CN115431131B - Polishing method for resin lens, alumina polishing powder and preparation method thereof - Google Patents
Polishing method for resin lens, alumina polishing powder and preparation method thereof Download PDFInfo
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- CN115431131B CN115431131B CN202211388339.4A CN202211388339A CN115431131B CN 115431131 B CN115431131 B CN 115431131B CN 202211388339 A CN202211388339 A CN 202211388339A CN 115431131 B CN115431131 B CN 115431131B
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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
- B24B13/00—Machines or devices designed for grinding or polishing optical surfaces on lenses or surfaces of similar shape on other work; Accessories therefor
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention discloses a polishing method of resin lenses, alumina polishing powder and a preparation method thereof, wherein the polishing method adopts a unique process for preparing the alumina polishing powder, then the alumina polishing powder is mixed with a solvent to prepare alumina polishing solution, and then the alumina polishing solution is adopted to polish the resin lenses; in the process for preparing the alumina polishing powder, the first pseudo-boehmite and the aluminum nitrate are mixed in a solvent to form a gelatinous mixture, the gelatinous mixture and the second pseudo-boehmite are uniformly mixed and dried to obtain an intermediate to be calcined, and then operations such as granularity control and material mixing are performed.
Description
Technical Field
The invention relates to the technical field of polishing of resin lenses, in particular to a polishing method of a resin lens, alumina polishing powder and a preparation method thereof.
Background
The optical resin lens is made of organic materials, is of a macromolecular chain structure, is of a three-dimensional net structure, is relatively loose in intermolecular structure, has a space capable of generating relative displacement between molecular chains, is high in light transmittance and good in light transmittance, and is widely applied to the fields of spectacle lenses, optical lenses, building material lamp decoration and the like due to the characteristics of light weight, high impact resistance, low cost, easiness in processing and the like.
At present, in the practical application process, resin lenses are usually required to be polished, in the polishing process of the resin lenses, aluminum oxide is often used as a polishing medium to prepare polishing liquid due to high hardness and high physical cutting force, wherein the aluminum oxide can be prepared by calcining pseudo-boehmite, but the polishing liquid prepared by preparing the aluminum oxide by adopting the pseudo-boehmite has the defects of more or less severe use conditions, poor polishing efficiency and polishing quality, poor Baume stability, short service life and the like.
In view of the above problems, patent CN113817411 discloses a method for polishing an alumina substrate polishing solution prepared by an improved method, however, although the patent achieves advantages of better polishing efficiency, low scratch and the like to a certain extent, on one hand, boric acid needs to be mixed with pseudo-boehmite by a dry method, and the phenomenon of uneven mixing easily occurs between boric acid as a substance in a powder form and pseudo-boehmite which is also a solid substance, and even if the mixing is even, higher requirements are put on equipment or even mixing time; on the other hand, the patent also requires compaction operation after mixing, and the method adopted by the patent is to pack the mixture into a box body for compaction, and the practice finds that the process has the problem of different compaction degrees of each batch, especially when the uniformity of the mixture of powder materials in the current period is different or the shape and the size of the raw materials are fluctuated, the uniformity and the compaction effect of the compaction have certain changes, the quality of the final polished product is more likely to be influenced, and the quality stability among batches is severely challenged.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming one or more defects in the prior art and providing an improved polishing method for resin lenses, which has relatively simple process and low equipment requirements on the basis of having relatively excellent polishing efficiency and polishing quality, and can also maintain the relative stability of the process and ensure the polishing quality stability of the polishing process among batches.
The invention also provides a preparation method of the alumina polishing powder and the alumina polishing powder prepared by the method.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method of polishing a resin lens, the method comprising: a step of polishing a resin lens with an alumina polishing liquid, a step of dispersing an alumina polishing powder in a first solvent to form the alumina polishing liquid, and a step of preparing the alumina polishing powder; wherein, the process for preparing the alumina polishing powder comprises the following steps:
mixing a first pseudo-boehmite with aluminum nitrate in a second solvent to form a colloidal mixture;
uniformly mixing the gelatinous mixture with second pseudo-boehmite, and drying to obtain an intermediate to be calcined; the total amount of the first pseudo-boehmite and the second pseudo-boehmite is calculated by 100 mass percent, the first pseudo-boehmite is controlled to occupy 5% -20% and the second pseudo-boehmite is controlled to occupy 80% -95%;
the intermediate to be calcined is calcined and then made into powder particles of a desired particle size, which are optionally mixed with an auxiliary agent.
According to some preferred aspects of the present invention, the total amount of the first pseudo-boehmite and the second pseudo-boehmite is controlled to be 7% -15% and the second pseudo-boehmite is controlled to be 85% -93% in terms of 100% by mass.
Further, the total amount of the first pseudo-boehmite and the second pseudo-boehmite is controlled to be 8% -12% by mass percent, and the amount of the second pseudo-boehmite is controlled to be 88% -92% by mass percent.
According to a specific aspect of the invention, the total amount of the first pseudo-boehmite and the second pseudo-boehmite is controlled to be 10% and the amount of the second pseudo-boehmite is controlled to be 90% in terms of 100% by mass.
In the invention, the description of the first pseudo-boehmite and the second pseudo-boehmite is only for distinguishing that the pseudo-boehmite is added in different stages, so that the pseudo-boehmite is convenient to distinguish and understand, and the method is not limited in other aspects.
In the present invention, the first pseudo-boehmite and the second pseudo-boehmite may be pseudo-boehmite of the same source, or pseudo-boehmite of different sources, preferably pseudo-boehmite of the same source, so as to facilitate control of process conditions and the like.
In some embodiments of the present invention, the first pseudo-boehmite and the second pseudo-boehmite may be common pseudo-boehmite, for example, pseudo-boehmite having Na content of 0.5% or less and Si content of 0.05% or less.
According to some preferred aspects of the invention, the added mass of the aluminum nitrate accounts for 0.5% -5.0% of the feeding mass of the first pseudo-boehmite.
Further, the addition mass of the aluminum nitrate accounts for 1.0% -4.0% of the feeding mass of the first pseudo-boehmite.
According to some preferred and specific aspects of the present invention, the aluminum nitrate is added by adding an aluminum nitrate solution including aluminum nitrate and a third solvent for dispersing the aluminum nitrate.
According to some preferred aspects of the invention, the method of preparing the gum-like mixture comprises: and dispersing the first pseudo-boehmite in the second solvent to prepare a mixed material, adding the aluminum nitrate solution into the mixed material under the stirring condition, and fully stirring.
According to some preferred and specific aspects of the invention, the second solvent is water.
According to some preferred and specific aspects of the invention, the third solvent is water.
According to some preferred and specific aspects of the present invention, the ratio of the first pseudo-boehmite to the second solvent is 1:0.8-1.2 by mass.
According to some preferred and specific aspects of the present invention, the aluminum nitrate solution contains 5% -15% by mass of aluminum nitrate, for example, 5%, 6%, 8%, 9%, 10%, 11%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15% by mass, etc.
According to some preferred aspects of the present invention, the process of preparing the alumina polishing powder further comprises: before the drying, the material obtained after the gelatinous mixture and the second pseudo-boehmite are uniformly mixed is placed for 5-20 hours, so that the material can be further fully peptized, and the growth of crystal grains is facilitated.
In some embodiments of the invention, the placing may be performed at room temperature, for a period of time ranging from 5 to 15 hours, alternatively from 8 to 16 hours, alternatively from 10 to 18 hours, etc.
In some embodiments of the invention, the drying prior to obtaining the intermediate to be calcined may be carried out using an oven, which may have a temperature of, for example, 100-120 ℃.
According to some preferred aspects of the invention, the calcination is carried out at 1000-1060 ℃.
Further, the calcination is performed at 1020 to 1060 ℃. Still further, the calcination is performed at 1040-1060 ℃.
According to some preferred aspects of the invention, the specific surface area of the calcined material is controlled to be 15-20m 2 /g。
According to some preferred aspects of the present invention, the method for preparing powder particles of the desired particle size comprises:
ball milling the calcined material by a wet method until D is obtained 50 1.5-2.5 μm, D 97 Less than 12 μm;
adding sodium hexametaphosphate into the ball-milled material, uniformly mixing, and freeze-drying to obtain powder particles with expected particle size; wherein, the adding amount of the sodium hexametaphosphate is controlled to be 0.2 to 2 percent of the materials after ball milling according to the mass percent.
According to the invention, the combination treatment mode of adding sodium hexametaphosphate before wet ball milling, freeze drying and freeze drying can be more beneficial to obtaining powder particles with expected particle sizes, wherein the powder particles are more uniformly dispersed and the morphology and structure of the powder particles are basically unchanged.
In some embodiments of the invention, during wet ball milling, the particle size of the milling beads is 4-6mm, the ball ratio is 1:5-7, and the solid content of the ball milling slurry is controlled to be 30% -40%.
In some embodiments of the invention, D during wet ball milling 50 、D 97 Can be monitored by a laser particle sizer, respectively.
According to some preferred aspects of the invention, the resin lens is made of allyl diglycol dicarbonate (CR 39) or Polycarbonate (PC).
According to some preferred and specific aspects of the invention, the first solvent is water.
According to some preferred and specific aspects of the present invention, the alumina polishing solution comprises 15% -25% by mass of alumina.
According to some preferred aspects of the invention, the polishing employs a Lour polisher at a pressure of 0.3-0.5bar, a motor frequency of 48-52Hz, an alumina polishing solution temperature of 10-15 ℃, and a polishing time of 3-8min.
The invention provides another technical scheme that: a method for preparing alumina polishing powder, comprising:
mixing a first pseudo-boehmite with aluminum nitrate in a second solvent to form a colloidal mixture;
uniformly mixing the gelatinous mixture with second pseudo-boehmite, and drying to obtain an intermediate to be calcined; the total amount of the first pseudo-boehmite and the second pseudo-boehmite is calculated by 100 mass percent, the first pseudo-boehmite is controlled to occupy 5% -20% and the second pseudo-boehmite is controlled to occupy 80% -95%;
the intermediate to be calcined is calcined and then made into powder particles of a desired particle size, which are optionally mixed with an auxiliary agent.
In some embodiments of the invention, the auxiliary agent is one or a combination of more selected from the group consisting of dispersants, suspending agents, defoamers.
In some embodiments of the invention, the dispersant may be acrylic acid.
In some embodiments of the present invention, the dispersant is added in an amount of 2.0% to 6.0% by mass of the powder particles of the desired particle size.
In some embodiments of the invention, the suspending agent may be a lubosch K739 suspending agent.
In some embodiments of the present invention, the suspending agent is added in an amount of 0.5% to 2.0% by mass of the powder particles of the desired particle size.
In some embodiments of the invention, the defoamer may be defoamer B-10, available from federal fine chemical company, inc.
In some embodiments of the present invention, the defoamer is added in an amount of 2.0% to 5.0% by mass of the powder particles of the desired particle size.
The invention provides another technical scheme that: the alumina polishing powder prepared by the preparation method. The alumina polishing powder disclosed by the invention can be used for conveniently matching polishing liquid with any concentration by a user according to the conditions of the material, the processing technology and the like of a polishing piece, has high flexibility, is convenient for adjusting the concentration according to the polishing effect, and is convenient for storing and transporting.
The invention provides another technical scheme that: an alumina polishing solution comprising the above alumina polishing powder and the above first solvent.
In some embodiments of the present invention, the alumina polishing solution can be formed by dispersing an alumina polishing powder in a first solvent.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention is based on the defects of high requirements on equipment, hidden danger of the polishing quality stability among batches and the like of the existing polishing process due to the characteristics of the process, and the like, in the process of a large number of experimental researches, the invention occasionally discovers that aluminum nitrate and a certain amount of pseudo-boehmite are firstly prepared into a colloid mixture with cohesiveness, and then are mixed with a specific amount of pseudo-boehmite. In addition, in the process of the invention, the uniform mixing operation can be qualitatively and quantitatively finished, so that the fluctuation caused by the fact that the consistency of the existing compacting effect is greatly limited by factors such as earlier-stage mixing is avoided.
Drawings
FIG. 1 is a metallographic microscope image of a CR39 resin lens prior to polishing in an application example of the present invention;
FIG. 2 is a metallographic microscope image of a PC resin lens prior to polishing in an application example of the present invention;
FIG. 3 is a metallographic microscope image of a CR39 resin lens polished in application example 1 of the present invention;
FIG. 4 is a metallographic microscope image of a PC resin lens polished in application example 1 of the present invention;
FIG. 5 is a metallographic microscope image of a CR39 resin lens polished in application example 2 of the present invention;
FIG. 6 is a metallographic microscope image of a PC resin lens polished in application example 2 of the present invention;
FIG. 7 is a metallographic microscope image of a CR39 resin lens polished in application example 3 of the present invention;
FIG. 8 is a metallographic microscope image of a PC resin lens polished in application example 3 of the present invention;
FIG. 9 is a metallographic microscope image of a CR39 resin lens of comparative example 1 after polishing as used in the present invention;
FIG. 10 is a metallographic microscope image of a PC resin lens of the invention after polishing in comparative example 1;
FIG. 11 is a metallographic microscope image of a CR39 resin lens of comparative example 2 after polishing as used in the present invention;
FIG. 12 is a metallographic microscope image of a PC resin lens of the invention after polishing in comparative example 2;
FIG. 13 is a metallographic microscope image of a CR39 resin lens of comparative example 3 after polishing as used in the present invention;
FIG. 14 is a metallographic microscope image of a PC resin lens polished in comparative example 3, to which the present invention was applied.
Detailed Description
The above-described aspects are further described below in conjunction with specific embodiments; it should be understood that these embodiments are provided to illustrate the basic principles, main features and advantages of the present invention, and that the present invention is not limited by the scope of the following embodiments; the implementation conditions employed in the examples may be further adjusted according to specific requirements, and the implementation conditions not specified are generally those in routine experiments.
In the following, all starting materials are commercially available or prepared by methods conventional in the art, unless otherwise specified. In the following, unless otherwise specified, "%" means mass percent.
Example 1
The embodiment provides a preparation method of alumina polishing powder and the alumina polishing powder prepared by the preparation method, and specifically, the preparation method of the alumina polishing powder comprises the following steps:
1) Common pseudo-boehmite (measured: na content: 0.5%, si content: 0.01% available from the Shandong aluminum industry) as a starting material;
preparing 10% of common pseudo-boehmite raw materials and deionized water with the same weight into suspension, adding an aluminum nitrate aqueous solution (the mass percentage of aluminum nitrate in the aluminum nitrate aqueous solution is 10%, controlling the adding mass of aluminum nitrate to be 2% of the adding mass of the common pseudo-boehmite prepared into the suspension at the time), and fully stirring to prepare a gelatinous mixture;
2) Uniformly mixing the gelatinous mixture with the rest 90% pseudo-boehmite in the common pseudo-boehmite raw material, and standing for 12 hours;
3) Placing the mixture into a baking oven after 12 hours, and drying the mixture at 110 ℃;
4) The dried material is put into a calciner for calcination, the calcination temperature is 1046 ℃, and the specific surface area of the calcined material is 19.3m 2 /g；
5) Ball milling the calcined material (ball milling particle size is 5mm, ball ratio is 1:6, mill power: 1.1kw, motor frequency at 30Hz for abrasive material), ball milling to monitor particle size D with a Markov laser particle sizer 50 =2.0μm、D 97 Stopping ball milling when the solid content is 9.8 mu m, and obtaining ball milling feed liquid with the solid content of 38.3% after ball milling;
6) Adding sodium hexametaphosphate (the added mass is 1% of the ball milling feed liquid) into the ball milling feed liquid after ball milling, uniformly mixing, and then enabling the materials to be at-40 DEG CPre-freezing for 4 hours under the condition of 0.5Pa vacuum pressure and drying for 8 hours, wherein the detection granularity of the obtained powder by using a Markov laser particle sizer is as follows: d (D) 50 =1.9μm，D 97 =9.0μm；
7) Dispersing agent acrylic acid is sequentially added into the material after freeze drying: 3.5 percent (accounting for mass percent of the material after freeze drying), mixing for 10 minutes, and adding a suspending agent: lu Borun K739:1.2 percent (accounting for mass percent of the material after freeze drying) of the raw materials, and mixing for 10 minutes; and then adding an antifoaming agent B-10:3.0 percent (accounting for mass percent of the material after freeze drying), purchased from Guangdong Federal fine chemical industry Co., ltd.) and mixed for 10 minutes to obtain alumina polishing powder.
Example 2
The embodiment provides a preparation method of alumina polishing powder and the alumina polishing powder prepared by the preparation method, and specifically, the preparation method of the alumina polishing powder comprises the following steps:
1) Common pseudo-boehmite (measured: na content: 0.3%, si content: 0.03%, purchased from the aluminum industry, shandong) as a raw material;
preparing 10% of common pseudo-boehmite raw materials and deionized water with the same weight into suspension, adding an aluminum nitrate aqueous solution (the mass percentage of aluminum nitrate in the aluminum nitrate aqueous solution is 10%, controlling the adding mass of aluminum nitrate to be 3.5% of the adding mass of the common pseudo-boehmite prepared into the suspension at the time), and fully stirring to prepare a colloidal mixture;
2) Uniformly mixing the gelatinous mixture with the rest 90% pseudo-boehmite in the common pseudo-boehmite raw material, and standing for 14h;
3) Placing the mixture into a baking oven after 14 hours, and drying the mixture at 110 ℃;
4) Calcining the dried material in a calciner at 1053 deg.c to obtain calcined material with specific surface area of 17.9m 2 /g；
5) Ball milling the calcined material (ball milling particle size is 5mm, ball ratio is 1:6, mill power: 1.1kw, motor frequency at 30Hz for abrasive material), ball milling to monitor particle size D with a Markov laser particle sizer 50 =1.8μm、D 97 Stop ball milling when=9.3 μm, after ball millingObtaining ball milling feed liquid with the solid content of 37.6%;
6) Adding sodium hexametaphosphate (the added mass is 1.5% of the ball milling feed liquid) into the ball milling feed liquid after ball milling, uniformly mixing, pre-freezing the material for 4 hours at the temperature of-43 ℃, and drying the material for 9 hours under the vacuum pressure of 0.6Pa, wherein the detection granularity of the obtained powder by using a Markov laser particle sizer is as follows: d (D) 50 =1.82μm，D 97 =8.9μm；
7) Dispersing agent acrylic acid is sequentially added into the material after freeze drying: 3.5 percent (accounting for mass percent of the material after freeze drying), mixing for 10 minutes, and adding a suspending agent: lu Borun K739:1.5 percent (accounting for mass percent of the material after freeze drying) of the raw materials, and mixing for 10 minutes; and then adding an antifoaming agent B-10:2.8 percent (accounting for mass percent of the material after freeze drying) of the powder is purchased from Guangdong Federal fine chemical industry Co., ltd, and is mixed for 10 minutes to obtain alumina polishing powder.
Example 3
The embodiment provides a preparation method of alumina polishing powder and the alumina polishing powder prepared by the preparation method, and specifically, the preparation method of the alumina polishing powder comprises the following steps:
1) Common pseudo-boehmite (measured: na content: 0.5%, si content: 0.01% available from the Shandong aluminum industry) as a starting material;
preparing a suspension from 12% of common pseudo-boehmite raw materials and deionized water with the same weight, adding an aluminum nitrate aqueous solution (the mass percentage of aluminum nitrate in the aluminum nitrate aqueous solution is 10%, controlling the adding mass of aluminum nitrate to be 2.5% of the adding mass of the common pseudo-boehmite prepared into the suspension at the time), and fully stirring to prepare a colloidal mixture;
2) Uniformly mixing the gelatinous mixture with the rest 88% pseudo-boehmite in the common pseudo-boehmite raw material, and standing for 12 hours;
3) Placing the mixture into a baking oven after 12 hours, and drying the mixture at 110 ℃;
4) The dried material is put into a calciner for calcination, the calcination temperature is 1050 ℃, and the specific surface area of the calcined material is 18.4m 2 /g；
5) Ball milling (grinding) the calcined materialBead diameter is 5mm, ball ratio is 1:6, mill power: 1.1kw, motor frequency at 30Hz for abrasive material), ball milling to monitor particle size D with a Markov laser particle sizer 50 =2.3μm、D 97 Ball milling feed liquid with a solid content of 35.9%, which is=14.8 μm;
6) Adding sodium hexametaphosphate (the added mass is 1.5% of the ball milling feed liquid) into the ball milling feed liquid after ball milling, uniformly mixing, pre-freezing the material for 4 hours at the temperature of minus 45 ℃, and drying the material for 8.5 hours under the vacuum pressure of 0.6Pa, wherein the detection granularity of the obtained powder by using a Markov laser particle sizer is as follows: d (D) 50 =2.23μm，D 97 =13.8μm；
7) Dispersing agent acrylic acid is sequentially added into the material after freeze drying: 3.5 percent (accounting for mass percent of the material after freeze drying), mixing for 10 minutes, and adding a suspending agent: lu Borun K739:1.5 percent (accounting for mass percent of the material after freeze drying) of the raw materials, and mixing for 10 minutes; and then adding an antifoaming agent B-10:2.8 percent (accounting for mass percent of the material after freeze drying) of the powder is purchased from Guangdong Federal fine chemical industry Co., ltd, and is mixed for 10 minutes to obtain alumina polishing powder.
Example 4
The embodiment provides a preparation method of alumina polishing powder and the alumina polishing powder prepared by the preparation method, and specifically, the preparation method of the alumina polishing powder comprises the following steps:
1) Common pseudo-boehmite (measured: na content: 0.5%, si content: 0.02%, available from Shandong aluminum industry) as a starting material;
preparing 10% of common pseudo-boehmite raw materials and deionized water with the same weight into suspension, adding an aluminum nitrate aqueous solution (the mass percentage of aluminum nitrate in the aluminum nitrate aqueous solution is 10%, controlling the adding mass of aluminum nitrate to be 2.0% of the adding mass of the common pseudo-boehmite prepared into the suspension at the time), and fully stirring to prepare a colloidal mixture;
2) Uniformly mixing the gelatinous mixture with the rest 90% pseudo-boehmite in the common pseudo-boehmite raw material, and standing for 12 hours;
3) Placing the mixture into a baking oven after 12 hours, and drying the mixture at 110 ℃;
4) Dried materialPlacing into a calciner for calcination, wherein the calcination temperature is 1050 ℃, and the specific surface area of the calcined material is 18.5m 2 /g；
5) Ball milling the calcined material (ball milling particle size is 5mm, ball ratio is 1:6, mill power: 1.1kw, motor frequency at 30Hz for abrasive material), ball milling to monitor particle size D with a Markov laser particle sizer 50 =2.2μm、D 97 Stopping ball milling when the solid content is 13.7 mu m, and obtaining ball milling feed liquid with the solid content of 36.8% after ball milling;
6) Adding sodium hexametaphosphate (the added mass is 1.0% of the ball milling feed liquid) into the ball milling feed liquid after ball milling, uniformly mixing, pre-freezing the material for 4 hours at the temperature of minus 45 ℃, and drying the material for 8 hours under the vacuum pressure of 0.6Pa, wherein the detection granularity of the obtained powder by using a Markov laser particle sizer is as follows: d (D) 50 =2.18μm，D 97 =13.2μm；
7) Dispersing agent acrylic acid is sequentially added into the material after freeze drying: 3.5 percent (accounting for mass percent of the material after freeze drying), mixing for 10 minutes, and adding a suspending agent: lu Borun K739:1.5 percent (accounting for mass percent of the material after freeze drying) of the raw materials, and mixing for 10 minutes; and then adding an antifoaming agent B-10:2.8 percent (accounting for mass percent of the material after freeze drying) of the powder is purchased from Guangdong Federal fine chemical industry Co., ltd, and is mixed for 10 minutes to obtain alumina polishing powder.
Example 5
The embodiment provides a preparation method of alumina polishing powder and the alumina polishing powder prepared by the preparation method, and specifically, the preparation method of the alumina polishing powder comprises the following steps:
1) Common pseudo-boehmite (measured: na content: 0.4%, si content: 0.02%, available from Shandong aluminum industry) as a starting material;
8% of common pseudo-boehmite raw materials and deionized water with the same weight are taken to prepare suspension, aluminum nitrate aqueous solution (the mass percentage of aluminum nitrate in the aluminum nitrate aqueous solution is 10 percent) is added while stirring, the adding mass of the aluminum nitrate is controlled to be 1.5% of the adding mass of the common pseudo-boehmite prepared into the suspension at the time, and the mixture is fully stirred to prepare a colloidal mixture;
2) Uniformly mixing the gelatinous mixture with the rest 92% pseudo-boehmite in the common pseudo-boehmite raw material, and standing for 13h;
3) 13h later, putting the mixture into a baking oven, and drying the mixture at 110 ℃;
4) Calcining the dried material in a calciner at 1055 deg.c to obtain calcined material with specific surface area of 17.1m 2 /g；
5) Ball milling the calcined material (ball milling particle size is 5mm, ball ratio is 1:6, mill power: 1.1kw, motor frequency at 30Hz for abrasive material), ball milling to monitor particle size D with a Markov laser particle sizer 50 =2.2μm、D 97 Stopping ball milling when the solid content is 14.0 mu m, and obtaining ball milling feed liquid with the solid content of 38.0% after ball milling;
6) Adding sodium hexametaphosphate (the added mass is 1.5% of the ball milling feed liquid) into the ball milling feed liquid after ball milling, uniformly mixing, pre-freezing the material for 4 hours at the temperature of minus 40 ℃, and drying the material for 9 hours under the vacuum pressure of 0.5Pa, wherein the detection granularity of the obtained powder by using a Markov laser particle sizer is as follows: d (D) 50 =2.16μm，D 97 =12.8μm；
7) Dispersing agent acrylic acid is sequentially added into the material after freeze drying: 3.5 percent (accounting for mass percent of the material after freeze drying), mixing for 10 minutes, and adding a suspending agent: lu Borun K739:1.5 percent (accounting for mass percent of the material after freeze drying) of the raw materials, and mixing for 10 minutes; and then adding an antifoaming agent B-10:2.8 percent (accounting for mass percent of the material after freeze drying) of the powder is purchased from Guangdong Federal fine chemical industry Co., ltd, and is mixed for 10 minutes to obtain alumina polishing powder.
Example 6
The embodiment provides a preparation method of alumina polishing powder and the alumina polishing powder prepared by the preparation method, and specifically, the preparation method of the alumina polishing powder comprises the following steps:
1) Common pseudo-boehmite (measured: na content: 0.3%, si content: 0.02%, available from Shandong aluminum industry) as a starting material;
preparing a suspension from 12% of common pseudo-boehmite raw materials and deionized water with the same weight, adding an aluminum nitrate aqueous solution (the mass percentage of aluminum nitrate in the aluminum nitrate aqueous solution is 10%, controlling the adding mass of aluminum nitrate to be 2.0% of the adding mass of the common pseudo-boehmite prepared into the suspension at the time), and fully stirring to prepare a colloidal mixture;
2) Uniformly mixing the gelatinous mixture with the rest 88% pseudo-boehmite in the common pseudo-boehmite raw material, and standing for 13h;
3) 13h later, putting the mixture into a baking oven, and drying the mixture at 110 ℃;
4) The dried material is put into a calciner for calcination, the calcination temperature is 1042 ℃, and the specific surface area of the calcined material is 19.9m 2 /g；
5) Ball milling the calcined material (ball milling particle size is 5mm, ball ratio is 1:6, mill power: 1.1kw, motor frequency at 30Hz for abrasive material), ball milling to monitor particle size D with a Markov laser particle sizer 50 =1.6μm、D 97 Stopping ball milling when the solid content is 7.9 mu m, and obtaining ball milling feed liquid with the solid content of 38.0% after ball milling;
6) Adding sodium hexametaphosphate (the added mass is 1.5% of the ball milling feed liquid) into the ball milling feed liquid after ball milling, uniformly mixing, pre-freezing the material for 4 hours at the temperature of minus 45 ℃, and drying the material for 9 hours under the vacuum pressure of 0.5Pa, wherein the detection granularity of the obtained powder by using a Markov laser particle sizer is as follows: d (D) 50 =1.61μm，D 97 =8.2μm；
7) Sequentially adding dispersant sodium hexametaphosphate into the freeze-dried material: 3.5 percent (accounting for mass percent of the material after freeze drying), mixing for 10 minutes, and adding a suspending agent: lu Borun K739:1.5 percent (accounting for mass percent of the material after freeze drying) of the raw materials, and mixing for 10 minutes; and then adding an antifoaming agent B-10:2.8 percent (accounting for mass percent of the material after freeze drying) of the powder is purchased from Guangdong Federal fine chemical industry Co., ltd, and is mixed for 10 minutes to obtain alumina polishing powder.
Comparative example 1
Compared with example 1, the difference is that: 1) In the process of forming a gelatinous mixture, 40% of common pseudo-boehmite raw materials and deionized water with the same weight are taken to prepare suspension; 2) Uniformly mixing the gelatinous mixture with the rest 60% pseudo-boehmite in the common pseudo-boehmite raw material; the remainder was the same as in example 1.
Comparative example 2
Compared with example 1, the difference is that: combining 1), 2) and 3) into one step, and combining to obtain the final product: all the common pseudo-boehmite raw materials and deionized water with the same weight are made into suspension, aluminum nitrate aqueous solution (the mass percentage of aluminum nitrate in the aluminum nitrate aqueous solution is 10 percent) is added while stirring, the adding mass of the aluminum nitrate is controlled to be 2 percent of the adding mass of the common pseudo-boehmite for making the suspension, the mixture is fully stirred to prepare a gelatinous mixture, and then spray drying is carried out. The remainder was the same as in example 1.
Comparative example 3
Compared with example 1, the difference is that: aluminum nitrate was replaced with boric acid, and boric acid was 5% -6% soluble in pure water at normal temperature, weak acid, and added as an aqueous boric acid solution, and the remainder was the same as in example 1.
Application example 1
The present example provides a polishing method of a resin lens, the polishing method comprising: a step of polishing a resin lens with an alumina polishing liquid, a step of dispersing an alumina polishing powder in water to form an alumina polishing liquid, and a step of preparing an alumina polishing powder;
wherein the resin lens is a CR39 resin lens; the mass percentage of alumina in the alumina polishing solution is 20%; the procedure of example 1 was used for the preparation of alumina polishing powder; polishing with a Layer polisher (model TORO-X-2S), pressure of 0.4bar, motor frequency of 50.4Hz, alumina polishing solution temperature of 13+ -2deg.C, and polishing time of 5min;
a metallographic microscope image of the CR39 resin lens before polishing is shown in fig. 1;
a metallographic microscope image of the PC resin lens before polishing is shown in fig. 2;
a metallographic microscope image of the CR39 resin lens after polishing is shown in fig. 3;
a metallographic microscope image of the polished PC resin lens is shown in fig. 4;
the average value of the removal amount of the CR39 resin lens is 165mg/5min, the quality yield of the lens is 96.5% (the statistical value of 200 lenses are polished, the lens is observed with naked eyes under a strong light after being wiped by alcohol, the condition that the scratches are little or no is considered to be satisfactory is considered as the same as the following), and the metallographic microscopic image of the polished CR39 resin lens shows that: the surface quality is good (a metallographic microscope can see the polished state of the surface more deeply, and the surface is more accurate than naked eyes);
the average value of the removal amount of the PC resin lens is 66mg/5min, the quality yield of the lens is 96.3% (the statistical value of 200 lenses is polished, the lens is observed with naked eyes under a strong light after being wiped by alcohol, the scratch is less or no, the following is the same), and the metallographic microscopic image of the polished PC resin lens shows that: the surface quality is good (a metallographic microscope can see the polished state of the surface more deeply, and the surface is more accurate than naked eyes).
Application example 2
Compared with application example 1, the difference is that: the procedure of example 2 was used for the preparation of alumina polishing powder, and the remainder was the same as in application example 1;
a metallographic microscope image of the CR39 resin lens after polishing is shown in fig. 5;
a metallographic microscope image of the PC resin lens after polishing is shown in fig. 6;
the average value of the removal amount of the CR39 resin lens is 160mg/5min, the quality yield of the lens is 98%, and the metallographic microscopic image of the polished CR39 resin lens shows that: the surface quality is good;
the average value of the removal amount of the PC resin lens is 63mg/5min, the quality yield of the lens is 97.5%, and the metallographic microscopic image of the polished PC resin lens shows that: the surface quality is good.
Application example 3
Compared with application example 1, the difference is that: the procedure of example 3 was used for the preparation of alumina polishing powder, and the remainder was the same as in application example 1.
A metallographic microscope image of the CR39 resin lens after polishing is shown in fig. 7;
a metallographic microscope image of the PC resin lens after polishing is shown in fig. 8;
the average value of the removal amount of the CR39 resin lens is 166mg/5min, the quality yield of the lens is 95.8%, and the metallographic microscopic image of the polished CR39 resin lens shows that: the surface quality is good;
the average value of the removal amount of the PC resin lens is 68mg/5min, the quality yield of the lens is 96%, and the metallographic microscopic image of the polished PC resin lens shows that: the surface quality is good.
Comparative example 1 was used
Compared with application example 1, the difference is that: the procedure of comparative example 1 was used for the preparation of alumina polishing powder, and the remainder was the same as in application example 1.
A metallographic microscope image of the CR39 resin lens after polishing is shown in fig. 9;
a metallographic microscope image of the PC resin lens after polishing is shown in fig. 10;
the average value of the removal amount of the CR39 resin lens is 170mg/5min, the quality yield of the lens is 80%, and the metallographic microscopic image of the polished CR39 resin lens shows that: the surface quality is relatively poor;
the average value of the removal amount of the PC resin lens is 68mg/5min, the quality yield of the lens is 79%, and the metallographic microscopic image of the polished PC resin lens shows that: the surface quality is relatively poor.
Comparative example 2 was used
Compared with application example 1, the difference is that: the procedure of comparative example 2 was used for the preparation of alumina polishing powder, and the remainder was the same as in application example 1.
A metallographic microscope image of the CR39 resin lens after polishing is shown in fig. 11;
a metallographic microscope image of the PC resin lens after polishing is shown in fig. 12;
the average value of the removal amount of the CR39 resin lens is 144mg/5min, the quality yield of the lens is 96%, and the metallographic microscopic image of the polished CR39 resin lens shows that: the surface quality is good;
the average value of the removal amount of the PC resin lens is 48mg/5min, the quality yield of the lens is 97.2%, and the metallographic microscopic image of the polished PC resin lens shows that: the surface quality is good.
Comparative example 3 was used
Compared with application example 1, the difference is that: the procedure of comparative example 3 was used for the preparation of alumina polishing powder, and the remainder was the same as in application example 1.
A metallographic microscope image of the CR39 resin lens after polishing is shown in fig. 13;
a metallographic microscope image of the PC resin lens after polishing is shown in fig. 14;
the average value of the removal amount of the CR39 resin lens is 105mg/5min, the quality yield of the lens is 95%, and the metallographic microscopic image of the polished CR39 resin lens shows that: the surface quality is good;
the average value of the removal amount of the PC resin lens is 46mg/5min, the quality yield of the lens is 95.6%, and the metallographic microscopic image of the polished PC resin lens shows that: the surface quality is good.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, but are not intended to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.
Claims (13)
1. A method of polishing a resin lens, the method comprising: the method is characterized by further comprising the steps of dispersing alumina polishing powder in a first solvent to form the alumina polishing solution and preparing the alumina polishing powder; wherein, the process for preparing the alumina polishing powder comprises the following steps:
mixing the first pseudo-boehmite with aluminum nitrate in a second solvent to form a gelatinous mixture, wherein the addition mass of the aluminum nitrate accounts for 0.5-5.0% of the feeding mass of the first pseudo-boehmite, and the second solvent is water;
uniformly mixing the gelatinous mixture with second pseudo-boehmite, standing for 5-20h, and drying to obtain an intermediate to be calcined; the total amount of the first pseudo-boehmite and the second pseudo-boehmite is calculated by 100 mass percent, the first pseudo-boehmite is controlled to occupy 5% -20% and the second pseudo-boehmite is controlled to occupy 80% -95%;
calcining the intermediate to be calcined, preparing the intermediate to be calcined into powder particles with expected particle size, and mixing the powder particles with expected particle size with an auxiliary agent;
allowing the calcination to proceed at 1000-1060 ℃;
the preparation method of the powder particles with the expected particle size comprises the following steps: ball milling the calcined material by a wet method until D is obtained 50 1.5-2.5 μm, D 97 Less than 12 μm;
adding sodium hexametaphosphate into the ball-milled material, uniformly mixing, and freeze-drying to obtain powder particles with expected particle size; wherein, the adding amount of the sodium hexametaphosphate is controlled to be 0.2 to 2 percent of the materials after ball milling according to the mass percent.
2. The method of claim 1, wherein the total amount of the first pseudo-boehmite and the second pseudo-boehmite is controlled to be 7% to 15% and the second pseudo-boehmite is controlled to be 85% to 93% in terms of 100% by mass.
3. The method of polishing a resin lens according to claim 2, wherein the total amount of the first pseudo-boehmite and the second pseudo-boehmite is controlled to be 8% to 12% and the second pseudo-boehmite is controlled to be 88% to 92% in terms of 100% by mass.
4. The method for polishing a resin lens according to claim 1, wherein the added mass of aluminum nitrate is 1.0% -4.0% of the charged mass of the first pseudo-boehmite.
5. The method of polishing a resin lens according to any one of claims 1 to 4, wherein the aluminum nitrate is added by adding an aluminum nitrate solution comprising aluminum nitrate and a third solvent for dispersing aluminum nitrate.
6. The method for polishing a resin lens according to claim 5, wherein the method for preparing the colloidal mixture comprises: and dispersing the first pseudo-boehmite in the second solvent to prepare a mixed material, adding the aluminum nitrate solution into the mixed material under the stirring condition, and fully stirring.
7. The method for polishing a resin lens according to claim 6, wherein the third solvent is water, and the mass ratio of the first pseudo-boehmite to the second solvent is 1:0.8-1.2; and/or the mass percentage of the aluminum nitrate in the aluminum nitrate solution is 5-15%.
8. The method for polishing a resin lens according to claim 1, wherein the placing is performed at room temperature for a period of 5 to 15 hours.
9. The method for polishing resin lens according to claim 1, wherein the specific surface area of the calcined material is controlled to be 15-20m 2 /g。
10. The method for polishing a resin lens according to claim 1, wherein the resin lens is allyl diglycol dicarbonate or polycarbonate.
11. The method for polishing a resin lens according to claim 1, wherein the first solvent is water, and the alumina content of the alumina polishing solution is 15 to 25% by mass; and/or, the polishing adopts a Layer polisher, the pressure is 0.3-0.5bar, the motor frequency is 48-52Hz, the temperature of the alumina polishing solution is 10-15 ℃, and the polishing time is 3-8min.
12. The preparation method of the alumina polishing powder is characterized by comprising the following steps:
mixing the first pseudo-boehmite with aluminum nitrate in a second solvent to form a gelatinous mixture, wherein the addition mass of the aluminum nitrate accounts for 0.5-5.0% of the feeding mass of the first pseudo-boehmite, and the second solvent is water;
uniformly mixing the gelatinous mixture with second pseudo-boehmite, standing for 5-20h, and drying to obtain an intermediate to be calcined; the total amount of the first pseudo-boehmite and the second pseudo-boehmite is calculated by 100 mass percent, the first pseudo-boehmite is controlled to occupy 5% -20% and the second pseudo-boehmite is controlled to occupy 80% -95%;
calcining the intermediate to be calcined, preparing the intermediate to be calcined into powder particles with expected particle size, and mixing the powder particles with expected particle size with an auxiliary agent;
allowing the calcination to proceed at 1000-1060 ℃;
the preparation method of the powder particles with the expected particle size comprises the following steps: ball milling the calcined material by a wet method until D is obtained 50 1.5-2.5 μm, D 97 Less than 12 μm;
adding sodium hexametaphosphate into the ball-milled material, uniformly mixing, and freeze-drying to obtain powder particles with expected particle size; wherein, the adding amount of the sodium hexametaphosphate is controlled to be 0.2 to 2 percent of the materials after ball milling according to the mass percent.
13. An alumina polishing powder, which is prepared by the preparation method of claim 12.
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| CN102516881A (en) * | 2011-12-14 | 2012-06-27 | 德米特（苏州）电子环保材料有限公司 | Manufacturing method of resin eyeglass polishing powder with alumina matrix |
| CN106637223A (en) * | 2016-12-28 | 2017-05-10 | 苏州华碧微科检测技术有限公司 | Titanium alloy material polishing method |
| CN109015204B (en) * | 2018-08-29 | 2020-11-27 | 包头市利晨科技有限公司 | Polishing method suitable for CR39 resin lens |
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