CN112574675A - Glass polishing solution, preparation method thereof and polishing method using glass polishing solution - Google Patents
Glass polishing solution, preparation method thereof and polishing method using glass polishing solution Download PDFInfo
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- CN112574675A CN112574675A CN201910925995.5A CN201910925995A CN112574675A CN 112574675 A CN112574675 A CN 112574675A CN 201910925995 A CN201910925995 A CN 201910925995A CN 112574675 A CN112574675 A CN 112574675A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
- B24B57/02—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents
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Abstract
The invention provides a glass polishing solution, a preparation method thereof and a polishing treatment method using the glass polishing solution. The glass polishing solution comprises a first concentrated solution and a second concentrated solution, wherein the first concentrated solution comprises: 40-60 parts by weight of polishing powder containing cerium oxide; 1-5 parts by weight of a first dispersant; 0.001 to 0.005 parts by weight of a surfactant; and 34.995-58.999 parts by weight of water, wherein the second concentrated solution comprises: 40-60 parts by weight of cerium oxide polishing powder; 0.2-0.5 parts by weight of a second dispersant; 0.2-0.5 parts by weight of a third dispersant; and 39 to 59.6 parts by weight of water, wherein the density of the first dispersant is not less than 1.5g/cm3The density of the second dispersant and the third dispersant is less than 1.5g/cm3. The glass polishing solution has the advantages of no accumulation of dispersant, good dispersing and suspending effects, and good stabilityThe method has the advantages of good qualitative performance, long service life, stable grinding rate, stable polishing effect and high yield; the surfactant can not be accumulated, a large amount of foam can not be generated in the polishing process, an additional defoaming agent is not needed, the grinding speed is high, and the polishing effect is good.
Description
Technical Field
The invention relates to the technical field of chemistry, in particular to a glass polishing solution, a preparation method thereof and a method for polishing treatment by using the glass polishing solution.
Background
At present, with the rapid development of 5G communication and wireless charging technologies and the continuous evolution of mobile phone appearance aesthetic designs, glass gradually replaces metal and becomes the mainstream material of high-end smart phone cover plates. Glass polishing is one of the indispensable processing steps in order to achieve a dazzling optical effect and a good touch. In the related art, there are 3 technical solutions for preparing glass polishing solutions: no. 1 is CeO2Directly adding water into the polishing powder to dilute the polishing powder to the required use concentration; 2, preparing polishing powder, a dispersing agent, a suspending agent, a surfactant, a polishing assistant, a pH regulator and the like into polishing solution with required use concentration; and the 3 rd is that polishing powder, dispersant, suspending agent, surfactant, polishing assistant, pH regulator, etc. are compounded into concentrated liquid and the concentrated liquid is diluted into required concentration. However, the glass polishing solution in the above scheme still has poor stability, and the grinding rate and polishing effect are still to be improved.
Thus, the related art of the existing glass polishing solution still needs to be improved.
Disclosure of Invention
The present invention has been completed based on the following findings of the inventors:
in the related art, CeO2The polishing solution prepared by directly adding water to dilute the polishing powder to the required use concentration has the following defects: only adding small amount of dispersant, CeO2The suspension effect of the particles is poor, and the particles are easy to sink when standingReducing, and the polishing powder particles are agglomerated after sedimentation and difficult to re-disperse; on the other hand, overflow of the foam in the liquid sump leads to CeO2The loss of particles increases the consumption of polishing powder, thereby causing waste; in addition, the concentration of the polishing solution during production is measured by measuring specific gravity, and the existence of foam can significantly affect the measurement result, thereby affecting the judgment of production personnel.
Based on the above, an object of the present invention is to provide a glass polishing solution, which has the advantages of no dispersion agent accumulation, no dispersion, good suspension effect, good stability, long service life, stable grinding rate, stable polishing effect, high polishing yield, no surfactant accumulation, no generation of a large amount of foam during polishing, no need of an additional defoaming agent, good grinding rate, or good polishing effect.
In one aspect of the present invention, the present invention provides a glass polishing solution. According to an embodiment of the present invention, the glass polishing liquid includes a first concentrated liquid and a second concentrated liquid, the first concentrated liquid including: 40 to 60 parts by weight of a polishing powder containing cerium oxide; 1 to 5 parts by weight of a first dispersant; 0.001 to 0.005 parts by weight of a surfactant; and 34.995-58.999 parts by weight of water, the second concentrated solution comprising: 40-60 parts by weight of cerium oxide polishing powder; 0.2 to 0.5 parts by weight of a second dispersant; 0.2 to 0.5 parts by weight of a third dispersant; and 39 to 59.6 parts by weight of water, wherein the density of the first dispersant is not less than 1.5g/cm3The density of the second dispersant and the third dispersant is less than 1.5g/cm3. The inventor finds that the dispersing agent can not be accumulated when the glass polishing solution is used, and the glass polishing solution has good dispersing and suspending effects, good stability, long service life, stable grinding speed, stable polishing effect and high polishing yield; the surfactant can not be accumulated, a large amount of foam can not be generated in the polishing process, an additional defoaming agent is not needed, the grinding speed is high, and the polishing effect is good.
In another aspect of the present invention, there is provided a method for preparing the glass polishing liquid as described above. According to an embodiment of the invention, the method comprises: mixing raw materials for preparing a first concentrated solution to obtain the first concentrated solution; and mixing the raw materials for preparing the second concentrated solution to obtain the second concentrated solution. The inventor finds that the method is simple and convenient to operate, easy to implement and easy for industrial production, the glass polishing solution can be effectively prepared, and the prepared glass polishing solution has the advantages of no dispersion agent accumulation, good dispersion and suspension effects, good stability, long service life, stable grinding rate, stable polishing effect and high polishing yield when in use; the surfactant can not be accumulated, a large amount of foam can not be generated in the polishing process, an additional defoaming agent is not needed, the grinding speed is high, and the polishing effect is good.
In still another aspect of the present invention, there is provided a method of polishing treatment using the glass polishing liquid described above. According to an embodiment of the invention, the method comprises: adding the first concentrated solution with the preset density into polishing equipment and carrying out the polishing treatment; and adding a second concentrated solution into the polishing equipment when the real-time density of the first concentrated solution in the polishing equipment is less than the preset density. The inventors found that when the glass polishing solution described above is used for polishing, the grinding rate is stable, the polishing effect is stable, and the polishing yield is high; a large amount of foam can not be generated in the polishing process, additional defoaming agent is not needed, the grinding speed is good, and the polishing effect is good.
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FIG. 1 shows a schematic flow chart of a method for preparing a glass polishing solution according to an embodiment of the present invention.
FIG. 2 is a schematic flow chart showing a method for preparing a glass polishing solution according to another embodiment of the present invention.
FIG. 3 is a schematic flow chart showing a method of polishing with a glass polishing liquid according to an embodiment of the present invention.
FIG. 4 is a schematic flow chart showing a method of polishing with a glass polishing liquid according to another embodiment of the present invention.
FIG. 5 is a schematic flow chart showing a method of polishing with a glass polishing liquid according to still another embodiment of the present invention.
FIG. 6 is a graph showing the grinding rate of the glass polishing liquids of example 1, example 2, example 3, example 4, comparative example 1, comparative example 2 and comparative example 3 according to the present invention as a function of time.
FIG. 7 is a graph showing the roughness of the polished products subjected to the polishing treatment with the glass polishing liquids of examples 1, 2, 3, 4, 1, 2 and 3 according to the present invention as a function of time.
FIG. 8 is a graph showing the change of the appearance yield with time of the polished products subjected to the polishing treatment with the glass polishing liquids of example 1, example 2, example 3, example 4, comparative example 1, comparative example 2 and comparative example 3 according to the present invention.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
In one aspect of the present invention, the present invention provides a glass polishing solution. According to an embodiment of the present invention, the glass polishing liquid includes a first concentrated liquid and a second concentrated liquid, the first concentrated liquid including: 40 to 60 parts by weight of a polishing powder containing cerium oxide; 1 to 5 parts by weight of a first dispersant; 0.001 to 0.005 parts by weight of a surfactant; and 34.995-58.999 parts by weight of water, the second concentrated solution comprising: 40-60 parts by weight of cerium oxide polishing powder; 0.2 to 0.5 parts by weight of a second dispersant; 0.2 to 0.5 parts by weight of a third dispersant; and 39 to 59.6 parts by weight of water, wherein the density of the first dispersant is not less than 1.5g/cm3The density of the second dispersant and the third dispersant is less than 1.5g/cm3. The inventor finds that the glassThe dispersing agent can not be accumulated when the glass polishing solution is used, and the glass polishing solution has good dispersing and suspending effects, good stability, long service life, stable grinding speed, stable polishing effect and high polishing yield; the surfactant can not be accumulated, a large amount of foam can not be generated in the polishing process, an additional defoaming agent is not needed, the grinding speed is high, and the polishing effect is good.
According to the embodiments of the present invention, the inventors have conducted intensive studies on a glass polishing solution, and found that the reason why the polishing effect of the glass polishing solution in the related art is poor is mainly that: when the glass polishing solution is used, the polishing powder and other components are consumed unevenly, the consumption of the polishing powder is high, concentrated solution with the same components is directly supplemented, the accumulation of other added components is caused, particularly, the accumulation of an additive with higher specific gravity causes the deficiency and the increase of the specific gravity of the working polishing solution, and then production personnel are misled to judge the effective component CeO according to the specific gravity2The concentration of the particles can not supplement effective grinding component CeO in time2Particles, resulting in a significant decrease in grinding rate and a deterioration in polishing effect. Therefore, the inventor breaks through the general cognition that each component in the glass polishing solution only can exist as a whole in the related technology, divides each component in the polishing solution into a first concentrated solution and a second concentrated solution, and adds a first dispersing agent with higher density in the glass polishing solution into the first concentrated solution, and because the density of the first dispersing agent is higher, the consumption period is longer than that of the polishing powder containing cerium oxide, if the first dispersing agent is added in the use process of the glass polishing solution, the first dispersing agent can be continuously accumulated, so that the density of the whole glass polishing solution is continuously accumulated, and the judgment of a producer on the adding time is influenced; then, the second dispersing agent with lower density is added into the second concentrated solution, and because the second dispersing agent with lower density and short consumption period are used, the second dispersing agent can not be accumulated even if the second dispersing agent is continuously added into the glass polishing solution, so that the glass polishing solution has stable grinding speed, stable polishing effect and high polishing yield; in addition, the surfactant is added into the first concentrated solution, so that the accumulation of the surfactant is avoided, a large amount of foam is not generated in the use process of the glass polishing solution, no additional defoaming agent is required to be added, and no additional defoaming agent is requiredThe grinding rate and polishing effect are affected.
According to the embodiment of the present invention, the specific kind of the first dispersant is not particularly limited as long as the density thereof is not less than 1.5g/cm3That is, specifically, the density of the first dispersant may be 1.6g/cm3、1.7g/cm3、1.8g/cm3、1.9g/cm3、2.0g/cm3、2.1g/cm3、2.2g/cm3、2.3g/cm3、2.4g/cm3Or 2.5g/cm3And the like. Therefore, the dispersing agent with higher density can be added into the first concentrated solution, the application range is wide, the dispersing agent can be applied to glass polishing solution formed by various kinds of polishing powder, and the using effect is good.
In some embodiments of the present invention, the first dispersant may specifically include sodium hexametaphosphate, sodium tripolyphosphate, and the like. Wherein the molecular formula of the sodium hexametaphosphate is (NaPO)3)6Total phosphate (as P)2O5Calculated as P) content of more than or equal to 68.0 percent and inactive phosphate (calculated as P)2O5Calculated) content is less than or equal to 7.5 percent, and content of water insoluble substances is less than or equal to 0.04 percent; molecular formula of sodium tripolyphosphate Na5P3O10The content is more than or equal to 96 percent, and the content of water insoluble substances is less than or equal to 0.1 percent. Therefore, the polishing powder containing cerium oxide in the first concentrated solution can be well dispersed and suspended, and CeO can be avoided2CeO with nano-scale particle size and poor particle dispersion effect2The particles are easy to be adsorbed on the surface of the glass, and are difficult to be removed by cleaning, thus easily causing the technical problem of dirt.
According to the embodiment of the present invention, the specific kinds of the second and third dispersants are not particularly limited as long as the density thereof is less than 1.5g/cm3That is, specifically, the density of the second dispersant and the third dispersant may be each independently 1.0g/cm3、1.1g/cm3、1.2g/cm3、1.3g/cm3Or 1.4g/cm3And the like. Therefore, the dispersing agent with low density can be added into the second concentrated solution, the application range is wide, the dispersing agent can be applied to glass polishing solution formed by various kinds of polishing powder, and the using effect is good.
In some specific embodiments of the present invention, the second dispersant may specifically include polyacrylic acid, sodium polyacrylate, and the like; the third dispersant may specifically include PEG-4000, PEG-2000, PEG-1000, or the like. Therefore, the polishing powder containing cerium oxide in the second concentrated solution can be well dispersed and suspended, wherein the second dispersing agent is adsorbed on the surfaces of cerium oxide particles to enable the cerium oxide particles to be negatively charged, and the dispersion and suspension effects are achieved through electrostatic repulsion; the third dispersing agent is adsorbed on the surface of the cerium oxide particles, and achieves the dispersing effect through the steric hindrance effect among long-chain molecules.
According to an embodiment of the present invention, specific kinds of the surfactant may include sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, and the like. Therefore, the polishing liquid has wide material source, is easy to obtain and low in cost, can reduce the surface tension of the polishing liquid, plays a role in wetting, enables the polishing liquid to be better contacted with glass to be polished, can play a role in lubricating simultaneously, enables the ground substances to be timely taken away from the surface of the glass to be polished, exposes a fresh surface, and avoids the phenomenon that plastic particles ground by a brush on a polishing disc, air in wool strips and sponge, relative movement between the polishing disc and glass, circular flow of the polishing liquid and stirring in a liquid storage tank can cause a machine table and the liquid storage tank to generate a large amount of foam in the related technology. On the one hand the bubbles occupy a space such that CeO is in contact with the glass2Particle reduction, grinding rate reduction, and possible entrapment of CeO by bubbles2Particles, which worsens the grinding effect.
According to embodiments of the present invention, the mass percentage of the cerium oxide in the cerium oxide-containing polishing powder is not particularly limited, for example, in some embodiments of the present invention, the mass percentage of the cerium oxide is 70% to 95%, and further, in some specific embodiments, the mass percentage of the cerium oxide in the cerium oxide-containing polishing powder may be 70% to 85% (i.e., medium cerium polishing powder) or not less than 95% (i.e., high cerium polishing powder). Therefore, the polishing powder of the glass polishing solution can contain cerium oxide with different contents, so that the application range is wider.
According to the embodiment of the invention, the polishing powder with the cerium oxide content of 70-85% by mass may further contain rare earth oxide, rare earth oxyfluoride, and the like. Specifically, the rare earth oxide may specifically include lanthanum oxide, neodymium oxide, praseodymium oxide, or the like; the rare earth oxyfluoride may specifically include lanthanum oxyfluoride, neodymium oxyfluoride, praseodymium oxyfluoride, or the like. Therefore, in the polishing powder of the glass polishing solution, the application range is wider, and the polishing effect is better.
According to the embodiment of the invention, the polishing powder containing the cerium oxide in a mass percentage of not less than 95% further contains a rare earth oxide, wherein specific components of the rare earth oxide are the same as those described above, and are not described in detail herein.
According to the embodiment of the present invention, the particle size and specific gravity of the polishing powder containing cerium oxide can be flexibly selected by those skilled in the art according to actual needs, and will not be described in detail herein.
In other embodiments of the present invention, the second concentrate may further include fluoride, inorganic electrolyte, and antimicrobial agent. According to the embodiment of the invention, the fluoride can be specifically sodium fluoride, potassium fluoride or ammonium fluoride and the like, and can better increase the grinding rate of the polishing solution and improve the polishing efficiency through the chemical corrosion effect; the inorganic electrolyte may include sodium chloride, sodium nitrate, potassium chloride, potassium nitrate, ammonium chloride, ammonium nitrate, or the like, which may enhance the surface electrical properties of the polishing powder particles, improve the dispersion effect, and further improve the polishing effect; the antimicrobial agent may specifically be barium metaborate, which is effective in preventing the polishing slurry from molding.
In another aspect of the present invention, there is provided a method for preparing the glass polishing liquid as described above. According to an embodiment of the invention, referring to fig. 1, the method comprises the steps of:
s10: and mixing the raw materials for preparing the first concentrated solution to obtain the first concentrated solution.
According to the embodiment of the present invention, the specific manner of mixing the raw materials for preparing the first concentrated solution is not particularly limited as long as the components in the first concentrated solution can be mixed and uniformly dispersed, and specifically, for example, the raw materials can be directly added into water to be uniformly mixed, which is not described in detail herein. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
S20: and mixing the raw materials for preparing the second concentrated solution to obtain the second concentrated solution.
According to the embodiment of the present invention, the specific manner of mixing the raw materials for preparing the second concentrated solution is not particularly limited as long as the components in the second concentrated solution can be mixed and dispersed uniformly, and specifically, for example, the raw materials can be directly added into water to be mixed uniformly, which is not described in detail herein. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
In further embodiments of the present invention, referring to fig. 2, in particular, the method may comprise the steps of:
s11: adding a first dispersant to water at 40-70 ℃ under stirring to obtain a first mixture.
According to the embodiment of the invention, the water can be conventional water, and can also be ultrapure water or deionized water.
According to the embodiment of the present invention, the temperature may be in the range of 40 ℃ to 70 ℃, and specifically, for example, 40 ℃, 50 ℃, 60 ℃, or 70 ℃ may be used. Therefore, the first mixture can be obtained well, and the temperature is not too high to cause excessive energy consumption or exceed the heat-resistant limit of the groove body, or is not too low to cause slow dissolution and caking of the dispersing agent.
According to the embodiment of the invention, the stirring mode, the stirring speed and the like are the conventional stirring mode and speed, and are not described in detail herein.
According to the embodiment of the invention, specifically, the required amount of water is heated to 40-70 ℃ in a first tank with a stirring and air blowing device, the stirring and bottom air blowing of the device is opened, the required amount of first dispersing agent is slowly added, and after the first dispersing agent is completely dissolved and does not adhere to the bottom of the tank, the solution is transferred to a second tank. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
S12: adding a surfactant to the first mixture while stirring the first mixture to obtain a second mixture.
According to an embodiment of the present invention, specifically, it may be that the desired amount of the surfactant is added in the second tank with stirring means while stirring. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
S13: adding a polishing powder containing cerium oxide to the second mixture under stirring of the second mixture to obtain the first concentrated solution.
According to the embodiment of the present invention, in the second tank described above, a desired amount of the polishing powder containing cerium oxide is slowly added under stirring and sufficiently stirred for 1 hour or more to ensure uniform dispersion. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
S21: adding the second dispersant and the third dispersant to water under stirring to obtain a third mixture.
According to the embodiment of the present invention, the required amount of water is added to the second tank described above, and the required amount of the second dispersant and the third dispersant are added while stirring, and sufficiently stirred until completely dissolved. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
S22: adding a polishing powder containing cerium oxide to the third mixture under stirring of the third mixture to obtain the second concentrated solution.
According to the embodiment of the present invention, a desired amount of the polishing powder containing cerium oxide is slowly added to the second tank under stirring, and sufficiently stirred for more than 1 hour to ensure uniform dispersion. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
According to the embodiment of the present invention, in particular, it can be understood by those skilled in the art that since the preparation processes of the first concentrated solution and the second concentrated solution are independent from each other, the sequence of the above steps is only an example, wherein the sequence between S11, S12, S13 and S21, S22 can be exchanged, for example, S21, S22 can be performed first, and then S11, S12, S13 can be performed; of course, S21, S22, S11, S12 and S13 may be performed simultaneously, and are not described herein in detail.
Still further, in a more specific embodiment of the present invention, the step of preparing the first concentrate may comprise: heating required amount of water to 40-70 ℃ in a first tank (the tank body is made of polyvinyl chloride, the capacity is 400-600L, and the inner diameter is 600-800 mm) with a heating device (the heating power is 4-8 kW); then opening stirring (the stirring device adopts a paddle type stirring paddle, the material of the blade is polyvinyl chloride, the shape of the blade is a straight blade type, the number of the blades is 2-4, the length of a single blade is 200-300 mm, the width of the blade is 30-60 mm, the distance between the stirring paddle and the bottom of the tank is 1/3-1/2 which accounts for the height of the tank body, the rotating speed of the stirring paddle is 60-90 rpm, the stirring power is 1-3 kW), and blowing air at the bottom (the air blowing device is a polyvinyl chloride pipe which is communicated with the bottom of the tank and is shaped like a Chinese character 'tian', the pipe diameter is 30-50 mm, the bottom of the pipe is drilled, the hole diameter is 3-5 mm, the hole spacing is 20-40 mm, the air blowing air pressure is 0.5-0.8 MPa, the required amount of sodium hexametaphosphate is slowly added, after the sodium hexametaphosphate is completely dissolved, and the sodium hexametaphosphate at the bottom of the tank is not bonded, and then pumping the solution; adding required amount of sodium dodecyl sulfate into a second tank (the tank body is made of SUS304 stainless steel, the volume is 600L-800L, and the inner diameter is 1200 mm-1500 mm) with a stirring device (the stirring device adopts a paddle type stirring paddle, the material of the blade is SUS304 stainless steel, the shape of the blade is a straight blade type, the number of the blades is 2-4, the length of a single blade is 500 mm-700 mm, the width of the blade is 30 mm-60 mm, the distance between the stirring paddle and the tank bottom accounts for 1/3-1/2 of the height of the tank body, the rotating speed of the stirring paddle is 50-80 rpm, and the stirring power is 2 kW-4 kW); in the second tank, a desired amount of CeO was slowly added under stirring2Polishing the powder, and fully stirring for more than 1h to ensure uniform dispersion.
Furthermore, in the present inventionIn a more specific embodiment, the step of preparing the second concentrate can include: adding required amount of water into a second tank (the tank body is made of SUS304 stainless steel, the volume is 600L-800L, and the inner diameter is 1200 mm-1500 mm), adding required amount of polyacrylic acid and polyethylene glycol PEG-4000 under stirring, and fully stirring until the polyacrylic acid and the polyethylene glycol PEG-4000 are completely dissolved; adding required amount of sodium fluoride or ammonium fluoride under stirring, and fully stirring until the sodium fluoride or ammonium fluoride is completely dissolved; adding required amount of sodium chloride (or sodium nitrate, potassium chloride, potassium nitrate, ammonium chloride or ammonium nitrate) under stirring, and stirring thoroughly to dissolve completely; adding the required amount of barium metaborate under the stirring state, and fully stirring until the barium metaborate is uniformly dispersed; slowly adding required amount of CeO under stirring2Polishing the powder and stirring for more than 1h to ensure uniform dispersion.
In addition, on one hand, in the related art, the polishing powder, the dispersing agent, the suspending agent, the surfactant, the polishing assistant, the pH regulator and the like are prepared into the polishing solution with the required use concentration without considering the consumption and supplement of each component, so that the grinding rate is continuously reduced, the polishing efficiency is reduced, and the production stability is poor. Effective component CeO in polishing liquid2The particles are continuously ground in the polishing process, edges and corners are ground, the particle size is reduced, and the effective grinding component CeO is carried out and settled along with the polishing powder2The particles are continuously consumed and the concentration decreases, while other components are unequally consumed. The concentration of polishing powder in the polishing solution cannot be accurately increased by directly adding the polishing solution with working concentration; if CeO is directly added2Polishing powder and various additives are prepared into polishing solution with working concentration, a plurality of large-capacity solution preparation tanks are needed, and the production is difficult to realize; the addition of suspending agents, such as insoluble particles of silica, kaolin, bentonite, etc., into the glass polishing solution is difficult to be mixed with CeO2Particle separation, difficult waste liquid treatment, CeO2It is difficult to recycle.
Based on this, in another aspect of the present invention, there is provided a method of polishing treatment using the glass polishing liquid described above. According to an embodiment of the invention, referring to fig. 3, the method comprises the steps of:
s100: adding the first concentrated solution with the preset density into polishing equipment and performing the polishing treatment.
According to an embodiment of the present invention, the concentration of diluting the first concentrate may be in a mass ratio of the first concentrate to water of 1: 2-1: and 5, diluting the solution, adding the diluted solution into polishing equipment as a slotting solution, wherein the concentration of the diluted first concentrated solution is the working concentration of the glass polishing solution during polishing treatment, and the working concentration can be characterized by measuring the density. Therefore, the concentration of the effective components in the first concentrated solution in the polishing equipment can be obtained, so that the second concentrated solution can be supplemented later.
S200: and adding a second concentrated solution into the polishing equipment when the real-time density of the first concentrated solution in the polishing equipment is less than the preset density.
According to the embodiment of the invention, specifically, after a first preset time, the real-time density of the first concentrated solution in the polishing equipment is measured, and if the real-time density is smaller than the preset density, a second concentrated solution is added into the polishing equipment, wherein the first preset time is 5-8 hours. In some specific embodiments of the present invention, the first predetermined time may be 5h, 6h, 7h, 8h, or the like. Therefore, the second concentrated solution has low density and short consumption period, so that the second dispersing agent cannot be accumulated even if the second concentrated solution is continuously supplemented during the glass polishing solution, and further, the glass polishing solution has stable grinding rate and stable polishing effect.
In other embodiments of the present invention, referring to fig. 4, the method may further comprise the steps of:
s300: adding the first concentrated solution to the polishing apparatus after every second predetermined time.
According to an embodiment of the invention, the second predetermined time is 7 to 15 days. In some specific embodiments of the present invention, the second predetermined time may be 7 days, 8 days, 9 days, 10 days, 11 days, 12 days, 13 days, 14 days, 15 days, or the like. Therefore, the polishing solution can keep good dispersion and suspension properties, the polished glass is easy to clean, the cleanliness is high, and the surfactant can be supplemented timely, so that excessive foams can be prevented.
In still other embodiments of the present invention, referring to fig. 5, the method may further comprise the steps of:
s400: and cleaning the glass polishing solution in the polishing device after a third preset time.
According to an embodiment of the invention, the third predetermined time is between 30 days and 60 days. In some specific embodiments of the present invention, the second predetermined time may be 30 days, 35 days, 40 days, 45 days, 50 days, 55 days, 60 days, or the like. Thus, after the third predetermined time has elapsed, the glass polishing solution is deactivated, so that the glass polishing solution in the polishing apparatus can be cleaned, and then S100 is repeated, thereby performing the polishing process again.
The following describes embodiments of the present invention in detail.
EXAMPLE 1 preparation of glass polishing solution
The first concentrate in this example had the following composition and weight percentages:
50 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
3 parts by weight of sodium hexametaphosphate (total phosphate as P)2O5Calculated) is 68.1 percent by mass; non-active phosphates (as P)2O5Calculated) is 6.5 percent; the mass percentage content of the water-insoluble substance is 0.03 percent);
0.002 parts by weight of sodium dodecyl sulfate;
46.998 parts by weight of water (conventional water).
The preparation process of the first concentrated solution comprises the following steps:
heating 500L of water to 50 ℃ in a first tank (the tank body is made of polyvinyl chloride, the capacity is 500L, and the inner diameter is 700mm) with a heating device (the heating power is 6 kW);
opening stirring (the number of blades is 4, the length of a single blade is 300mm, the width of the blade is 50mm, the distance between the stirring paddle and the bottom of the tank is 1/2 which accounts for the height of the tank body, the rotating speed of the stirring paddle is 70rpm, the stirring power is 2kW), blowing gas at the bottom of the pipe (the pipe diameter is 40mm, the hole diameter is 4mm, the hole distance is 30mm, and the blowing gas pressure is 0.6MPa), slowly adding 32kg of sodium hexametaphosphate, and pumping the solution to a second tank by using a water pump (the power is 1.5kW) after the sodium hexametaphosphate is completely dissolved and is not bonded at the bottom of the tank;
0.021kg of sodium dodecyl sulfate is added into a second tank (the volume is 700L, the inner diameter is 1300mm) with a stirring device (the number of blades is 4, the length of a single blade is 600mm, the width of the blade is 50mm, the distance between a stirring paddle and the bottom of the tank accounts for 1/2 of the height of the tank body, the rotating speed of the stirring paddle is 50rpm, and the stirring power is 4 kW);
in the second tank, 532kg of CeO was slowly added under stirring2Polishing the powder, and fully stirring for more than 1h to ensure uniform dispersion.
The second concentrate of this example had the following composition and weight percentages:
50 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
0.3 parts by weight of polyacrylic acid ((CH)2CH)nCOOH)；
0.3 parts by weight of polyethylene glycol PEG-4000(HO (CH)2CH2O)nH)；
0.2 parts by weight of sodium chloride (NaCl);
0.2 parts by weight of barium metaborate (Ba (BO)2)2)；
49 parts by weight of water (conventional water).
The preparation process of the second concentrated solution comprises the following steps: adding 500L of water into a second tank, adding 3kg of polyacrylic acid and 3kg of polyethylene glycol PEG-4000 under stirring, and fully stirring until the polyacrylic acid and the polyethylene glycol PEG-4000 are completely dissolved; adding 2kg of sodium chloride under stirring, and fully stirring until the sodium chloride is completely dissolved; adding 2kg of barium metaborate under stirring, and fully stirring until the barium metaborate is uniformly dispersed; 510kg of CeO was slowly added under stirring2Polishing the powder and stirring for more than 1h to ensure uniform dispersion.
Example 2 preparation of glass polishing solution
In comparison to example 1, sodium fluoride was added to the second concentrate.
The components and the manufacturing process of the first concentrated solution in this example are the same as those in example 1.
The second concentrate of this example had the following composition and weight percentages:
50 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
0.3 parts by weight of polyacrylic acid (CH)2CH)nCOOH)；
0.3 parts by weight of polyethylene glycol PEG-4000(HO (CH)2CH2O)nH)；
0.2 parts by weight of sodium fluoride (NaF);
0.2 parts by weight of sodium chloride (NaCl);
0.2 parts by weight of barium metaborate (Ba (BO)2)2)；
48.8 parts by weight of water (conventional water).
The manufacturing process comprises the following steps:
adding 500L of water into a second tank, adding 3kg of polyacrylic acid and 3kg of polyethylene glycol PEG-4000 under stirring, and fully stirring until the polyacrylic acid and the polyethylene glycol PEG-4000 are completely dissolved; adding 2kg of sodium chloride and 2kg of sodium fluoride under stirring, and fully stirring until the sodium chloride and the sodium fluoride are completely dissolved; adding 2kg of barium metaborate under stirring, and fully stirring until the barium metaborate is uniformly dispersed; 510kg of CeO was slowly added under stirring2Polishing the powder and stirring for more than 1h to ensure uniform dispersion.
Method of polishing treatment using the glass polishing liquids of example 1 and example 2: mixing the first concentrated solution with water according to the mass ratio of the first concentrated solution to the water of 1: 3.5 adding water for dilution to serve as a polishing machine grooving liquid, wherein the specific gravity of the diluted first concentrated solution is 1.10; measuring the specific gravity of the groove opening liquid of the polishing machine every 5 hours, and supplementing the groove opening liquid with the second polishing liquid until the concentration is 1.10 when the concentration is less than 1.10; adding the first concentrated solution every 7 days according to the use condition of the machine; and cleaning the polishing machine every 30 days, and repeating the steps.
Example 3 glass polishing solution
The first concentrate in this example had the following composition and weight percentages:
40 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
2 parts by weight of sodium hexametaphosphate (total phosphate as P)2O5Calculated) is 68.1 percent by mass; non-active phosphates (as P)2O5Calculated) is 6.5 percent; the mass percentage content of the water-insoluble substance is 0.03 percent);
0.001 parts by weight of sodium dodecyl sulfate;
58.999 parts by weight of water (conventional water).
The second concentrate of this example had the following composition and weight percentages:
40 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
0.2 parts by weight of polyacrylic acid ((CH)2CH)nCOOH)；
0.2 parts by weight of polyethylene glycol PEG-4000(HO (CH)2CH2O)nH)；
0.2 parts by weight of sodium chloride (NaCl);
0.2 parts by weight of barium metaborate (Ba (BO)2)2)；
49 parts by weight of water (conventional water).
The first and second concentrated solutions in this embodiment are prepared by a similar process and using method to those in embodiment 1.
Example 4 glass polishing solution
The first concentrate in this example had the following composition and weight percentages:
60 parts by weight of middle cerium polishing powder (CeO)2Is prepared from the following components in percentage by mass80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
5 parts by weight of sodium hexametaphosphate (total phosphate as P)2O5Calculated) is 68.1 percent by mass; non-active phosphates (as P)2O5Calculated) is 6.5 percent; the mass percentage content of the water-insoluble substance is 0.03 percent);
0.005 parts by weight of sodium dodecyl sulfate;
34.995 parts by weight of water (conventional water).
The second concentrate of this example had the following composition and weight percentages:
60 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
0.5 parts by weight of polyacrylic acid ((CH)2CH)nCOOH)；
0.5 parts by weight of polyethylene glycol PEG-4000(HO (CH)2CH2O)nH)；
0.2 parts by weight of sodium chloride (NaCl);
0.2 parts by weight of barium metaborate (Ba (BO)2)2)；
39 parts by weight of water (conventional water).
The first and second concentrated solutions in this embodiment are prepared by a similar process and using method to those in embodiment 1.
Comparative example 1
The formula of the glass polishing solution is as follows:
50 parts by weight of middle cerium polishing powder (CeO)2The mass percentage of (A) is 80%: the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
3 parts by weight of sodium hexametaphosphate;
0.002 parts by weight of sodium dodecyl sulfate;
46.998 parts by weight of water (conventional water).
The using method comprises the following steps: according to the mass ratio of the glass polishing solution to water of 1: 3.5 diluting the mixture until the specific gravity is 1.10, measuring the specific gravity of the glass polishing solution every 5 hours, and supplementing the glass polishing solution with the specific gravity of 1.10 when the specific gravity is less than 1.10.
Comparative example 2
The formula of the glass polishing solution is as follows:
50 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
0.3 parts by weight of polyacrylic acid ((CH)2CH)nCOOH)；
0.3 parts by weight of polyethylene glycol PEG-4000(HO (CH)2CH2O)nH)；
0.2 parts by weight of sodium chloride (NaCl);
0.2 parts by weight of barium metaborate (Ba (BO)2)2)；
49 parts by weight of water (conventional water).
The using method comprises the following steps: according to the mass ratio of the glass polishing solution to water of 1: 3.5 diluting the mixture until the specific gravity is 1.10, measuring the specific gravity of the glass polishing solution every 5 hours, and supplementing the glass polishing solution with the specific gravity of 1.10 when the specific gravity is less than 1.10.
Comparative example 3
The components and weight percentages of the first concentrate in this comparative example are as follows:
50 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent; particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
3 parts by weight of bentonite;
0.002 parts by weight of fatty alcohol-polyoxyethylene ether;
46.998 parts by weight of water (conventional water).
The components and weight percentages of the second concentrate in this comparative example are as follows:
50 parts by weight of middle cerium polishing powder (CeO)2The mass percentage content of the compound is 80 percent; the mass percentage of the lanthanum oxide is 20 percent(ii) a Particle size: d50: 0.55 μm; d90: 1.46 μm, specific gravity 6.5);
0.3 part by weight of sodium methylene bis (methylnaphthalenesulfonate);
0.3 parts by weight of sodium ethylnaphthalenesulfonate;
0.2 parts by weight of sodium chloride (NaCl);
0.2 parts by weight of barium metaborate (Ba (BO)2)2)；
49 parts by weight of water (conventional water).
The using method comprises the following steps: mixing the first concentrated solution with water according to the mass ratio of the first concentrated solution to the water of 1: 3.5 adding water for dilution to serve as a polishing machine grooving liquid, wherein the specific gravity of the diluted first concentrated solution is 1.10; measuring the specific gravity of the groove opening liquid of the polishing machine every 5 hours, and supplementing the groove opening liquid with the second polishing liquid until the concentration is 1.10 when the concentration is less than 1.10; adding the first concentrated solution every 7 days according to the use condition of the machine; and cleaning the polishing machine every 30 days, and repeating the steps.
The performance test method comprises the following steps: 6 Yujing YJ-QP1135E curved surface polishing machines (Hunan Yujing machines, Inc.) with the same working state and capacity are selected, wherein 3 of the three curved surface polishing machines are used for 3D glass concave surface polishing, and the other 3 curved surface polishing machines are used for convex surface polishing. After cleaning the machine, the polishing solutions were added according to examples 1, 2, 3, 4 and comparative examples 1, 2, 3, and the rotational speed of the polishing pad (made of porous polyurethane) was set at 100rpm and the pressure was set at 138N/cm2The polishing time for the concave surface and the convex surface is 30 min. And after the glass is polished, the glass enters an automatic cleaning line to be cleaned for 1 h.
Grinding rate test of polishing treatment
In examples 1, 2, 3, 4, 1, 2 and 3, 30pcs 3D glass samples were taken each day, and the difference between the average thicknesses (average thickness per piece) of the 30pcs samples before and after polishing was measured by a high-precision digital thickness gauge (precision 0.001mm) and converted into the grinding thickness per unit time, thereby obtaining the grinding rate. The sampling time was 30 days. The thickness measuring method of each sample comprises the following steps: and (4) selecting upper, middle and lower 3 fixed positions to measure the thickness, and taking an average value. Before polishing, the specific gravity of the polishing solution of each machine is ensured to be 1.10, and the service time of the polishing pad is the same.
The test results of example 1, example 2, example 3, and example 4 of the present invention and comparative example 1, comparative example 2, and comparative example 3 are shown in fig. 6. As can be seen from fig. 6, the grinding rate of comparative example 1 was similar to that of example 1 at the initial stage of use of the polishing liquid, and the cumulative effect of sodium hexametaphosphate began to appear 10 days after use, and the grinding rate of the polishing liquid began to drop sharply about 20 days after use, and the grinding rate fell to half of the initial stage after 30 days after use. The grinding rate of comparative example 2 and comparative example 3 is significantly lower than that of example 1, example 2, example 3 and example 4, but the cumulative effect in comparative example 1 does not appear. In contrast, the glass polishing solutions of examples 1, 2, 3 and 4 have high grinding rate of more than 30 μm/h and good grinding stability, and example 2 preferably adds fluorine ions to further increase the grinding rate to 35 μm/h.
Roughness test of polished products
Each of examples 1, 2, 3, 4, 1, 2, and 3 was a 30-pc 3D glass sample taken every day, and the average roughness of the 30-pc sample before and after polishing was measured by a roughness tester, with a sampling time of 30 days. The thickness measuring method of each sample comprises the following steps: and (4) selecting upper, middle and lower 3 fixed positions to measure the roughness, and taking an average value. Before polishing, the specific gravity of the polishing solution of each machine is ensured to be 1.10, and the service time of the polishing pad is the same.
The test results of examples 1, 2, 3 and 4 of the present invention and comparative examples 1, 2 and 3 are shown in FIG. 7. As is clear from fig. 7, the roughness of comparative example 1 was similar to that of example 1 at the initial stage of use of the polishing liquid, and the roughness started to increase after 10 days of use, and the roughness sharply increased and the polishing effect sharply decreased after about 20 days of use. The roughness of the comparative examples 2 and 3 is obviously larger than that of the examples 1, 2, 3 and 4. In contrast, the glass polishing solutions of examples 1, 2, 3, and 4 have low surface roughness of 15nm or less and good stability after polishing, and example 2 preferably adds fluorine ions to achieve a surface roughness of 10nm or less, thereby further reducing the surface roughness and improving the polishing effect and quality.
Appearance yield test of polished products
300pcs 3D glass samples are selected in each day in the examples 1, 2, 3, 4, 1, 2 and 3, the appearance of the samples is detected by the same quality inspector, the samples without obvious appearance defects such as scratches, dirt and various marks are good products, and the good product number/inspection number (300pcs) is the appearance yield. The sampling time was 30 days.
The test results of example 1, example 2, example 3, and example 4 of the present invention and comparative example 1, comparative example 2, and comparative example 3 are shown in fig. 8. As can be seen from fig. 8, the glass polishing solutions of examples 1 and 2, 3 and 4 have good polishing effect, good surface quality, a yield of appearance of 90% or more, and stable yield.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (13)
1. A glass polishing solution is characterized by comprising a first concentrated solution and a second concentrated solution,
the first concentrate includes:
40 to 60 parts by weight of a polishing powder containing cerium oxide;
1 to 5 parts by weight of a first dispersant;
0.001 to 0.005 parts by weight of a surfactant; and
34.995 to 58.999 parts by weight of water,
the second concentrate includes:
40-60 parts by weight of cerium oxide polishing powder;
0.2 to 0.5 parts by weight of a second dispersant;
0.2 to 0.5 parts by weight of a third dispersant; and
39 to 59.6 parts by weight of water,
wherein the density of the first dispersant is not less than 1.5g/cm3The density of the second dispersant and the third dispersant is less than 1.5g/cm3。
2. The glass polishing solution according to claim 1, wherein the first dispersant comprises at least one of sodium hexametaphosphate and sodium tripolyphosphate.
3. The glass polishing solution according to claim 1, wherein the second dispersant comprises at least one of polyacrylic acid and sodium polyacrylate.
4. The glass polishing solution according to claim 1, wherein the third dispersant comprises at least one of PEG-4000, PEG-2000, and PEG-1000.
5. The glass polishing solution according to claim 1, wherein the surfactant comprises at least one of sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, and sodium dodecyl sulfate.
6. The glass polishing solution according to claim 1, wherein the cerium oxide-containing polishing powder contains 70 to 95 mass% of cerium oxide,
optionally, the content of cerium oxide in the polishing powder containing cerium oxide is 70-85% by mass or not less than 95% by mass,
optionally, the polishing powder with the cerium oxide content of 70-85% by mass also contains at least one of rare earth oxide and rare earth oxyfluoride,
optionally, the polishing powder contains a rare earth oxide in an amount of not less than 95% by mass of the cerium oxide.
7. The glass polishing solution according to claim 1, wherein the second concentrated solution further comprises at least one of a fluoride, an inorganic electrolyte, and an antibacterial agent.
8. A method for preparing the glass polishing liquid according to any one of claims 1 to 7, comprising:
mixing raw materials for preparing a first concentrated solution to obtain the first concentrated solution;
and mixing the raw materials for preparing the second concentrated solution to obtain the second concentrated solution.
9. The method of claim 8, comprising:
adding a first dispersant into water at the temperature of 40-70 ℃ under the stirring condition to obtain a first mixture;
adding a surfactant to the first mixture under the condition of stirring the first mixture to obtain a second mixture;
adding a polishing powder containing cerium oxide to the second mixture under stirring of the second mixture to obtain the first concentrated solution;
adding a second dispersant and a third dispersant into water under the stirring condition to obtain a third mixture;
adding a polishing powder containing cerium oxide to the third mixture under stirring of the third mixture to obtain the second concentrated solution.
10. A method for polishing with the glass polishing liquid according to any one of claims 1 to 7, comprising:
adding the first concentrated solution with the preset density into polishing equipment and carrying out the polishing treatment;
and adding a second concentrated solution into the polishing equipment when the real-time density of the first concentrated solution in the polishing equipment is less than the preset density.
11. The method according to claim 10, wherein a real-time density of the first concentrated solution in the polishing apparatus is measured after every lapse of a first predetermined time, and a second concentrated solution is added to the polishing apparatus if the real-time density is less than the predetermined density, the first predetermined time being 5 to 8 hours.
12. The method according to claim 10 or 11, wherein the first concentrated solution is added to the polishing apparatus every second predetermined time,
optionally, the second predetermined time is 7 days to 15 days.
13. The method according to claim 12, wherein the glass polishing liquid in the polishing apparatus is cleaned after a third predetermined time has elapsed,
optionally, the third predetermined time is 30 days to 60 days.
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