CN112592050A - Isolating agent for glass bead production and recycling method thereof - Google Patents
Isolating agent for glass bead production and recycling method thereof Download PDFInfo
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- CN112592050A CN112592050A CN202011409583.5A CN202011409583A CN112592050A CN 112592050 A CN112592050 A CN 112592050A CN 202011409583 A CN202011409583 A CN 202011409583A CN 112592050 A CN112592050 A CN 112592050A
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- powder
- glass
- separant
- glass beads
- zircon
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B40/00—Preventing adhesion between glass and glass or between glass and the means used to shape it, hold it or support it
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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
- C03B19/10—Forming beads
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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
- C03B19/10—Forming beads
- C03B19/1095—Thermal after-treatment of beads, e.g. tempering, crystallisation, annealing
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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
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- Engineering & Computer Science (AREA)
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- Thermal Sciences (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a separant for glass bead production and a recycling method thereof. The paint comprises the following components in parts by weight: 50-90 parts of graphite powder and 10-20 parts of perovskite powder and/or zircon. The separant is used for preparing the glass beads, so that the yield and the refractive index of the glass beads are improved, the reflection performance of the glass beads is improved, the reflection effect is good and the identification degree of the identification is improved when the glass beads are applied to the fields of traffic marking, labels, police uniforms and the like. After the separant is washed by acid, the perovskite powder or zircon raw material is added for renaturation, so that the separant can be recycled, the separant is saved, and the economic benefit is improved.
Description
Technical Field
The invention belongs to the technical field of glass bead manufacturing, and particularly relates to a separant for glass bead production and a recycling method thereof.
Background
The glass beads are prepared by crushing waste glass to prepare glass powder, then heating and melting the glass powder through a high-temperature furnace and forming beads under the action of surface tension. In order to prevent sintering phenomenon caused by agglomeration of the microspheres under heating, the glass powder is required to be in a floating state in the heating process, and the glass powder is rapidly peeled off through a high-temperature area, cooled, recovered and classified to finally obtain a microsphere product.
In order to reduce the bonding condition between the glass beads, a release agent is required to be added, the release agent has the function of isolating gaps between the glass beads and preventing the formed glass beads from being bonded, the release agent generally adopts carbon powder, boron nitride, magnesium oxide and the like, and the dosage of the release agent is generally 2-4 times that of the glass powder. The boron nitride and magnesium oxide separant has poor separation effect and high bonding rate, and the carbon powder is adopted as the separant, is easy to adhere to the glass beads and is difficult to completely remove even through subsequent cleaning.
The glass beads are used as a reflective material for preparing traffic markings, labels, police uniforms and the like with warning effects, the use effect can be enhanced by improving the refractive index of glass, elements such as Pb, Bi and the like are generally added into glass powder to improve the refractive index of the glass beads, but the elements such as Pb, Bi and the like are toxic elements, and the addition amount of the elements is limited by the nation. The glass beads have certain retro-reflection performance when the diameter is less than 0.8mm and the refractive index is about 1.9, and the refractive index of the currently prepared glass beads cannot meet the requirement due to the limitation of adding elements such as Pb, Bi and the like.
Disclosure of Invention
The invention aims to provide a separant for glass bead production and a recycling method thereof.
The release agent for producing the glass beads comprises the following components in parts by weight: 50-90 parts of graphite powder and 10-20 parts of perovskite powder and/or zircon.
A preparation method of glass beads comprises the following steps:
(1) cleaning waste glass, airing, crushing and sieving to obtain glass powder with the particle size of less than 300 microns;
(2) uniformly mixing glass powder and a separant, heating to 850-950 ℃, preserving heat for 20-40min, cooling to 40-60 ℃, washing with water to remove the separant, and obtaining glass beads;
(3) and (4) sending the glass beads into a color sorter to pick out the glass beads which are not cleaned, bagging the rest cleaned glass beads, and warehousing.
The mass ratio of the glass powder to the separant is 1: (2-6).
The diameter of the glass powder is 100-150 microns.
The method for recycling the collected separant after being washed by water comprises the following steps:
(1) adding acid into the collected separant washed with water, soaking for 30-60min, washing with clear water, and oven drying;
(2) crushing the separant treated in the step (1), grinding and sieving to obtain powder with the particle size of less than 30 microns;
(3) and (3) adding perovskite powder and/or zircon into the powder obtained in the step (2), and uniformly mixing to obtain the powder.
The acid is 5-10% hydrochloric acid, 3-8% sulfuric acid or 8-15% phosphoric acid.
And (3) the calcium-titanium mineral powder and/or zircon which are added account for 5-10% of the mass of the powder in the step (2).
The invention has the beneficial effects that: the separant adopts the technical scheme of compounding the graphite powder and the perovskite powder or the zircon, is used for preparing the glass beads, improves the yield and the refractive index of the glass beads, improves the reflection performance of the glass beads, and has good reflection effect and improved identification when the glass beads are applied to the fields of traffic markings, labels, police uniforms and the like. After the separant is washed by acid, the perovskite powder or zircon raw material is added for renaturation, so that the separant can be recycled, the separant is saved, and the economic benefit is improved.
Drawings
FIG. 1 shows the yield of glass beads prepared by using different dosage ratios of the separant doped with perovskite powder.
FIG. 2 shows the yield of glass microspheres prepared by using different dosage ratios of the release agent doped with zircon.
FIG. 3 shows the yield of glass beads at different heating temperatures.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
EXAMPLE 1 Release agent component selection
The inventor finds that the situation that the glass beads prepared by adopting graphite powder as the separant are seriously adhered to the separant, so that the finished product rate is low and the separant is difficult to recover through long-term practice; the preparation method of the glass beads comprises the following steps of mixing certain kinds of mineral powder with graphite powder, dispersing the mixture into a separant, and damaging a firm adhesive film of graphene adhered to the glass beads, so that the film is broken more in the process of water washing, and the separant is easy to clean, wherein the inventor adopts the compounding of the graphite powder with calcite (group 1), perovskite powder (group 2), sodalite (group 3), zircon (group 4), carbo-silica (group 5), tourmaline (group 6) or mica (group 7) to carry out experimental verification, the addition amount of the mineral powder is 25% of the mass of the graphite powder, the comparative example is no addition of the mineral powder, and the preparation method of the glass beads is carried out according to the following steps: cleaning waste glass, airing, crushing and sieving to obtain glass powder with the particle size of 120-150 microns; uniformly mixing the glass powder and the separant (the mass ratio of the glass powder to the separant is 1: 2.5), heating to 850 ℃, keeping the temperature for 25min, cooling to 50 ℃, and washing with water to remove the separant to obtain the glass beads.
Adopting a vibration color sorter to screen the prepared glass beads, wherein the black glass beads are glass beads which are not washed clean, the white glass beads are glass beads which are washed clean, and the finished product rate of the qualified finished glass beads is calculated by adopting a counter as a qualified finished product, and the calculation formula is as follows:
the yield is equal to the number of white glass bead particles/(the number of white glass bead particles + the number of black glass bead particles) X100%
The refractive indices of the samples were measured using a full-automatic refractometer GR60 (Shanghai Zollinger light apparatus), 3 of each sample were measured and averaged, and the results are shown in tables 1 and 2:
TABLE 1
Note: represents P <0.05 compared to the example 1 group.
As can be seen from Table 1, the yield of the group 2 and the group 4 is remarkably improved, and the results prove that the separation of the separant and the glass beads can be promoted by doping the perovskite powder or the zircon into the graphite powder under the washing condition, the separation of the separant and the glass beads can not be promoted by doping the calcite, the sodalite, the carbo-silica, the tourmaline or the mica into the graphite powder under the washing condition, and other types of mineral powder are selected by the inventor for tests, so that the types of the minerals which are compatible with the graphite powder and promote the separation of the separant are not found.
TABLE 2
Note: represents P <0.05 compared to the example 1 group.
As can be seen from Table 2, the refractive index of group 2 is significantly improved, and the other groups have no significant change compared with the comparative example, which proves that the refractive index of the glass beads can be significantly improved by adding the perovskite powder, and the refractive index is improved by supposing that the titanium element in the perovskite powder is mixed and blended with the glass beads.
Example 2 the amount mass ratio of the glass powder to the release agent is preferably
The best use effect is to be achieved by the release agent, the use amount is a key factor, and the application ratio gradient of the glass powder and the release agent is set in the embodiment: 1: 1. 1: 2. 1: 3. 1: 4. 1: 5. 1: 6. 1: 7. 1: 8; the preparation method of the glass beads comprises the following steps: cleaning waste glass, airing, crushing and sieving to obtain glass powder with the particle size of 120-150 microns; and (2) uniformly mixing glass powder and a separant, wherein the separant is prepared by doping 25% of perovskite powder or zircon into graphene, heating to 850 ℃, keeping the temperature for 25min, cooling to 50 ℃, and washing with water to remove the separant to obtain the glass beads.
Adopting a vibration color sorter to screen the prepared glass beads, wherein the black glass beads are glass beads which are not washed clean, the white glass beads are glass beads which are washed clean, and the finished product rate of the qualified finished glass beads is calculated by adopting a counter as a qualified finished product, and the calculation formula is as follows:
the yield is equal to the number of white glass bead particles/(the number of white glass bead particles + the number of black glass bead particles) X100%
The test results are shown in fig. 1 and fig. 2, and the release agent doped with 25% perovskite powder or zircon powder is mixed in the glass powder: the release agent is 1: the 3 places have the maximum yield and the best preparation effect.
EXAMPLE 3 optimization of melting temperature
The formation of the glass beads is mainly characterized in that the glass beads are naturally rounded at high temperature, and the melting temperature of glass in the separant is a key, so that the most appropriate heating temperature is searched, the most appropriate heating temperature is also a key factor for improving the yield of the glass beads, and a temperature gradient is set: 800 deg.C, 825 deg.C, 850 deg.C, 875 deg.C, 900 deg.C, 925 deg.C, 950 deg.C, 975 deg.C; the preparation method of the glass beads comprises the following steps: cleaning waste glass, airing, crushing and sieving to obtain glass powder with the particle size of 120-150 microns; and (3) uniformly mixing glass powder and a separant, wherein the separant is 25% of perovskite powder doped with graphene, heating to the gradient temperature, keeping the temperature for 25min, cooling to 50 ℃, and washing with water to remove the separant to obtain the glass beads.
Adopting a vibration color sorter to screen the prepared glass beads, wherein the black glass beads are glass beads which are not washed clean, the white glass beads are glass beads which are washed clean, and the finished product rate of the qualified finished glass beads is calculated by adopting a counter as a qualified finished product, and the calculation formula is as follows:
the yield is equal to the number of white glass bead particles/(the number of white glass bead particles + the number of black glass bead particles) X100%
The test results are shown in fig. 3, with the highest yield at 900 c, selected as the optimal heating temperature.
Example 4
A preparation method of glass beads comprises the following steps: cleaning waste glass, airing, crushing and sieving to obtain glass powder with the particle size of 120-150 microns; and (3) uniformly mixing glass powder and a separant, wherein the separant is prepared by doping 25% of perovskite powder into graphene, heating to 900 ℃, keeping the temperature for 25min, cooling to 50 ℃, and washing with water to remove the separant to obtain the glass beads.
Example 5
A preparation method of glass beads comprises the following steps: cleaning waste glass, airing, crushing and sieving to obtain glass powder with the particle size of 120-150 microns; and (2) uniformly mixing glass powder and a separant, wherein the separant is prepared by doping 25% zircon into graphene, heating to 900 ℃, keeping the temperature for 25min, cooling to 50 ℃, and washing with water to remove the separant to obtain the glass beads.
EXAMPLE 6 Recycling of the separant
The release agent after washing in example 4 was collected and treated as follows:
(1) adding 8% hydrochloric acid into the separant washed with water, soaking for 40min, washing with clear water, and oven drying;
(2) crushing the separant treated in the step (1), grinding and sieving to obtain powder with the particle size of less than 30 microns;
(3) and (3) adding 8% of perovskite powder into the powder obtained in the step (2), and uniformly mixing to obtain the powder.
The release agent recovered in the embodiment is added into graphene, the addition amount of the release agent is 25% of the mass of the graphene, the glass beads are prepared by the method in the embodiment 4, and the yield of the prepared glass beads is 95% of that of the embodiment 4 compared with that of the embodiment 5.
EXAMPLE 7 Recycling of the separant
The release agent after washing in example 5 was collected and treated as follows:
(1) adding 8% phosphoric acid into the separant washed with water, soaking for 40min, washing with clear water, and oven drying;
(2) crushing the separant treated in the step (1), grinding and sieving to obtain powder with the particle size of less than 30 microns;
(3) adding 8% zircon into the powder obtained in the step (2), and uniformly mixing to obtain the final product.
The release agent recovered in the embodiment is added into graphene, the addition amount of the release agent is 25% of the mass of the graphene, the glass beads are prepared by the method in the embodiment 5, and the yield of the prepared glass beads is 92% of that of the embodiment 5 compared with that of the embodiment 5.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. The release agent for producing the glass beads is characterized by comprising the following components in parts by weight: 50-90 parts of graphite powder and 10-20 parts of perovskite powder and/or zircon.
2. The preparation method of the glass beads is characterized by comprising the following steps of:
(1) cleaning waste glass, airing, crushing and sieving to obtain glass powder with the particle size of less than 300 microns;
(2) uniformly mixing glass powder and a separant, heating to 850-950 ℃, preserving heat for 20-40min, cooling to 40-60 ℃, washing with water to remove the separant, and obtaining glass beads;
(3) and (4) sending the glass beads into a color sorter to pick out the glass beads which are not cleaned, bagging the rest cleaned glass beads, and warehousing.
3. The method for preparing glass microspheres according to claim 2, wherein the amount by mass ratio of the glass powder to the release agent is 1: (2-6).
4. A method for preparing glass microspheres according to claim 2, wherein the diameter of the glass frit is 100-150 μm.
5. The method for recycling the separating agent collected after rinsing with water according to claim 2, wherein the method comprises the steps of:
(1) adding acid into the collected separant washed with water, soaking for 30-60min, washing with clear water, and oven drying;
(2) crushing the separant treated in the step (1), grinding and sieving to obtain powder with the particle size of less than 30 microns;
(3) and (3) adding perovskite powder and/or zircon into the powder obtained in the step (2), and uniformly mixing to obtain the powder.
6. The method of claim 5, wherein the acid is 5-10% hydrochloric acid, 3-8% sulfuric acid, or 8-15% phosphoric acid.
7. The method for recycling the separating agent collected after the water washing according to claim 5, wherein the supplementary perovskite powder and/or zircon accounts for 5-10% of the mass of the powder in the step (2).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014529A (en) * | 2021-12-17 | 2022-02-08 | 中国建筑材料科学研究总院有限公司 | Isolating agent for fire polishing of borosilicate glass beads |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020042088A (en) * | 2000-11-30 | 2002-06-05 | 정주일 | Production method of glass bead and its apparatus |
| CN107235639A (en) * | 2017-07-18 | 2017-10-10 | 合肥鼎亮光学科技有限公司 | A kind of preparation method of hydrophobicity reflective glass beads |
| CN110002725A (en) * | 2019-04-18 | 2019-07-12 | 中国建筑材料科学研究总院有限公司 | The preparation method of porous glass beads, the porous glass beads by this method preparation and its application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020042088A (en) * | 2000-11-30 | 2002-06-05 | 정주일 | Production method of glass bead and its apparatus |
| CN107235639A (en) * | 2017-07-18 | 2017-10-10 | 合肥鼎亮光学科技有限公司 | A kind of preparation method of hydrophobicity reflective glass beads |
| CN110002725A (en) * | 2019-04-18 | 2019-07-12 | 中国建筑材料科学研究总院有限公司 | The preparation method of porous glass beads, the porous glass beads by this method preparation and its application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014529A (en) * | 2021-12-17 | 2022-02-08 | 中国建筑材料科学研究总院有限公司 | Isolating agent for fire polishing of borosilicate glass beads |
| CN114014529B (en) * | 2021-12-17 | 2023-02-21 | 中国建筑材料科学研究总院有限公司 | Isolating agent for fire polishing of borosilicate glass beads |
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Denomination of invention: Isolating agent for glass bead production and its recovery and reuse method Effective date of registration: 20221226 Granted publication date: 20220531 Pledgee: Bank of China Limited Yongqing Sub branch Pledgor: CHIYE GLASS BEAD (HEBEI) CO.,LTD. Registration number: Y2022110000349 |