CN110790511B - Low-temperature environment-friendly black glass paste with high optical density - Google Patents
Low-temperature environment-friendly black glass paste with high optical density Download PDFInfo
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- CN110790511B CN110790511B CN201911097863.4A CN201911097863A CN110790511B CN 110790511 B CN110790511 B CN 110790511B CN 201911097863 A CN201911097863 A CN 201911097863A CN 110790511 B CN110790511 B CN 110790511B
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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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
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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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
-
- 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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
Abstract
The invention discloses a low-temperature environment-friendly black glass paste with high optical density, which comprises the following raw materials in parts by weight: 40-75% of a cullet block, 15-45% of a black pigment and 12-25% of varnish, wherein the cullet block comprises the following raw materials in parts by weight: 17 to 37% SiO2、20～60％Bi2O3、4～20％ZnO、4～19％B2O3、1～12％Na2O、0～5％K2O、1～4％TiO2、0.5～6％ZrO2. The glass slurry prepared by the invention does not contain Pb, Cr and halogen elements, is environment-friendly and meets the environmental protection standard of RoHS of European Union, the raw materials of the raw materials are treated by heat treatment and dry grinding processes, the optical density of the glass slurry is greatly improved, the glaze surface has good glossiness after tempering at 640-680 ℃, and the glass slurry has extremely high blackness and excellent acid and alkali resistance.
Description
Technical Field
The invention relates to low-temperature environment-friendly black glass paste with high optical density, and belongs to the technical field of glass paste.
Background
The glass slurry is a glaze which is printed on the glass through a medium such as a silk screen or a roller and can be firmly bonded on the glass after being toughened. After being bonded on glass, different glass pastes have different performances such as decoration, light shielding, protection and the like due to different performances such as color, glaze texture, covering power and the like, so that the glass paste has very wide application in various aspects such as buildings, household appliances, kitchens and bathrooms, automobiles and the like.
After the glass slurry is toughened, the covering power of the glass slurry is obviously reduced, and the use and development of the toughened glass slurry are seriously influenced sometimes. The hiding power of the glass paste can be expressed by optical density, and the higher the optical density, the better the hiding power of the glass paste. There are many factors that affect the optical density, such as the number and content of air bubbles in the finished slurry, the size and morphology of the solid powder, the wettability between the solid powder and the varnish, the printing process and the mesh number of the screen, etc., wherein the size and morphology of the solid powder have a crucial role in the optical density of the slurry. The powder has too large particle size, improper particle size distribution or irregular powder shape, the particles cannot be effectively densely packed, and the optical density is greatly reduced after toughening; the particle size of the powder is too small, so that the particle surface has very high surface energy, the powder cannot be well wetted with ink mixing oil and the like, and effective close packing cannot be performed, sand holes and gaps in an ink film are caused, obvious light transmission points appear in the ink film, and the optical density of the slurry is also reduced.
In order to improve the covering power of the glass slurry, chinese patent 201811290757.3 introduces "black environmental protection toughened glass slurry with high covering power and its preparation method", wherein it is mentioned that the glass powder is ball milled for the second time, and is mixed with pigment for wet milling to obtain the environmental protection toughened glass slurry with high covering power; chinese patent 201810302045.2 describes "a high-temperature environment-friendly high-covering black slurry and a preparation method thereof", wherein the high-temperature environment-friendly high-covering black slurry is obtained by melting glass powder, quenching with water, wet-grinding, filter-pressing, dewatering, drying to prevent secondary agglomeration. Although the covering power of the glass paste is improved, the use and development of the glass paste are restricted due to the fact that the glass paste is high in temperature and poor in blackness. Therefore, there is a need for a low-temperature environment-friendly black glass paste with high optical density and a preparation method thereof, so as to solve the problem of poor covering power of the glass paste and simultaneously achieve other necessary properties.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the low-temperature environment-friendly black glass slurry with high optical density, which does not contain Pb, Cr and halogen elements, meets the environmental protection standard of RoHS of European Union and is environment-friendly.
In order to achieve the purpose, the invention adopts the following technical scheme: the low-temperature environment-friendly black glass paste with high optical density comprises the following raw materials in parts by weight: 40-75% of broken glass blocks, 15-45% of black pigment and 12-25% of varnish.
Preferably, the cullet pieces comprise the following raw materials in parts by weight: 17 to 37% SiO2、20～60％Bi2O3、4～20％ZnO、4～19％B2O3、1～12％Na2O、0～5％K2O、1～4％TiO2、0.5～6％ZrO2(ii) a The black pigment is copper-chromium black pigment; the varnish is prepared by mixing 15-35 wt% of polymer resin and 40-85 wt% of water-based solvent.
Preferably, the cullet pieces are prepared from the following raw materials in parts by weight: 17.3% SiO2、55％Bi2O3、14.5％ZnO、4.1％B2O3、3.1％Na2O、1.6％K2O、3.9％TiO2、0.5％ZrO2。
Preferably, the polymer resin is one or more of ethyl cellulose, acrylic resin and polyvinyl alcohol resin; the aqueous solvent is one or more of diethylene glycol butyl ether, terpineol, diethylene glycol butyl ether acetate and ethyl oleate.
The invention also provides a preparation method of the low-temperature environment-friendly black glass slurry with high optical density, which comprises the following steps:
s1, preparation of a cullet base material:
s1.1 mixing: weighing SiO according to the weight ratio2、Bi2O3、ZnO、B2O3、Na2O、K2O、TiO2、ZrO2Mixing in a mixer to obtain mixture;
s1.2, melting: placing the mixture obtained in the step S1.1 into a crucible and placing the crucible into a muffle furnace for melting, wherein the melting temperature is 1000-1200 ℃, and the heat preservation time is 40-120 min, so as to obtain glass liquid;
s1.3, ice water quenching: quenching the glass liquid obtained in the step S1.2 by deionized ice water, and drying to obtain a glass cullet block base material;
s2, heat treatment: placing the glass cullet block base material obtained in the step S1.3 in a muffle furnace for heat treatment, performing deionized water quenching after the heat treatment, and repeating for 3-5 times to obtain glass cullet blocks;
s3, preparing solid powder:
dry grinding: respectively weighing the glass cullet blocks and the black pigment obtained in the step S2 according to the proportion, mixing, placing the mixture into a ball mill for medium-free ball milling with a material-ball ratio of 1:5, performing high-speed dry milling treatment, performing low-speed dry milling treatment, and repeating for 3-6 times to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
s4, preparing glass slurry: and (4) weighing the varnish according to the proportion, adding the solid powder obtained in the step S3 into the varnish, fully and uniformly mixing, and then mixing for 4-6 times by using a three-roll grinder to obtain the glass slurry.
Preferably, in the step S2, the heat treatment temperature is 350 to 450 ℃ and the heat treatment time is 25 to 35 min.
Preferably, in the step S3, the high-speed dry milling: the ball milling speed is 230-270 rpm, the ball milling time is 10-30 min, and the low-speed dry milling is carried out: the ball milling speed is 90-120 rpm, and the ball milling time is 110-140 min.
Preferably, the glass slurry obtained in step S4 is tempered, and the tempering method is as follows: and (2) screen-printing the glass slurry on glass by using a 250-mesh screen, wherein the wet film thickness of the glass slurry is 18-22 mu m, and then sintering at 640-680 ℃ to form a slurry layer with the thickness of 13-17 mu m.
Preferably, the optical density of the slurry layer is greater than 5.
The invention has the beneficial effects that:
1. the glass slurry comprises broken glass blocks, black pigment and varnish raw materials, and the raw materials do not contain Pb, Cr and halogen elements, meet the environmental protection standard of RoHS of European Union, and are environment-friendly materials.
2. The raw materials of the glass slurry are treated by heat treatment and dry grinding processes, so that the optical density of the glass slurry is greatly improved, and the covering power of the glass slurry is improved; the broken glass block base material is subjected to repeated heat treatment and water quenching, so that the stress in the broken glass block can be released to the maximum extent, and the initial granularity of the broken glass block is reduced; the black pigment and the heat-treated broken glass blocks are mixed and ground by adopting a high-speed and low-speed mixing dry grinding mode to obtain solid powder, the uniformity is higher, the particle size of the solid powder is obviously reduced, the solid powder achieves proper particle size distribution, the appearance and the appearance are further modified, the sphericity is better, the solid powder can be well wetted with ink mixing oil, and the closest accumulation is effectively achieved.
3. After the glass slurry is subjected to sintering tempering treatment at 640-680 ℃, the glaze surface has good glossiness, no air holes, extremely high blackness and excellent acid and alkali resistance.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
EXAMPLES 1-6 preparation of cullet base
The preparation method of the glass cullet base material comprises the following steps:
s1.1 mixing: SiO was weighed in the weight ratio shown in Table 12、Bi2O3、ZnO、B2O3、Na2O、K2O、TiO2、ZrO2Mixing in a mixer to obtain mixture;
s1.2, melting: placing the mixture obtained in the step S1.1 into a crucible and placing the crucible into a muffle furnace for melting, wherein the melting temperature is 1000-1200 ℃, and the heat preservation time is 40-120 min, so as to obtain glass liquid;
s1.3, ice water quenching: and (3) quenching the glass liquid obtained in the step (S1.2) by deionized ice water, and drying to obtain a glass cullet block base material.
TABLE 1
Examples 7-12 black glass pastes were prepared using cullet base materials prepared in examples 1-6 above
Example 7 the cullet base prepared in example 1 was selected;
example 8 the cullet base prepared in example 2 was selected;
example 9 the cullet base prepared in example 3 was selected;
example 10 the cullet base prepared in example 4 was selected;
example 11 the cullet base prepared in example 5 was selected;
example 12 the cullet base prepared in example 6 was selected.
The preparation method comprises the following steps:
s2, heat treatment: placing the broken glass block base material in a muffle furnace for heat treatment at 350-450 ℃ for 25-35 min, performing deionized water quenching after heat treatment, and repeating for 3-5 times to obtain a broken glass block;
s3, preparing solid powder:
dry grinding: respectively weighing the cullet blocks and the black pigment obtained in the step S2 according to the proportion, mixing, placing in a ball mill for medium-free ball milling with a material-ball ratio of 1:5, and firstly performing high-speed dry milling: the ball milling speed is 230-270 rpm, the ball milling time is 10-30 min, and then the low-speed dry milling is carried out: the ball milling rotation speed is 90-120 rpm, the ball milling time is 110-140 min, and the ball milling is repeated for 3-6 times to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
s4, preparing glass slurry: and (4) weighing the varnish according to the proportion, adding the solid powder obtained in the step S3 into the varnish, fully and uniformly mixing, and then mixing for 4-6 times by using a three-roll grinder to obtain the glass slurry.
In examples 7 to 12, the weight ratios of the glass cullet pieces, the black pigment, and the varnish (polymer resin and aqueous solvent), the heat treatment temperature and time, and the ball milling rotation speed and the ball milling time of the dry milling are shown in table 2 below.
Comparative example black glass paste was prepared using cullet base prepared in examples 1-4 above
Comparative example 1 the cullet block base prepared in example 1 was selected;
comparative example 2 the cullet block base prepared in example 2 was selected;
comparative example 3 the cullet block base prepared in example 3 was selected;
comparative example 4 the cullet base prepared in example 4 was used.
Comparative example 1
This comparative example differs from example 7 in that:
the cullet base material is directly prepared into solid powder without being subjected to heat treatment in step S2.
S3, preparing solid powder:
wet grinding: respectively weighing broken glass block base materials and black pigment according to the proportion, mixing, putting the mixture into a ball mill for wet milling after mixing, wherein the ball milling rotation speed is 270rpm, the ball milling time is 120min, and drying to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
the rest steps are the same.
Comparative example 2
This comparative example differs from example 8 in that:
the cullet base material is directly prepared into solid powder without being subjected to heat treatment in step S2.
S3, preparing solid powder:
wet grinding: respectively weighing broken glass block base materials and black pigment according to the proportion, mixing, putting the mixture into a ball mill for wet milling after mixing, wherein the ball milling rotation speed is 270rpm, the ball milling time is 120min, and drying to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
the rest steps are the same.
Comparative example 3
This comparative example differs from example 9 in that:
the cullet base material is directly prepared into solid powder without being subjected to heat treatment in step S2.
S3, preparing solid powder:
wet grinding: respectively weighing broken glass block base materials and black pigment according to the proportion, mixing, putting the mixture into a ball mill for wet milling after mixing, wherein the ball milling rotation speed is 270rpm, the ball milling time is 120min, and drying to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
the rest steps are the same.
Comparative example 4
This comparative example differs from example 10 in that:
the cullet base material is directly prepared into solid powder without being subjected to heat treatment in step S2.
S3, preparing solid powder:
wet grinding: respectively weighing broken glass block base materials and black pigment according to the proportion, mixing, putting the mixture into a ball mill for wet milling after mixing, wherein the ball milling rotation speed is 270rpm, the ball milling time is 120min, and drying to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
the rest steps are the same.
In comparative examples 1 to 4, the weight ratios of the raw material cullet pieces, the black pigment powder, and the varnish (polymer resin and aqueous solvent), the ball milling rotation speed and the ball milling time in the wet milling are shown in table 2 below.
Comparative example 5
Comparative example 5 cullet base prepared in example 4 was selected
This comparative example differs from example 10 in that:
s3, preparing solid powder:
wet grinding: respectively weighing the broken glass blocks and the black pigment according to the proportion, mixing, putting the mixture into a ball mill for wet milling at the ball milling speed of 270rpm for 120min, and drying to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
comparative example 6
Comparative example 6 cullet base prepared in example 4 was selected
This comparative example differs from example 10 in that:
the cullet base material was not subjected to the heat treatment of step S2, and the rest of the steps were the same.
In comparative example 6, the weight ratios of the glass cullet pieces, the black pigment, and the varnish (polymer resin and aqueous solvent), the ball milling rotation speed and the ball milling time of the dry milling are shown in table 2 below.
Effects of the embodiment
The black glass pastes prepared in the above examples 7 to 12 and comparative examples 1 to 6 were respectively tempered by the following method:
and (2) screen-printing the glass slurry on glass by using a 250-mesh screen, wherein the wet film thickness of the glass slurry is 18-22 mu m, and then sintering the glass slurry at a certain temperature to form a slurry layer with the thickness of 13-17 mu m.
The slurry layers after tempering of examples 7 to 12 and comparative examples 1 to 6 were subjected to the optical density and acid resistance tests, and the test results are shown in table 2 below.
TABLE 2
In conclusion, the low-temperature environment-friendly black glass slurry with high optical density prepared by the invention does not contain Pb, halogen elements and Cr which are harmful to the environment6+The glass paste meets the environmental protection standard of RoHS of European Union, the broken glass block base material is subjected to heat treatment and water quenching, and the solid powder is subjected to high-speed and low-speed dry grinding treatment, so that the optical density value of the glass paste is greater than 5, the covering power of the glass paste is greatly improved, the glaze surface gloss is good after tempering at 640-680 ℃, and the glass paste has extremely high blackness and excellent acid and alkali resistance.
Finally, it should be noted that the above embodiments are only used for illustrating and not limiting the technical solutions of the present invention, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the present invention without departing from the spirit and scope of the present invention, and all modifications or partial substitutions should be covered by the scope of the claims of the present invention.
Claims (8)
1. The low-temperature environment-friendly black glass paste with high optical density is characterized by comprising the following raw materials in parts by weight: 40-75% of broken glass blocks, 15-45% of black pigment and 12-25% of varnish; the sum of the weight proportions of the broken glass blocks, the black pigment and the varnish is 100%;
the preparation method of the low-temperature environment-friendly black glass paste with high optical density comprises the following steps:
s1, preparation of a cullet base material:
s1.1 mixing: weighing SiO according to the weight ratio2、Bi2O3、ZnO、B2O3、Na2O、K2O、TiO2、ZrO2Mixing in a mixer to obtain a mixture;
s1.2, melting: placing the mixture obtained in the step S1.1 into a crucible and placing the crucible into a muffle furnace for melting, wherein the melting temperature is 1000-1200 ℃, and the heat preservation time is 40-120 min, so as to obtain glass liquid;
s1.3, ice water quenching: quenching the glass liquid obtained in the step S1.2 by deionized ice water, and drying to obtain a glass cullet block base material;
s2, heat treatment: placing the glass cullet block base material obtained in the step S1.3 in a muffle furnace for heat treatment, performing deionized water quenching after the heat treatment, and repeating for 3-5 times to obtain glass cullet blocks;
s3, preparing solid powder:
dry grinding: respectively weighing the glass cullet blocks and the black pigment obtained in the step S2 according to the proportion, mixing, placing the mixture into a ball mill for medium-free ball milling with a material-ball ratio of 1:5, performing high-speed dry milling treatment, performing low-speed dry milling treatment, and repeating for 3-6 times to obtain mixed powder of glass powder and black pigment powder with the particle size of 2-10 mu m, namely solid powder;
s4, preparing glass slurry: and (4) weighing the varnish according to the proportion, adding the solid powder obtained in the step S3 into the varnish, fully and uniformly mixing, and then mixing for 4-6 times by using a three-roll grinder to obtain the glass slurry.
2. The low-temperature environment-friendly black glass paste with high optical density as claimed in claim 1, wherein the cullet pieces comprise the following raw materials by weight: 17 to 37% SiO2、20～60％Bi2O3、4～20％ZnO、4～19％B2O3、1～12％Na2O、0～5％K2O、1～4％TiO2、0.5～6％ZrO2(ii) a The black pigment is copper-chromium black pigment; the varnish is prepared by mixing 15-35 wt% of polymer resin and 40-85 wt% of water-based solvent.
3. The low-temperature environment-friendly black glass paste with high optical density as claimed in claim 2, wherein the cullet pieces are prepared from the following raw materials in parts by weight: 17.3% SiO2、55％Bi2O3、14.5％ZnO、4.1％B2O3、3.1％Na2O、1.6％K2O、3.9％TiO2、0.5％ZrO2。
4. The low-temperature environment-friendly black glass paste with high optical density as claimed in claim 2, wherein the polymer resin is one or more of ethyl cellulose, acrylic resin and polyvinyl alcohol resin; the aqueous solvent is one or more of diethylene glycol butyl ether, terpineol, diethylene glycol butyl ether acetate and ethyl oleate.
5. The low-temperature eco-friendly black glass paste according to claim 1, wherein in the step S2, the heat treatment temperature is 350 to 450 ℃ and the heat treatment time is 25 to 35 min.
6. The low-temperature eco-friendly black glass paste having high optical density according to claim 1, wherein in the step S3, dry grinding at high speed: the ball milling speed is 230-270 rpm, the ball milling time is 10-30 min, and the low-speed dry milling is carried out: the ball milling speed is 90-120 rpm, and the ball milling time is 110-140 min.
7. The low-temperature environment-friendly black glass paste with high optical density according to claim 5, wherein the glass paste obtained in the step S4 is tempered by the following method: and (2) screen-printing the glass slurry on glass by using a 250-mesh screen, wherein the wet film thickness of the glass slurry is 18-22 mu m, and then sintering at 640-680 ℃ to form a slurry layer with the thickness of 13-17 mu m.
8. The low-temperature eco-friendly black glass paste according to claim 7, wherein the optical density of the paste layer is greater than 5.
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| CN113087399A (en) * | 2021-04-07 | 2021-07-09 | 淄博宝晶新材料股份有限公司 | Environment-friendly low-expansion high-covering-power glass powder for electrical appliance |
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Effective date of registration: 20220923 Address after: In Qingyuan National Industrial Park, Chengnan, Lianzhou City, Qingyuan City, Guangdong Province, 511500 Patentee after: QINGYUAN BAOJING NEW MATERIAL Co.,Ltd. Address before: 245702 Huangshan Industrial Park, Huangshan City, Anhui Province Patentee before: Huangshan Jingtemei New Materials Co.,Ltd. |