight proportion: 75 parts of nano silica, carbon nanotube dust 25
Part, 14 parts of borax, 5 parts of zirconium oxide, 8 parts of potassium carbonate, 0.9 part of lithium carbonate, 8 parts of niobium pentaoxide, 10 parts of antimony oxide, oxidation
7 parts of boron, 5 parts of titanium dioxide.
Mixed glass raw material is sent into microwave processing equipment and carries out interval microwave treatment;It is spaced the item of microwave treatment
Part are as follows: microwave frequency 1900MHz, power 270W, interval time are 4 minutes, and each microwave treatment 20 minutes is carried out continuously
25 times.
2) raw material after microwave treatment being melted in pot furnace, melting temperature is 1460 DEG C, and the melting time is 7 hours,
Obtain glass metal;
3) glass metal melted is cooled to 900 DEG C, is subsequently placed in molding machine and forms, be then naturally cooling to 450
℃;
4) product after molding is sent into annealing kiln and is annealed, annealing temperature is 490 DEG C, keeps the temperature 5 hours, naturally cools to
Room temperature.
5) counterdie is coated: by tributyl tin organic acid esters, silica, acetic anhydride and butanol 5:10:10 according to the weight ratio:
32 mixing, are configured to mixed liquor, then immerse glass in mixed liquor, pulling film forming, pull rate 2mm/s, after dry,
2.5h is roasted at 550 DEG C, it is cooling, obtain counterdie;
6) coat secondary film, tempering: butyl acetate and ethyl alcohol are configured to hydrophilic agent according to weight ratio 1:17, by glassware
It is placed in tempering case, is heated to 700 DEG C, by N2It is first passed through in hydrophilic agent bottle, then N2Hydrophilic agent is carried into tempering case from each
It realizes while being passed through N in direction2And hydrophilic agent stops ventilation, after glassware is cooled to room temperature rapidly, tempering after twenty minutes
Terminate, glassware is taken out from tempering case, obtains hydrophilic glass product.The contact angle of water droplet on the hydrophilic glass product
It is 6.9 °, light transmittance 91%.
Embodiment 3
A kind of preparation method of hydrophilic glass product, comprising the following steps:
1) it is mixed by glass raw material according to following weight proportion: 78 parts of nano silica, carbon nanotube dust 27
Part, 15 parts of borax, 7 parts of zirconium oxide, 11 parts of potassium carbonate, 1.5 parts of lithium carbonate, 5 parts of niobium pentaoxide, 14 parts of antimony oxide, oxygen
Change 9 parts of boron, 4 parts of titanium dioxide.
Mixed glass raw material is sent into microwave processing equipment and carries out interval microwave treatment;It is spaced the item of microwave treatment
Part are as follows: microwave frequency 2000MHz, power 300W, interval time are 5 minutes, and each microwave treatment 25 minutes is carried out continuously
20 times.
2) raw material after microwave treatment being melted in pot furnace, melting temperature is 1500 DEG C, and the melting time is 5 hours,
Obtain glass metal;
3) glass metal melted is cooled to 910 DEG C, is subsequently placed in molding machine and forms, be then naturally cooling to 470
℃;
4) product after molding is sent into annealing kiln and is annealed, annealing temperature is 490 DEG C, keeps the temperature 5 hours, naturally cools to
Room temperature.
5) counterdie is coated: by tributyl tin organic acid esters, silica, acetic anhydride and butanol 5:15:10 according to the weight ratio:
32 mixing, are configured to mixed liquor, then immerse glass in mixed liquor, pulling film forming, pull rate 7mm/s, after dry,
2.5h is roasted at 550 DEG C, it is cooling, obtain counterdie;
6) coat secondary film, tempering: butyl acetate and ethyl alcohol are configured to hydrophilic agent according to weight ratio 1:17, by glassware
It is placed in tempering case, is heated to 700 DEG C, by N2It is first passed through in hydrophilic agent bottle, then N2Hydrophilic agent is carried into tempering case from each
It realizes while being passed through N in direction2And hydrophilic agent stops ventilation, after glassware is cooled to room temperature rapidly, tempering after twenty minutes
Terminate, glassware is taken out from tempering case, obtains hydrophilic glass product.The contact angle of water droplet on the hydrophilic glass product
It is 5.2 °, light transmittance 93%.
Embodiment 4
A kind of preparation method of hydrophilic glass product, comprising the following steps:
1) it is mixed by glass raw material according to following weight proportion: 80 parts of nano silica, carbon nanotube dust 22
Part, 18 parts of borax, 10 parts of zirconium oxide, 15 parts of potassium carbonate, 1.9 parts of lithium carbonate, 10 parts of niobium pentaoxide, 16 parts of antimony oxide,
12 parts of boron oxide, 2 parts of titanium dioxide.
Mixed glass raw material is sent into microwave processing equipment and carries out interval microwave treatment;It is spaced the item of microwave treatment
Part are as follows: microwave frequency 2000MHz, power 300W, interval time are 5 minutes, and each microwave treatment 20 minutes is carried out continuously
20 times.
2) raw material after microwave treatment being melted in pot furnace, melting temperature is 1500 DEG C, and the melting time is 5 hours,
Obtain glass metal;
3) glass metal melted is cooled to 910 DEG C, is subsequently placed in molding machine and forms, be then naturally cooling to 420
℃;
4) product after molding is sent into annealing kiln and is annealed, annealing temperature is 490 DEG C, keeps the temperature 5 hours, naturally cools to
Room temperature.
5) counterdie is coated: by tributyl tin organic acid esters, silica, acetic anhydride and butanol 5:10:10 according to the weight ratio:
32 mixing, are configured to mixed liquor, then immerse glass in mixed liquor, pulling film forming, pull rate 3mm/s, after dry,
2.5h is roasted at 600 DEG C, it is cooling, obtain counterdie;
6) coat secondary film, tempering: butyl acetate and ethyl alcohol are configured to hydrophilic agent according to weight ratio 1:17, by glassware
It is placed in tempering case, is heated to 700 DEG C, by N2It is first passed through in hydrophilic agent bottle, then N2Hydrophilic agent is carried into tempering case from each
It realizes while being passed through N in direction2And hydrophilic agent, after 30 minutes, stop ventilation, after glassware is cooled to room temperature rapidly, tempering
Terminate, glassware is taken out from tempering case, obtains hydrophilic glass product.The contact angle of water droplet on the hydrophilic glass product
It is 7.8 °, light transmittance 89%.
More than, only presently preferred embodiments of the present invention should not to the present invention in any form with substantial limitation
It points out, for those skilled in the art, under the premise of not departing from the method for the present invention, can also make several
It improves and supplement, these improvement and supplement also should be regarded as protection scope of the present invention.All those skilled in the art, not
Be detached from the spirit and scope of the present invention in the case where, when a little change made using disclosed above technology contents,
Modification and the equivalent variations developed, are equivalent embodiment of the invention;Meanwhile all substantial technologicals according to the present invention are to above-mentioned
The variation, modification and evolution of any equivalent variations made by embodiment, in the range of still falling within technical solution of the present invention.
Claims (8)
1. a kind of preparation method of hydrophilic glass product, which comprises the following steps:
1) it after by glass raw material mixing, is sent into microwave processing equipment and carries out interval microwave treatment;
2) raw material after microwave treatment is melted in pot furnace, obtains glass metal;
3) glass metal melted is cooled to 850~910 DEG C, is subsequently placed in molding machine and forms, be then naturally cooling to
420-510℃;
4) product after molding is sent into annealing kiln and is annealed, kept the temperature, naturally cool to room temperature;
5) it coats counterdie: glass being immersed in the mixed liquor of tributyl tin organic acid esters, silica, acetic anhydride and butanol, lifting
Film forming, pull rate 1-10mm/s roast 2-3h after dry at 520-600 DEG C, cooling, obtain counterdie;
6) secondary film, tempering are coated: glassware being placed in tempering case, is heated to 650-710 DEG C, while same from all directions
When be passed through N2And hydrophilic agent, after 20-30 minutes, stop ventilation, after glassware is cooled to room temperature rapidly, tempering terminates, will
Glassware takes out from tempering case, obtains hydrophilic glass product.
2. the preparation method of hydrophilic glass product as described in claim 1, which is characterized in that the glass raw material includes following
Raw material and parts by weight: 70-80 parts of nano silica, 20-30 parts of carbon nanotube dust, 10-18 parts of borax, zirconium oxide 5-12
Part, 6-15 parts of potassium carbonate, 0.5-2 parts of lithium carbonate, 5-12 parts of niobium pentaoxide, 8-16 parts of antimony oxide, 4-12 parts of boron oxide,
2-7 parts of titanium dioxide.
3. the preparation method of hydrophilic glass product as described in claim 1, which is characterized in that in step 1), be spaced microwave
The condition of processing are as follows: microwave frequency 1800-2000MHz, power 250-300W, interval time are 2-5 minutes, each microwave
Processing 20-25 minutes, is carried out continuously 20-30 times.
4. the preparation method of hydrophilic glass product as described in claim 1, which is characterized in that in step 2), melting temperature
It is 1425~1500 DEG C, the melting time is 5~8 hours.
5. the preparation method of hydrophilic glass product as described in claim 1, which is characterized in that in step 4), annealing temperature
It is 480~500 DEG C, keeps the temperature 4~6 hours.
6. the preparation method of hydrophilic glass product as described in claim 1, which is characterized in that in step 5), tributyl tin
Organic acid esters, silica, acetic anhydride and butanol weight proportion be (2-20): (10-20): (5-17): (27-40).
7. the preparation method of hydrophilic glass product as described in claim 1, which is characterized in that in step 6), while being passed through N2
With the specific steps of hydrophilic agent are as follows: by N2It is first passed through in hydrophilic agent bottle, then hydrophilic agent is carried in tempering case and is realized simultaneously
It is passed through N2And hydrophilic agent.
8. the preparation method of hydrophilic glass product as described in claim 1, which is characterized in that described hydrophilic in step 6)
Agent forming according to weight ratio 1:(15-20) by butyl acetate and ethyl alcohol.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111995223A (en) * | 2020-07-22 | 2020-11-27 | 安徽省凤阳县前力玻璃制品有限公司 | Method for manufacturing hydrophilic glass product |
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2019
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Non-Patent Citations (2)
Title |
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中华人民共和国物资管理部制订: "《物资技术保管规程 试行本 第四分册 化工和轻工》", 28 February 1965, 中国工业出版社 * |
崔虹云: "《碳纳米管网络复合结构与纳米膜接触特性的研究》", 31 August 2017, 东北大学出版社 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111995223A (en) * | 2020-07-22 | 2020-11-27 | 安徽省凤阳县前力玻璃制品有限公司 | Method for manufacturing hydrophilic glass product |
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