Silicon oxide polishing solution and preparation method thereof
By combining modified silica and specific suspension synergists, the dispersion and stability of the resin lens polishing liquid is solved, and efficient and environmentally friendly resin lens polishing is achieved, reducing scratches, and improving the circulation life and dispersion of the polishing liquid.
Patent Information
- Application Number
- CN202510532171.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-25
- Publication Date
- 2025-08-08
AI Technical Summary
The existing resin lens polishing liquid dispersant has poor effect, easy precipitation, low grinding efficiency, short circulation life, and easy scratches.
Modified silica is used as abrasive, and the suspension synergist is mixed with a suspension synergist, which is prepared by mixing modified polyacrylamide, sodium dodecylbenzenesulfonate and modified cetyl trimethylammonium bromide. The suspension and dispersion are improved through electrostatic action and charge neutralization, and pH adjuster, defoamer and organic solvent are added to form a silicon oxide polishing liquid with high stability suspension, high dispersion and high polishing efficiency.
It achieves good suspension under long-term shearing, improves polishing efficiency, reduces scratches, enhances stability, is safe and environmentally friendly, and is suitable for polishing of various resin lenses.
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Figure BDA0005376943330000101
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of resin lens polishing technology, and in particular to a silicon oxide polishing liquid and a preparation method thereof. Background Art
[0002] Compared to traditional glass lenses, resin lenses are not only lighter, but also offer higher clarity and superior light transmittance. However, glass lenses are harder than resin lenses because they are made of an organic material, with an internal polymer chain structure forming a three-dimensional network. The intermolecular structure is relatively loose, allowing space for relative displacement between the molecular chains. Therefore, they are easily scratched by hard objects, which creates special requirements for the polishing fluid used for resin lenses.
[0003] The grinding of hard materials such as resin lenses is carried out by grinding with a grinding disc. The grinding process requires the continuous injection of grinding fluid into the grinding disc. The quality of the grinding fluid is the main factor affecting the grinding effect. At present, the grinding fluid used for grinding resin lenses mainly adopts large-particle boron carbide, silicon carbide or diamond powder as abrasives, and then adds a certain proportion of water and dispersant. The dispersant has poor dispersion effect, is very easy to precipitate, has low grinding efficiency, and has a short cycle life. In addition, during the grinding process, the liquid film on the grinding disc is unevenly dispersed, the grinding lubricity is insufficient, the grinding rate is low, and the particles are easy to agglomerate after grinding, resulting in high scratches and high Ra. Summary of the Invention
[0004] The present application aims to address the shortcomings of current technologies by providing a silicon oxide polishing fluid and a method for preparing the same. The silicon oxide polishing fluid of the present application maintains good suspension of the modified silicon dioxide abrasive under prolonged shearing, resulting in a long cycle life and high grinding efficiency. The polishing fluid of the present application also exhibits excellent dispersing properties, effectively dispersing the nanoparticles produced during the grinding process, preventing the formation of large agglomerated particles and reducing scratches caused by grinding. Therefore, the polishing fluid of the present application exhibits the advantages of shear resistance, high stability of suspension, high dispersion, and high polishing efficiency, and is safe and environmentally friendly, making it widely applicable to polishing various resin lenses.
[0005] In a first aspect, the present application provides a silicon oxide polishing liquid, which adopts the following technical solution: A silicon oxide polishing liquid comprises the following raw materials, calculated by weight: 18-22 parts of modified silicon dioxide, 3-4 parts of a suspension synergist, 0.5-0.7 parts of a pH regulator, 0.2-0.3 parts of a defoamer, 5-8 parts of an organic solvent, and 60-65 parts of deionized water. The suspension synergist is prepared by mixing modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide.
[0006] By adopting the above technical solution, modified silica, as the primary abrasive component of the polishing fluid, maintains excellent suspension properties under shear, ensuring the fluid's cycle life and grinding efficiency. Furthermore, surface modification of the modified silica enables excellent dispersibility in water, helping to improve polishing efficiency and reduce scratching. The suspension enhancer is a mixture of modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide. The modified polyacrylamide electrostatically bonds to the silica, preventing sedimentation and improving the cutting rate. Sodium dodecylbenzenesulfonate provides excellent dispersibility and stability. Modified hexadecyltrimethylammonium bromide, through its positive charge, adsorbs on the surface of the silica particles, improving dispersion and polishing efficiency. The synergistic effect of these three components significantly enhances the polishing fluid's highly stable suspension, high dispersibility, and high polishing efficiency. A pH adjuster adjusts the pH of the polishing fluid to ensure stability and optimal reaction conditions. A defoamer eliminates foam generated during the polishing process, preventing it from affecting the polishing effect. Organic solvents: Lubricate and moisturize, extending the life of the abrasive, reducing scratches, and improving polishing efficiency. Deionized water: As the primary solvent in the polishing fluid, it provides the necessary medium environment for the various components to fully mix and function. Through the synergistic effect of these components, the silica polishing fluid of this application achieves shear resistance, highly stable suspension, high dispersibility, and high polishing efficiency, while ensuring safety and environmental protection requirements. This polishing fluid is particularly suitable for polishing various resin lenses.
[0007] Preferably, the mass ratio of the modified polyacrylamide, sodium dodecylbenzenesulfonate and modified hexadecyltrimethylammonium bromide is 3:3:4.
[0008] By adopting the above technical solution, the modified polyacrylamide exhibits excellent suspension and dispersibility, effectively preventing silica particles from settling in the polishing solution and maintaining its stability. Furthermore, the electrostatic interaction between the modified polyacrylamide and the silica particles helps form larger agglomerates, further enhancing suspension stability. Sodium dodecylbenzenesulfonate exhibits excellent wettability and dispersibility, improving the dispersion of silica particles in the polishing solution and reducing interparticle agglomeration. Furthermore, its long-chain structure contributes to the stability and high-temperature resistance of the polishing solution. Modified hexadecyltrimethylammonium bromide, through its positive charge, adsorbs on the surface of silica particles, partially neutralizing the negative charge and reducing interparticle repulsion, thereby improving the dispersion of silica in the polishing solution. Furthermore, the introduction of polytriethanolamine and N,N-dimethylferrocenylmethylamine increases the electronegativity of the silica surface, strengthening chemical bonds and further improving the polishing efficiency of the polishing solution. A synergistic effect exists among the modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide. Modified polyacrylamide provides suspension stability and dispersibility, sodium dodecylbenzenesulfonate provides wettability and dispersibility, and modified hexadecyltrimethylammonium bromide improves polishing efficiency through its charge neutralization and increased chemical bonding strength. This synergistic effect gives the polishing fluid the characteristics of highly stable suspension, high dispersibility, and high polishing efficiency. In summary, the suspension enhancer significantly improves the performance of the silica polishing fluid through the specific effects and synergistic effects of its components, enabling it to maintain excellent suspension stability under prolonged shear, while also improving polishing efficiency and dispersibility and reducing scratches during the grinding process, thereby ensuring the high performance and wide applicability of the polishing fluid.
[0009] Preferably, the preparation method of the modified silicon dioxide comprises the following steps: S31. Mix 1 part corn starch, 20 parts silicon dioxide, 3 parts sodium pyrophosphate, and 150 parts deionized water, by weight, heat to 80-85° C., stir for 30-40 minutes, dry at 105-110° C. for 6-8 hours, and then heat at 800-850° C. for 5-6 hours to obtain a reaction product A. S32. Mix 20 parts of reaction product A, 10 parts of lactide, and 0.1 parts of dibutyltin diacetate by mass, evacuate for 3-4 hours, introduce nitrogen, seal, heat to 120-125°C, stir, add 20 parts of chloroform, precipitate, filter, and dry to obtain reaction product B. S33. Mix 20 parts of reaction product B, 7 parts of polyaniline, 4 parts of salicylic acid and 50 parts of deionized water by mass, ultrasonicate for 3-4 hours, add 10 parts of anhydrous ethanol and 5% dilute sulfuric acid to a pH of 5.5-6.0, stir for 30-40 minutes, centrifuge and dry to obtain modified silica.
[0010] By adopting the above technical solution, the modified silica is prepared by gelatinizing corn starch under heating and the action of sodium pyrophosphate and then surface treating the silica. The crystalline structure of the corn starch is destroyed during the gelatinization process, which is conducive to the reaction between the corn starch and the silica, thereby enhancing the strength of the silica. The silica modified by the gelatinized starch is further carbonized to weaken the interaction between the silica particles, which is conducive to improving the dispersibility of the silica in the polishing liquid. On the one hand, the lactide and the silica modified by the carbonized starch are reacted under the catalysis of dibutyltin diacetate to introduce the long straight chain in the polylactic acid, so that crosslinking points are generated between the silica modified by the carbonized starch and the polylactic acid, thereby increasing the strength of the silica. The internal binding force of the modified silica is conducive to improving the strength of the modified silica. On the other hand, by introducing polyaniline having a benzene ring and an amino group to synthesize the modified silica, the modified silica has the characteristics of high strength and good wettability, which is conducive to the dispersion of the modified silica in the polishing liquid. Furthermore, hydrogen bonding occurs between the polyaniline and the polylactic acid, which is conducive to enhancing the stability and strength of the modified silica, thereby promoting the improvement of the polishing efficiency of the silica polishing liquid. Preferably, the silica is prepared by mixing nano-scale silica and micro-scale silica in a mass ratio of 2:5, the particle size of the nano-scale silica is 10-20 nanometers, and the particle size of the micro-scale silica is 1-2 microns.
[0011] By adopting the above technical solution, a combination of nano- and micro-sized silica can improve grinding efficiency while also reducing and controlling the degree of mirror scratching. The combination of nano- and micro-sized silica provides a wider particle size distribution. Nano-sized silica has a higher specific surface area and activity, while micro-sized silica provides sufficient mechanical strength and grinding ability. This diverse particle size distribution helps improve the grinding efficiency and polishing quality of the polishing slurry. The high specific surface area of nano-sized silica enables higher localized grinding forces and a higher polishing rate during polishing. Meanwhile, the large micro-sized silica particles provide sufficient mechanical abrasive action, resulting in rapid material removal during polishing. Due to the high activity of nano-sized silica, it effectively disperses the fine particles generated during grinding, preventing them from agglomerating into larger particles and thus reducing the risk of scratching. Furthermore, the large micro-sized silica particles provide a stable grinding action during polishing, reducing instability. The combination of nano- and micro-sized silica improves the stability of the polishing slurry. The high activity of nano-silica helps maintain a uniform dispersion in the polishing slurry, while micro-silica provides sufficient mechanical strength to resist shear forces and prevent sedimentation or stratification of the polishing slurry. The synergistic effect of nano-silica and micro-silica can further enhance the performance of the polishing slurry. The high activity of nano-silica enhances the grinding effect of micro-silica, while the large particles of micro-silica protect the nano-silica from premature wear or damage. This synergistic effect helps achieve higher polishing efficiency and better polishing quality. In summary, the combination of nano-silica and micro-silica in silica polishing slurries plays multiple roles, including optimizing particle size distribution, improving polishing efficiency, reducing the risk of scratching, enhancing polishing slurry stability, and achieving synergistic effects.
[0012] Preferably, the preparation method of the modified polyacrylamide comprises the following steps: S51. Add 30 parts of p-aminobenzyl chloride, 68.7 parts of N,N-carbonyldiimidazole, and 32.2 parts of triethylamine to 600 parts of N,N-dimethylformamide solution in order by mass, raise the temperature to 110°C, and react for 5-6 hours to generate intermediate A. After the reaction is completed, naturally cool to room temperature, add 600 parts of water and 1200 parts of ethyl acetate to the reaction solution for extraction, perform aqueous back extraction once, combine the organic phases, dry, and concentrate under reduced pressure to obtain intermediate A; S52. Dissolve 20 parts of polyacrylamide in 200 parts of deionized water, add 25 parts of intermediate A and 24 parts of N,N-diisopropylethylamine, raise the temperature to 85°C, and react for 8-9 hours. After the reaction is completed, cool naturally to room temperature, filter out insoluble matter, and concentrate the filtrate under reduced pressure to obtain intermediate B; S53. According to the mass ratio, 20 parts of intermediate B and 26 parts of octadecyldimethyl tertiary amine were added to 30 parts of ethanol for quaternization reaction. The reaction was refluxed at 85°C for 10-12 hours. After the reaction was completed, it was naturally cooled to room temperature. The reaction solution was concentrated to remove most of the ethanol, and 300 parts of water and 300 parts of ethyl acetate were added thereto for extraction. The organic phases were reversed and the aqueous phases were combined. After drying, the modified polyacrylamide was obtained.
[0013] By adopting the above technical solution, the modified polyacrylamide prepared has a molecular structure containing amide, benzene ring, urea group and long-chain quaternary ammonium salt group, and has good suspension, dispersibility and stability. It is positively charged in aqueous solution and can attract negatively charged silica through electrostatic interaction to form larger agglomerates. On the one hand, it prevents the silica from settling for a long time. On the other hand, the agglomerates of the two can be used as pseudo-abrasives, which not only reduces the amount of abrasives used, but also improves the cutting rate and removal rate.
[0014] Preferably, the preparation method of the modified hexadecyltrimethylammonium bromide comprises the following steps: S61. Add 80 parts by mass of triethanolamine and 1 part of sodium hydroxide to a reaction vessel, heat to 250-255° C., stir for 2.5-3 hours, cool to 90-100° C., add 10 parts by mass of 15% glacial acetic acid solution, cool to room temperature, rotary evaporate, and freeze-dry to obtain product A; S62. According to the mass parts, 10 parts of product A, 15 parts of hexadecyltrimethylammonium bromide, 10 parts of N,N-dimethylferrocenylmethylamine, 5 parts of epichlorohydrin, 20 parts of anhydrous ethanol and 100 parts of deionized water are introduced with nitrogen, stirred at 60-70°C for 50-60 minutes, recrystallized with acetone 4 times, and dried in vacuum at room temperature for 16 hours to obtain modified hexadecyltrimethylammonium bromide.
[0015] By adopting the above technical solution, hexadecyltrimethylammonium bromide is modified with polytriethanolamine and N,N-dimethylferrocenylmethylamine, so that the polishing efficiency of the polishing liquid can be effectively improved. On the one hand, the modified hexadecyltrimethylammonium bromide has a positive charge and can be adsorbed on the surface of the silicon dioxide particles to neutralize part of the negative charge, thereby reducing the repulsion between the silicon dioxide particles, thereby improving the dispersibility of the silicon dioxide in the polishing liquid. In addition, the long-chain saturated alkyl group in the hexadecyltrimethylammonium bromide is conducive to improving the stability and high temperature resistance of the polishing liquid. On the other hand, polytriethanolamine has a large number of hydrophilic groups, such as hydroxyl groups and amino groups, which makes the modified Hexadecyltrimethylammonium bromide has good wettability, which is beneficial to improving the dispersibility of silica particles in the polishing liquid. On the other hand, the introduction of N,N-dimethylferrocenylmethylamine increases the electronegativity of the silica surface, which is beneficial to increasing the binding force of the chemical bond between N,N-dimethylferrocenylmethylamine and silica, thereby improving the stability of the modified hexadecyltrimethylammonium bromide. In addition, the redox reaction between N,N-dimethylferrocenylmethylamine and hexadecyltrimethylammonium bromide can reversibly control the formation of micelle-like substances in the polishing liquid, which is beneficial to promoting the dispersion of components in the polishing liquid, thereby improving the polishing efficiency of the polishing liquid.
[0016] Preferably, the pH adjuster is one of citric acid and malic acid.
[0017] Preferably, the organic solvent is one of ethylene glycol and glycerol.
[0018] Preferably, the defoaming agent is silicone 1522.
[0019] In a second aspect, the present application provides a method for preparing a silicon oxide polishing liquid, which adopts the following technical solution: As a general technical concept, the present application also provides a method for preparing the above-mentioned silicon oxide polishing liquid, comprising the following steps: S101, adding deionized water, organic solvent, modified silica and suspension enhancer to a stirred tank in order according to their mass fractions, stirring at high speed to form a suspension; S102. Add a pH regulator and a defoaming agent to the suspension according to their mass fractions, stir thoroughly, and then age at room temperature for 30-40 minutes. Restart stirring until the system is dispersed and stabilized to obtain a silicon oxide polishing liquid.
[0020] In summary, the beneficial technical effects of this application are: 1. Highly stable suspension: Through the use of a specific suspension enhancer formula and modified silica, the abrasive in the polishing liquid can maintain a good suspension state even under long-term shearing action, avoiding the sedimentation and agglomeration of the abrasive.
[0021] 2. Excellent dispersing effect: The polishing fluid can effectively disperse the nanoparticles produced during the grinding process, preventing the particles from agglomerating into large particles, thereby reducing scratches caused by grinding.
[0022] 3. High polishing efficiency: By optimizing the ratio of abrasive and suspension enhancer, the polishing efficiency of the polishing fluid has been significantly improved. At the same time, the synergistic effect of modified polyacrylamide and modified hexadecyltrimethylammonium bromide further improves polishing efficiency.
[0023] 4. Safety and environmental protection: The polishing liquid of the present application does not contain harmful substances during the preparation and use process, is environmentally friendly, and is harmless to the human body, meeting the requirements of green environmental protection.
[0024] 5. Improve rheology: The use of organic solvents improves the rheology of the polishing fluid, making the polishing process smoother and reducing scratches caused by drying or agglomeration of abrasives.
[0025] 6. Improve grinding efficiency and mirror surface quality: The compound use of nano-scale and micron-scale silica not only improves the grinding efficiency, but also improves the scratch degree of the mirror surface, ensuring the quality of the mirror surface after polishing.
[0026] 7. Enhanced stability: The use of modified silica enhances the stability of the polishing liquid, allowing it to maintain good performance even after long-term use.
[0027] 8. Improved wettability and strength: The unique treatment of modified silica gives it high strength and good wettability, further improving its dispersibility and stability in the polishing liquid. DETAILED DESCRIPTION
[0028] The embodiments of the present application will be described in detail below with reference to the examples, but it will be understood by those skilled in the art that the following examples are merely illustrative of the present application and should not be considered as limiting the scope of the present application. In the examples, if specific conditions are not specified, the conditions are carried out according to conventional conditions or manufacturer recommendations. The reagents or instruments used are not specified by the manufacturer and are conventional products that can be purchased commercially.
[0029] In the following examples and preparation examples, 1 part means 100 g.
[0030] Preparation Example 1 Preparation of modified silica The preparation method of modified silicon dioxide comprises the following steps: S31. Mix 1 part corn starch, 20 parts silicon dioxide, 3 parts sodium pyrophosphate, and 150 parts deionized water, by mass, heat to 83° C., stir for 35 min, dry at 108° C. for 7 h, and then heat at 830° C. for 6 h to obtain a reaction product A; wherein the silicon dioxide is prepared by mixing nano-sized silicon dioxide and micro-sized silicon dioxide in a mass ratio of 2:5, the particle size of the nano-sized silicon dioxide is 10-20 nm, and the particle size of the micro-sized silicon dioxide is 1-2 μm; S32. Mix 20 parts of reaction product A, 10 parts of lactide, and 0.1 parts of dibutyltin diacetate by mass, evacuate for 3.4 hours, introduce nitrogen, seal, heat to 123°C, stir, add 20 parts of chloroform, precipitate, filter, and dry to obtain reaction product B. S33. Mix 20 parts of reaction product B, 7 parts of polyaniline, 4 parts of salicylic acid and 50 parts of deionized water in parts by mass, ultrasonicate for 3.4 hours, add 10 parts of anhydrous ethanol and 5% dilute sulfuric acid to a pH of 5.7, stir for 35 minutes, centrifuge and dry to obtain modified silica.
[0031] Preparation Example 2 Preparation of modified polyacrylamide The preparation method of modified polyacrylamide comprises the following steps: S51. Add 30 parts of p-aminobenzyl chloride, 68.7 parts of N,N-carbonyldiimidazole, and 32.2 parts of triethylamine to 600 parts of N,N-dimethylformamide solution in order by mass, raise the temperature to 110°C, and react for 5 hours to generate intermediate A. After the reaction is completed, naturally cool to room temperature, add 600 parts of water and 1200 parts of ethyl acetate to the reaction solution for extraction, perform aqueous back extraction once, combine the organic phases, dry, and concentrate under reduced pressure to obtain intermediate A; S52. Dissolve 20 parts of polyacrylamide in 200 parts of deionized water, add 25 parts of intermediate A and 24 parts of N,N-diisopropylethylamine, raise the temperature to 85°C, and react for 9 hours. After the reaction is completed, cool naturally to room temperature, filter out insoluble matter, and concentrate the filtrate under reduced pressure to obtain intermediate B; S53. According to the mass ratio, 20 parts of intermediate B and 26 parts of octadecyldimethyl tertiary amine were added to 30 parts of ethanol to carry out quaternization reaction. The reaction was refluxed at 85°C for 11 hours. After the reaction was completed, it was naturally cooled to room temperature. The reaction solution was concentrated to remove most of the ethanol, and 300 parts of water and 300 parts of ethyl acetate were added thereto for extraction. The organic phases were reversed and extracted once. The aqueous phases were combined, dried, and concentrated under reduced pressure to obtain modified polyacrylamide.
[0032] Preparation Example 3 Preparation of modified hexadecyltrimethylammonium bromide The preparation method of modified hexadecyltrimethylammonium bromide comprises the following steps: S61. Add 80 parts by mass of triethanolamine and 1 part of sodium hydroxide to a reaction vessel, heat to 253° C., stir for 2.7 hours, cool to 95° C., add 10 parts by mass of 15% glacial acetic acid solution, cool to room temperature, rotary evaporate, and freeze-dry to obtain product A; S62. According to the mass parts, 10 parts of product A, 15 parts of hexadecyltrimethylammonium bromide, 10 parts of N,N-dimethylferrocenylmethylamine, 5 parts of epichlorohydrin, 20 parts of anhydrous ethanol and 100 parts of deionized water are introduced with nitrogen, stirred at 65°C for 55 minutes, recrystallized with acetone 4 times, and dried in vacuum at room temperature for 16 hours to obtain modified hexadecyltrimethylammonium bromide.
[0033] Preparation of Comparative Example 1 Preparation of Modified Silica A The method is the same as Preparation Example 1, except that the silicon dioxide is nano-scale silicon dioxide with a particle size of 10-20 nanometers.
[0034] Preparation of Comparative Example 2: Preparation of Modified Silica B The same as Preparation Example 1, except that the silicon dioxide has a particle size of 1-2 microns.
[0035] Example 1 A silicon oxide polishing liquid, comprising the following raw materials, calculated by weight: 18 parts of modified silicon dioxide, 3 parts of a suspension synergist, 0.5 parts of citric acid, 0.2 parts of organosilicon 1522, 5 parts of glycerol, and 60 parts of deionized water, wherein the suspension synergist is prepared by mixing modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide in a weight ratio of 3:3:4. The preparation method of the above-mentioned silicon oxide polishing liquid comprises the following steps: S101, adding deionized water, glycerol, modified silica and suspension enhancer to a stirred tank in order according to their mass fractions, stirring at high speed to form a suspension; S102. Add citric acid and organosilicon 1522 to the suspension according to their mass fractions, stir thoroughly, and then age at room temperature for 30 minutes. Restart stirring until the system is dispersed and stabilized to obtain a silicon oxide polishing liquid.
[0036] Example 2 A silicon oxide polishing liquid, comprising the following raw materials, calculated by weight: 22 parts of modified silicon dioxide, 4 parts of a suspension synergist, 0.7 parts of citric acid, 0.3 parts of organosilicon 1522, 8 parts of glycerol, and 65 parts of deionized water, wherein the suspension synergist is prepared by mixing modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide in a weight ratio of 3:3:4. The preparation method of the above-mentioned silicon oxide polishing liquid comprises the following steps: S101, adding deionized water, glycerol, modified silica and suspension enhancer to a stirred tank in order according to their mass fractions, stirring at high speed to form a suspension; S102. Add citric acid and organosilicon 1522 to the suspension according to their mass fractions, stir thoroughly, and then age at room temperature for 40 minutes. Restart stirring until the system is dispersed and stabilized to obtain a silicon oxide polishing liquid.
[0037] Example 3 A silicon oxide polishing liquid, comprising the following raw materials, calculated by weight: 20 parts of modified silicon dioxide, 3.5 parts of a suspension synergist, 0.6 parts of citric acid, 0.25 parts of organosilicon 1522, 7 parts of glycerol, and 63 parts of deionized water, wherein the suspension synergist is prepared by mixing modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide in a weight ratio of 3:3:4. The preparation method of the above-mentioned silicon oxide polishing liquid comprises the following steps: S101, adding deionized water, glycerol, modified silica and suspension enhancer to a stirred tank in order according to their mass fractions, stirring at high speed to form a suspension; S102. Add citric acid and organosilicon 1522 to the suspension according to their mass fractions, stir thoroughly, and then age at room temperature for 35 minutes. Restart stirring until the system is dispersed and stabilized to obtain a silicon oxide polishing liquid.
[0038] Comparative Example 1 The same as Example 3, except that an equal amount of silica (prepared by mixing nano-scale silica and micron-scale silica in a mass ratio of 2:5, the particle size of the nano-scale silica is 10-20 nm, and the particle size of the micron-scale silica is 1-2 μm) is used instead of the modified silica.
[0039] Comparative Example 2 The same as Example 3, except that an equal amount of modified silica A prepared in Comparative Preparation Example 1 is used instead of modified silica.
[0040] Comparative Example 3 The same as Example 3, except that an equal amount of modified silica B prepared in Comparative Preparation Example 2 is used instead of modified silica.
[0041] Comparative Example 4 The same as Example 3, except that the suspension enhancer is modified polyacrylamide.
[0042] Comparative Example 5 The same as Example 3, except that the suspension synergist is sodium dodecylbenzenesulfonate.
[0043] Comparative Example 6 The same as Example 3, except that the suspension synergist is modified hexadecyltrimethylammonium bromide.
[0044] Performance Testing The silicon oxide polishing liquids prepared in Example 1 and Example 3 and Comparative Examples 1 to 6 were sampled and subjected to the following evaluation tests. The test results are shown in Table 1.
[0045] A resin lens was used for grinding tests to test the removal rate, Ra, surface scratches, surface dirt after grinding, and surface dirt after cleaning. The details are as follows: The surface is dirty after grinding: After grinding, take out the resin lens, rinse it with deionized water for 1 minute, blow it dry, and observe the surface under a microscope to see if there are any grinding chips or particles remaining.
[0046] Surface dirt after cleaning: First use 5% concentration cleaning solution for two sections of ultrasonic cleaning at 40℃ for 10 minutes, then use deionized water for ultrasonic cleaning at 40℃. After drying, observe the surface under a microscope to see if there are any grinding chips or other residues.
[0047] Surface scratch test: Detect scratches on the surface of the resin lens. Polish the resin lens according to the following polishing conditions. Use a FUNATECH lighting inspection lamp (model: FY-18L) to inspect the surface quality of the resin lens by manual inspection. Record the number of scratches on the surface of the resin lens (unit: scratches). Suspension after continuous stirring for 24 hours: Take 200g of deionized water, add 50g of silicon oxide polishing liquid, stir at 500r / min for 24 hours, pour into a test tube, let it stand for 1 hour to observe the suspension of modified boron nitride.
[0048] The specific grinding experimental equipment and conditions are as follows: Grinding equipment: Chuangji double-sided grinding machine; Resin lens size: 2 inches; Number of test pieces: 900 pieces; divided into 9 groups (corresponding to Examples 1 to 3 and Comparative Examples 1 to 6), with 100 pieces in each group.
[0049] Speed: 20r / min; Pressure: 4.0kpa; Plate temperature: 20-30℃; Grinding time: 10min.
[0050] Table 1 Performance test Analyzing the data in Table 1, we can see that: The silica polishing fluids prepared in Examples 1-3 maintain good suspension of the modified silica abrasives under prolonged shear, resulting in a long cycle life and high grinding efficiency. The polishing fluids of this application exhibit excellent dispersibility, effectively dispersing the nanoparticles produced during the grinding process, preventing the formation of large agglomerated particles and reducing scratches caused by grinding. The polishing fluids of this application exhibit shear resistance, stable suspension, high dispersion, and high polishing efficiency, and are safe and environmentally friendly, making them widely applicable to polishing various resin lenses.
[0051] 2) A comparative analysis of the performance of the silica polishing solutions prepared in Example 3 and Comparative Example 1 shows that the addition of the modified silica prepared in this application not only increases the strength of silica in the polishing solution, but also further improves its dispersibility, stability, and polishing efficiency of the polishing solution, thereby improving the surface quality of the resin lens.
[0052] 3) The comparative analysis of the performance of the silicon oxide polishing liquids prepared in Example 3 and Comparative Examples 2-3 shows that the use of a compound of nano-scale silicon dioxide and micro-scale silicon dioxide can improve the grinding efficiency and improve and control the degree of mirror scratches.
[0053] 4) A comparative analysis of the performance of the silicon oxide polishing liquid prepared in combination with Example 3 and Comparative Examples 4-6 shows that the suspension synergist is prepared by mixing modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide in a mass ratio of 3:3:4. The modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide have a synergistic effect. The modified polyacrylamide provides suspension stability and dispersibility, the sodium dodecylbenzenesulfonate provides wettability and dispersibility, and the modified hexadecyltrimethylammonium bromide improves the polishing efficiency by its charge neutralization and increased chemical bond strength. This synergistic effect gives the polishing liquid the characteristics of high stable suspension, high dispersibility, and high polishing efficiency, significantly improving the performance of the silicon oxide polishing liquid, allowing it to maintain good suspension stability under long-term shearing, while improving the polishing efficiency and dispersibility, reducing scratches during the grinding process, thereby ensuring the high performance and wide applicability of the polishing liquid.
[0054] The above embodiments are only used to illustrate the technical solutions of the present application and are not intended to limit the present application. Although the above embodiments provide a detailed description of the present application, relevant technical personnel should understand that the specific implementation methods of the present invention can still be modified or replaced by equivalents. Any modifications and equivalent replacements that do not depart from the spirit and scope of the present application should be included in the scope of protection of the present application.
Claims
1. A silicon oxide polishing liquid, characterized in that The preparation method comprises the following raw materials, calculated by weight: 18-22 parts of modified silicon dioxide, 3-4 parts of suspension enhancer, 0.5-0.7 parts of pH regulator, 0.2-0.3 parts of defoamer, 5-8 parts of organic solvent, and 60-65 parts of deionized water. The suspension enhancer is prepared by mixing modified polyacrylamide, sodium dodecylbenzenesulfonate, and modified hexadecyltrimethylammonium bromide.
2. A silicon oxide polishing liquid according to claim 1, characterized in that: The mass ratio of the modified polyacrylamide, sodium dodecylbenzenesulfonate and modified hexadecyltrimethylammonium bromide is 3:3:
4.
3. A silicon oxide polishing liquid according to claim 1, characterized in that: The preparation method of the modified silicon dioxide comprises the following steps: S31. Mix 1 part corn starch, 20 parts silicon dioxide, 3 parts sodium pyrophosphate, and 150 parts deionized water, by weight, heat to 80-85° C., stir for 30-40 minutes, dry at 105-110° C. for 6-8 hours, and then heat at 800-850° C. for 5-6 hours to obtain a reaction product A. S32. Mix 20 parts of reaction product A, 10 parts of lactide, and 0.1 parts of dibutyltin diacetate by mass, evacuate for 3-4 hours, introduce nitrogen, seal, heat to 120-125°C, stir, add 20 parts of chloroform, precipitate, filter, and dry to obtain reaction product B. S33. Mix 20 parts of reaction product B, 7 parts of polyaniline, 4 parts of salicylic acid and 50 parts of deionized water by mass, ultrasonicate for 3-4 hours, add 10 parts of anhydrous ethanol and 5% dilute sulfuric acid dropwise to a pH of 5.5-6.0, stir for 30-40 minutes, centrifuge and dry to obtain modified silica.
4. A silicon oxide polishing liquid according to claim 3, characterized in that: The silicon dioxide is prepared by mixing nano-sized silicon dioxide and micro-sized silicon dioxide in a mass ratio of 2:
5. The particle size of the nano-sized silicon dioxide is 10-20 nanometers, and the particle size of the micro-sized silicon dioxide is 1-2 micrometers.
5. A silicon oxide polishing liquid according to claim 1, characterized in that: The preparation method of the modified polyacrylamide comprises the following steps: S51. Add 30 parts of p-aminobenzyl chloride, 68.7 parts of N,N-carbonyldiimidazole, and 32.2 parts of triethylamine to 600 parts of N,N-dimethylformamide solution in order by mass, raise the temperature to 110° C., and react for 5-6 hours to generate intermediate A. After the reaction is completed, naturally cool to room temperature, add 600 parts of water and 1200 parts of ethyl acetate to the reaction solution for extraction, perform aqueous back extraction once, combine the organic phases, dry, and concentrate under reduced pressure to obtain intermediate A; S52. Dissolve 20 parts of polyacrylamide in 200 parts of deionized water, add 25 parts of intermediate A and 24 parts of N,N-diisopropylethylamine, raise the temperature to 85°C, and react for 8-9 hours. After the reaction is completed, cool naturally to room temperature, filter out insoluble matter, and concentrate the filtrate under reduced pressure to obtain intermediate B; S53. According to the mass ratio, 20 parts of intermediate B and 26 parts of octadecyldimethyl tertiary amine were added to 30 parts of ethanol for quaternization reaction. The reaction was refluxed at 85°C for 10-12 hours. After the reaction was completed, it was naturally cooled to room temperature. The reaction solution was concentrated to remove most of the ethanol, and 300 parts of water and 300 parts of ethyl acetate were added thereto for extraction. The organic phases were reversed and the aqueous phases were combined. After drying, the modified polyacrylamide was obtained.
6. A silicon oxide polishing liquid according to claim 1, characterized in that: The preparation method of the modified hexadecyltrimethylammonium bromide comprises the following steps: S61. Add 80 parts by mass of triethanolamine and 1 part of sodium hydroxide to a reaction vessel, heat to 250-255° C., stir for 2.5-3 hours, cool to 90-100° C., add 10 parts by mass of 15% glacial acetic acid solution, cool to room temperature, rotary evaporate, and freeze-dry to obtain product A; S62. According to the mass parts, 10 parts of product A, 15 parts of hexadecyltrimethylammonium bromide, 10 parts of N,N-dimethylferrocenylmethylamine, 5 parts of epichlorohydrin, 20 parts of anhydrous ethanol and 100 parts of deionized water are introduced with nitrogen, stirred at 60-70°C for 50-60 minutes, recrystallized with acetone 4 times, and dried in vacuum at room temperature for 16 hours to obtain modified hexadecyltrimethylammonium bromide.
7. A silicon oxide polishing liquid according to claim 1, characterized in that: The pH regulator is one of citric acid and malic acid.
8. A silicon oxide polishing liquid according to claim 1, characterized in that: The organic solvent is one of ethylene glycol and glycerol.
9. A silicon oxide polishing liquid according to claim 1, characterized in that: The defoaming agent is silicone 1522.
10. A method for preparing a silicon oxide polishing liquid according to any one of claims 1 to 9, characterized in that: The following steps are involved: S101, adding deionized water, organic solvent, modified silica and suspension enhancer to a stirred tank in order according to their mass fractions, stirring at high speed to form a suspension; S102. Add a pH regulator and a defoaming agent to the suspension according to their mass fractions, stir thoroughly, and then age at room temperature for 30-40 minutes. Restart stirring until the system is dispersed and stabilized to obtain a silicon oxide polishing liquid.