Environment-friendly water-based diamond grinding fluid as well as preparation process and recovery method thereof

Abstract

The invention discloses environment-friendly water-based diamond grinding fluid as well as a preparation process and a recovery method thereof. The grinding fluid is prepared from the following raw materials in parts by weight: 1 to 10 parts of grinding material, 0.1 to 2 parts of wetting agent, 0.1 to 1 part of thickening agent, 0.1 to 1 part of anti-settling agent, 1 to 10 parts of pH regulator, 0.1 to 2 parts of defoaming agent, 0.1 to 1 part of corrosion inhibitor and 73 to 97.5 parts of water. By means of the innovative formula and preparation method, the higher material removal rate is achieved, the better surface machining quality is achieved, the environmental influence is reduced, and the cost effectiveness is improved. The diamond grinding fluid prepared by the preparation process provided by the invention has the advantages of high grinding efficiency, uniform grinding material dispersion, good suspension effect, no precipitation layering phenomenon after long-time placement, adjustable viscosity as required, reduction of the harm of additives in the grinding fluid to the environment, meeting of the environmental protection requirement, and good application prospects. According to the recovery method provided by the invention, the recovery of the diamond micro-powder in the grinding fluid is simply realized, and the recovery cost is reduced.

Description

Technical Field

[0001] The invention relates to the technical field of precision machining grinding and polishing, and in particular to an environmentally friendly water-based diamond grinding liquid and a preparation process and a recovery method thereof. Background Art

[0002] As a highly efficient abrasive material, diamond slurry plays an important role in the mechanical industry, optical glass, semiconductor manufacturing and various precision machining fields. In the mechanical machining industry, diamond slurry greatly increases the grinding rate compared to traditional slurries. In semiconductor manufacturing, diamond slurry can achieve accurate removal of surface materials. In precision machining fields such as automobiles, electronics, aerospace and other industries, diamond slurry can effectively improve surface quality, reduce surface defects, increase surface hardness, and improve corrosion resistance. In particular, in the surface treatment of hard materials such as sapphire, ceramics and certain metal alloys, due to the high hardness of the material to be ground, diamond slurry becomes an ideal choice due to its high grinding rate and high-quality surface.

[0003] The Chinese patent with the document number CN105440953B discloses a method for preparing an aqueous diamond grinding liquid with continuous suspension of abrasives, which is mainly composed of diamond micropowder, surface modifier, suspending agent, cosolvent, lubricating agent and water, wherein the suspending agent is N-methylpyrrolidone of modified polyurea, the lubricating agent is ethylene glycol or polyethylene glycol, and the surfactant is alkylphenol polyoxyethylene ether. With this technical solution, the prepared diamond grinding liquid can make the abrasives continuously suspended without precipitation and aggregation; however, the surfactant and a high proportion of organic solvents used in the formula are harmful to the environment, the viscosity of the grinding liquid cannot be freely adjusted, and the recycling process is relatively complicated. Summary of the invention

[0004] In view of the deficiencies of the prior art, the present invention provides an environmentally friendly water-based diamond grinding liquid and its preparation process and recycling method. The present invention achieves faster material removal rate and better surface processing quality through innovative formula and preparation method, reduces environmental impact and improves cost-effectiveness; the diamond grinding liquid prepared by the preparation process provided by the present invention has high grinding efficiency, uniform abrasive dispersion, good suspension effect, no precipitation and stratification phenomenon is found after long-term placement, and the viscosity of the grinding liquid can be adjusted according to demand, reducing the harm of additives in the grinding liquid to the environment, meeting environmental protection requirements; at the same time, the present invention also provides a method for recovering micropowder in water-based diamond grinding liquid, and the recovery method provided by the present invention can simply realize the recovery of diamond micropowder in the grinding liquid, reducing the recovery cost.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] In a first aspect of the present invention, an environmentally friendly water-based diamond grinding liquid is provided, comprising the following raw materials in parts by weight: 1-10 parts of abrasive, 0.1-2 parts of wetting agent, 0.1-1 parts of thickener, 0.1-1 parts of anti-settling agent, 1-10 parts of pH regulator, 0.1-2 parts of defoaming agent, 0.1-1 parts of anti-corrosion agent and 73-97.5 parts of water;

[0007] The abrasive is single crystal diamond powder, and the particle size of the single crystal diamond powder is 0.5-20 μm. The particle size of the abrasive is concentrated to prevent the appearance of large particles and avoid scratches caused by large particles during the grinding process;

[0008] The wetting agent is one or more of ethanol, glycerol, and polyethylene glycol;

[0009] The thickener is one or more of acrylic acid monomer polymer, acrylic acid derivative, alkali-soluble anionic thickener, and anionic polymer thickener;

[0010] The anti-settling agent is modified polyurea N-methylpyrrolidone;

[0011] The pH regulator is sodium hydroxide or hydrogen peroxide;

[0012] The defoamer is one of a water-based polyvinyl alcohol defoamer and a polyether siloxane copolymer;

[0013] The anticorrosive agent is one of sodium benzoate, organic amine TPP, and silicated triethanolamine;

[0014] Preferably, the particle size of the single crystal diamond powder is 0.5-20 μm.

[0015] Preferably, the pH value of the diamond grinding liquid is in the range of 7-11.

[0016] Preferably, the water used as the matrix is ​​purified pure water.

[0017] Preferably, an environmentally friendly water-based diamond grinding liquid comprises the following raw materials in parts by weight: 1 part of diamond micropowder with a particle size of 0.5um, 0.1 part of ethanol, 0.1 part of acrylic monomer polymer thickener, 0.1 part of modified polyurea N-methylpyrrolidone, 0.1 part of polyvinyl alcohol defoamer, 0.1 part of organic amine TPP, 1 part of sodium hydroxide and 97.5 parts of pure water.

[0018] Preferably, an environmentally friendly water-based diamond grinding liquid comprises the following raw materials in parts by weight: 1 part of diamond micropowder with a particle size of 20 μm, 0.1 part of ethanol, 0.1 part of acrylic monomer polymer thickener, 0.1 part of modified polyurea N-methylpyrrolidone, 0.1 part of polyvinyl alcohol defoamer, 0.1 part of organic amine TPP, 1 part of sodium hydroxide and 97.5 parts of pure water.

[0019] Preferably, an environmentally friendly water-based diamond polishing liquid comprises the following raw materials in parts by weight: 2 parts of diamond micropowder with a particle size of 3 μm, 1 part of ethanol, 1 part of acrylic monomer polymer thickener, 0.1 parts of modified polyurea N-methylpyrrolidone, 1 part of polyvinyl alcohol defoamer, 1 part of organic amine (TPP), 2 parts of sodium hydroxide and 91.9 parts of pure water.

[0020] Preferably, an environmentally friendly water-based diamond grinding liquid comprises the following raw materials in parts by weight: 1 part of diamond micropowder with a particle size of 1 um, 1 part of ethylene glycol, 1 part of anionic polymer thickener, 0.1 part of modified polyurea N-methylpyrrolidone, 1 part of water-based polyvinyl alcohol defoamer, 1 part of organic amine TPP, 2 parts of pH regulator sodium hydroxide and 92.9 parts of pure water.

[0021] Preferably, an environmentally friendly water-based diamond grinding fluid comprises the following raw materials in parts by weight: 5 parts of diamond micropowder with a particle size of 12um, 1 part of propylene glycol, 1 part of an acrylic derivative thickener, 0.1 parts of a modified polyurea N-methylpyrrolidone anti-settling agent, 1 part of an aqueous polyvinyl alcohol defoamer, 1 part of an anti-corrosion agent organic amine TPP, 2 parts of a pH regulator sodium hydroxide, and 88.9 parts of pure water.

[0022] Preferably, an environmentally friendly water-based diamond grinding liquid comprises the following raw materials in parts by weight:

[0023] 10 parts of diamond micropowder with a diameter of 0.5um, 2 parts of ethanol, 1 part of acrylic monomer polymer thickener, 1 part of modified polyurea N-methylpyrrolidone, 2 parts of polyvinyl alcohol defoamer, 1 part of organic amine TPP, 10 parts of sodium hydroxide and 73 parts of pure water.

[0024] Preferably, an environmentally friendly water-based diamond grinding liquid comprises the following raw materials in parts by weight: 10 parts of diamond micropowder with a diameter of 20 μm, 2 parts of ethanol, 1 part of acrylic monomer polymer thickener, 1 part of modified polyurea N-methylpyrrolidone, 2 parts of polyvinyl alcohol defoamer, 1 part of organic amine TPP, 10 parts of sodium hydroxide and 73 parts of pure water.

[0025] The second aspect of the present invention provides a preparation process based on the above-mentioned water-based diamond grinding liquid, and the preparation process comprises the following steps:

[0026] Step (1): mixing diamond micropowder and water and stirring evenly, adding a dispersant and a wetting agent and stirring evenly, and ultrasonically treating for 5-20 minutes to obtain a surface-modified diamond micropowder solution;

[0027] Step (2): adding the thickener to pure water and stirring with a stirrer for 10-30 minutes to obtain a uniformly dispersed viscous solution;

[0028] Step (3): pouring the uniformly dispersed diamond powder solution obtained in step (1) into the uniformly dispersed viscous solution in step (2), and continuing to stir with a stirrer for 10-30 minutes;

[0029] Step (4): adding an anti-settling agent to the solution obtained in step (3), stirring for 5-10 minutes to obtain a uniformly dispersed aqueous solution 1;

[0030] Step (5): adding a defoamer and an anti-corrosion agent to the uniformly dispersed aqueous solution 1 obtained in step (4), and continuing stirring for 5-10 minutes to obtain a uniformly dispersed aqueous solution 2;

[0031] Step (6): Add a pH regulator to the uniformly dispersed aqueous solution obtained in step (5) to adjust the pH value of the grinding liquid, and continue stirring for 10-30 minutes to obtain a uniformly dispersed diamond grinding liquid.

[0032] A third aspect of the present invention provides a method for recovering micropowder in a water-based diamond grinding liquid, the method specifically comprising the following steps:

[0033] Step (1): adding a treatment agent to the used diamond polishing liquid or expired polishing liquid to agglomerate the diamond powder in the polishing liquid, and leaving it for a period of time until all the agglomerates are precipitated;

[0034] Step (2): pour the upper solution into a wastewater treatment tank, retain the precipitated powder, and wash the precipitated material with clean water 1-2 times;

[0035] Step (3): adding water and hydrogen peroxide solution to the cleaned precipitate and reacting for 1-3 hours to allow the hydrogen peroxide to completely degrade the treatment agent added in step (1), thereby obtaining a micropowder solution without the treatment agent, thereby completing the complete recovery of the diamond micropowder.

[0036] Preferably, the treating agent in step (1) is sodium dodecylbenzene sulfonate, and the amount used is 0.5-5%.

[0037] Preferably, the ratio of water to hydrogen peroxide in the water and hydrogen peroxide solution in step (3) is 10:1-2.

[0038] Preferably, the hydrogen peroxide concentration is 30%.

[0039] Compared with the prior art, the present invention has the following advantages:

[0040] 1. The diamond grinding liquid provided by the present invention meets the environmental protection requirements of modern industry for grinding liquid, has a simple preparation process, and is easy to realize batch production;

[0041] 2. It has stronger and more stable grinding quality. The grinding fluid has moderate viscosity and stable dispersion, which avoids surface scratches during grinding and polishing. The grinding fluid has good suspension effect and will not produce sedimentation and stratification after long-term storage;

[0042] 3. The water-based diamond grinding liquid recovery and treatment method provided by the present invention is simple and environmentally friendly. The treatment agent is used to make the diamond micropowder in the grinding liquid produce agglomeration precipitation, and then the oxidant is used to degrade the treatment agent. The process is simple and will not introduce secondary pollution, thereby realizing the recovery of diamond micropowder, reducing costs, and achieving green and environmentally friendly production;

[0043] 4. The method for recovering micropowder in diamond polishing liquid provided by the present invention is not only applicable to the polishing liquid formula described in the present invention, but also applicable to the recovery of micropowder in various water-based polishing liquids. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 A flow chart of the preparation of a diamond polishing liquid provided in one embodiment of the present invention;

[0045] Figure 2 A microscope picture of the diamond polishing liquid provided in Example 3 of the present invention;

[0046] Figure 3 A microscope picture of the diamond polishing liquid provided in Example 4 of the present invention;

[0047] Figure 4 A recovery flow chart of diamond polishing liquid provided in one embodiment of the present invention;

[0048] Figure 5 This is a particle size distribution diagram of the 3 μm diamond polishing liquid prepared in Example 1 of the present invention;

[0049] Figure 6 This is the appearance of the diamond polishing liquid in Example 1 of the present invention after natural sedimentation for one month;

[0050] Figure 7 This is the appearance of the diamond polishing liquid in Example 1 of the present invention after natural sedimentation for 6 months;

[0051] Figure 8 This is the particle size distribution diagram of the product obtained after being treated by the recovery method of the present invention in Example 3. DETAILED DESCRIPTION

[0052] In order to better understand the technical content of the present invention, specific embodiments are given and illustrated in conjunction with the accompanying drawings. The embodiments of the present invention are not necessarily defined to include all aspects of the present invention. It should be understood that the various concepts and embodiments introduced above, as well as those described in more detail below, can be implemented in any of many ways, because the concepts and embodiments disclosed in the present invention are not limited to any implementation. In addition, some aspects disclosed in the present invention can be used alone or in any appropriate combination with other aspects disclosed in the present invention.

[0053] The present invention will be further described below in conjunction with embodiments:

[0054] Example 1

[0055] The environmentally friendly water-based diamond polishing liquid of this embodiment is made of the following raw materials in parts by weight: 1 part of diamond micropowder with a particle size of 0.5um, 0.1 part of ethanol, 0.1 part of acrylic monomer polymer thickener, 0.1 part of modified polyurea N-methylpyrrolidone, 0.1 part of polyvinyl alcohol defoamer, 0.1 part of organic amine TPP, 1 part of sodium hydroxide and 97.5 parts of pure water.

[0056] The preparation method of the diamond grinding liquid of the present invention comprises the following steps:

[0057] Step (1): add 1 part of diamond powder with a particle size of 0.5 μm to 10 parts of pure water solution and stir evenly, add 0.1 part of ethanol, stir evenly and perform ultrasonic treatment for 10 minutes to obtain a uniformly dispersed diamond powder solution;

[0058] Step (2): adding 0.1 parts of acrylic acid monomer polymer thickener to 80 parts of water, stirring with a stirrer for 30 minutes at a speed of 1500 r / min to evenly disperse the thickener to form an evenly dispersed thickening solution;

[0059] Step (3): keep the agitator in step (2) running, add the solution containing surface-modified diamond powder prepared in step (1) into the thickened solution, keep the speed unchanged, and continue stirring for 5 minutes to obtain a solution with uniform abrasive dispersion;

[0060] Step (4): add 0.1 parts of modified polyurea N-methylpyrrolidone anti-settling agent to the solution obtained in step (3), stir for 5 minutes at a constant stirrer speed to obtain a uniformly dispersed aqueous solution;

[0061] Step (5): adding 0.1 parts of aqueous polyvinyl alcohol defoamer and 0.1 parts of organic amine TPP anticorrosive agent to the uniformly dispersed aqueous solution obtained in step (4), maintaining the stirrer speed unchanged, and continuing stirring for 5 minutes to obtain a uniformly dispersed aqueous solution;

[0062] Step (6): Add 1 part of sodium hydroxide as a pH regulator to the uniformly dispersed aqueous solution obtained in step (5), replenish the pure aqueous solution until the total content of all additives and the aqueous solution is 100 parts, keep the agitator speed unchanged, and continue stirring for 30 minutes to obtain a uniformly dispersed diamond polishing liquid with a pH value of 8.

[0063] Example 2

[0064] The environmentally friendly water-based diamond polishing liquid of this embodiment is made of the following raw materials in parts by weight: 1 part of diamond micropowder with a particle size of 20 μm, 0.1 part of ethanol, 0.1 part of acrylic monomer polymer thickener, 0.1 part of modified polyurea N-methylpyrrolidone, 0.1 part of polyvinyl alcohol defoamer, 0.1 part of organic amine TPP, 1 part of sodium hydroxide and 97.5 parts of pure water.

[0065] The preparation method of the diamond grinding liquid of the present invention comprises the following steps:

[0066] Step (1): add 1 part of diamond powder with a particle size of 20 μm to 10 parts of pure water solution and stir evenly, add 0.1 part of ethanol, stir evenly and perform ultrasonic treatment for 10 minutes to obtain a uniformly dispersed diamond powder solution;

[0067] Step (2): adding 0.1 parts of acrylic acid monomer polymer thickener to 80 parts of water, stirring with a stirrer for 30 minutes at a speed of 1500 r / min to evenly disperse the thickener to form an evenly dispersed thickening solution;

[0068] Step (3): keep the agitator in step (2) running, add the solution containing surface-modified diamond powder prepared in step (1) into the thickened solution, keep the speed unchanged, and continue stirring for 5 minutes to obtain a solution with uniform abrasive dispersion;

[0069] Step (4): add 0.1 parts of modified polyurea N-methylpyrrolidone anti-settling agent to the solution obtained in step (3), stir for 5 minutes at a constant stirrer speed to obtain a uniformly dispersed aqueous solution;

[0070] Step (5): adding 0.1 parts of aqueous polyvinyl alcohol defoamer and 0.1 parts of organic amine TPP anticorrosive agent to the uniformly dispersed aqueous solution obtained in step (4), maintaining the stirrer speed unchanged, and continuing stirring for 5 minutes to obtain a uniformly dispersed aqueous solution;

[0071] Step (6): Add 1 part of sodium hydroxide as a pH regulator to the uniformly dispersed aqueous solution obtained in step (5), replenish the pure aqueous solution until the total content of all additives and the aqueous solution is 100 parts, keep the agitator speed unchanged, and continue stirring for 30 minutes to obtain a uniformly dispersed diamond polishing liquid with a pH value of 8.

[0072] Example 3

[0073] The environmentally friendly water-based diamond polishing liquid of this embodiment is made of the following raw materials in parts by weight: 2 parts of diamond micropowder with a particle size of 3um, 1 part of ethanol, 1 part of acrylic monomer polymer thickener, 0.1 parts of modified polyurea N-methylpyrrolidone, 1 part of polyvinyl alcohol defoamer, 1 part of organic amine TPP, 2 parts of sodium hydroxide and 91.9 parts of pure water.

[0074] The preparation method of the diamond grinding liquid of the present invention is as follows Figure 3 As shown, the following steps are included:

[0075] Step (1): Add 2 parts of diamond micropowder with a particle size of 3 μm to 10 parts of pure water solution and stir evenly, add 1 part of ethanol, stir evenly and perform ultrasonic treatment for 10 minutes to obtain a solution containing evenly dispersed diamond micropowder.

[0076] Step (2): Add 1 part of acrylic acid monomer polymer thickener to 80 parts of water, and stir with a stirrer for 30 minutes at a speed of 1000 r / min to evenly disperse the thickener to form an evenly dispersed thickening solution.

[0077] Step (3): keep the agitator in step (2) running, add the solution containing surface-modified diamond powder prepared in step (1) into the thickened solution, keep the speed unchanged, and continue stirring for 10 minutes to obtain a solution with uniform abrasive dispersion;

[0078] Step (4): add 0.1 parts of modified polyurea N-methylpyrrolidone anti-settling agent to the solution obtained in step (3), stir for 5 minutes at a constant stirrer speed to obtain a uniformly dispersed aqueous solution;

[0079] Step (5): adding 1 part of a defoaming agent, aqueous polyvinyl alcohol defoaming agent, and 1 part of an organic amine TPP anticorrosive agent to the uniformly dispersed aqueous solution obtained in step (4), maintaining the stirrer speed unchanged, and continuing stirring for 5 minutes to obtain a uniformly dispersed aqueous solution;

[0080] Step (6): Add 2 parts of sodium hydroxide as a pH regulator to the uniformly dispersed aqueous solution obtained in step (5), replenish the pure aqueous solution until the total content of all additives and the aqueous solution is 91.9 parts, keep the agitator speed unchanged, and continue stirring for 30 minutes to obtain a uniformly dispersed diamond polishing liquid with a pH value of 9.

[0081] Example 4

[0082] The environmentally friendly water-based diamond polishing liquid of the embodiment is made of the following raw materials in parts by weight: 1 part of diamond micropowder with a particle size of 1 um, 1 part of ethylene glycol, 1 part of anionic polymer thickener, 0.1 part of modified polyurea N-methylpyrrolidone, 1 part of aqueous polyvinyl alcohol defoamer, 1 part of organic amine TPP, 2 parts of pH regulator sodium hydroxide and 92.9 parts of pure water.

[0083] The preparation method of the diamond grinding liquid of the present invention comprises the following steps:

[0084] Step (1): add 1 part of diamond micropowder with a particle size of 1 μm to 10 parts of pure water solution and stir evenly, add 1 part of polyethylene glycol, stir evenly and perform ultrasonic treatment for 10 minutes to obtain a uniformly dispersed diamond micropowder solution;

[0085] Step (2): adding 1 part of anionic polymer thickener to 80 parts of water, stirring with a stirrer for 30 minutes at a speed of 1500 r / min to evenly disperse the thickener to form an evenly dispersed thickening solution;

[0086] Step (3): keep the agitator in step (2) running, add the solution containing surface-modified diamond powder prepared in step (1) into the thickened solution, keep the speed unchanged, and continue stirring for 5 minutes to obtain a solution with uniform abrasive dispersion;

[0087] Step (4): add 0.1 parts of modified polyurea N-methylpyrrolidone anti-settling agent to the solution obtained in step (3), stir for 5 minutes at a constant stirrer speed to obtain a uniformly dispersed aqueous solution;

[0088] Step (5): adding 1 part of aqueous polyvinyl alcohol defoamer and 1 part of organic amine TPP anticorrosive agent to the uniformly dispersed aqueous solution obtained in step (4), maintaining the stirrer speed unchanged, and continuing stirring for 5 minutes to obtain a uniformly dispersed aqueous solution;

[0089] Step (6): Add 2 parts of sodium hydroxide as a pH regulator to the uniformly dispersed aqueous solution obtained in step (5), replenish the pure aqueous solution until the total content of all additives and the aqueous solution is 100 parts, keep the agitator speed unchanged, and continue stirring for 30 minutes to obtain a uniformly dispersed diamond polishing liquid with a pH value of 9.

[0090] Example 5

[0091] The environmentally friendly water-based diamond polishing liquid of the embodiment is made of the following raw materials in parts by weight: 5 parts of diamond micropowder with a particle size of 12 μm, 1 part of propylene glycol, 1 part of an acrylic derivative thickener, 0.1 parts of a modified polyurea N-methylpyrrolidone anti-settling agent, 1 part of an aqueous polyvinyl alcohol defoamer, 1 part of an organic amine TPP anti-corrosion agent, 2 parts of a pH regulator sodium hydroxide, and 88.9 parts of pure water.

[0092] The preparation method of the diamond grinding liquid of the present invention comprises the following steps:

[0093] Step (1): adding 5 parts of diamond micropowder with a particle size of 12 μm to 10 parts of pure water solution, adding 1 part of propylene glycol, and ultrasonically treating for 5 minutes to obtain a uniformly dispersed diamond micropowder solution;

[0094] Step (2): adding 1 part of acrylic acid derivative thickener to 70 parts of water, stirring with a stirrer for 30 minutes at a speed of 800 r / min to evenly disperse the thickener to form an evenly dispersed thickening solution;

[0095] Step (3): Keep the stirrer in the second step running, add the evenly dispersed diamond micro-solution prepared in the first step into the thickened solution, keep the speed unchanged, and continue stirring for 5 minutes to obtain a solution with evenly dispersed abrasives;

[0096] Step (4): add 0.1 parts of modified polyurea N-methylpyrrolidone anti-settling agent to the solution obtained in step (3), stir for 5 minutes at a constant stirrer speed to obtain a uniformly dispersed aqueous solution;

[0097] Step (5): adding 1 part of a defoaming agent, aqueous polyvinyl alcohol defoaming agent, and 1 part of an organic amine TPP anticorrosive agent to the uniformly dispersed aqueous solution obtained in step (4), maintaining the stirrer speed unchanged, and continuing stirring for 5 minutes to obtain a uniformly dispersed aqueous solution;

[0098] Step (6): Add 2 parts of sodium hydroxide as a pH regulator to the uniformly dispersed aqueous solution obtained in step (5), replenish the pure aqueous solution until the total content of all additives and the aqueous solution is 100 parts, keep the agitator speed unchanged, and continue stirring for 30 minutes to obtain a uniformly dispersed diamond polishing liquid with a pH value of 9.

[0099] Example 6

[0100] Preferably, an environmentally friendly water-based diamond grinding liquid comprises the following raw materials in parts by weight: 10 parts of diamond micropowder with a particle size of 20 μm, 2 parts of propylene glycol, 1 part of acrylic monomer polymer thickener, 1 part of modified polyurea N-methylpyrrolidone, 2 parts of polyvinyl alcohol defoamer, 1 part of organic amine TPP, 10 parts of sodium hydroxide and 73 parts of pure water.

[0101] The preparation method of the diamond grinding liquid of the present invention comprises the following steps:

[0102] Step (1): adding 5 parts of diamond micropowder with a particle size of 20 μm to 10 parts of pure water solution, adding 2 parts of propylene glycol, and ultrasonically treating for 5 minutes to obtain a uniformly dispersed diamond micropowder solution;

[0103] Step (2): adding 1 part of acrylic acid derivative thickener to 70 parts of water, stirring with a stirrer for 30 minutes at a speed of 800 r / min to evenly disperse the thickener to form an evenly dispersed thickening solution;

[0104] Step (3): Keep the stirrer in the second step running, add the evenly dispersed diamond micro-solution prepared in the first step into the thickened solution, keep the speed unchanged, and continue stirring for 5 minutes to obtain a solution with evenly dispersed abrasives;

[0105] Step (4): add 1 part of modified polyurea N-methylpyrrolidone anti-settling agent to the solution obtained in step (3), stir for 5 minutes at a constant stirrer speed to obtain a uniformly dispersed aqueous solution;

[0106] Step (5): add 2 parts of a defoaming agent, aqueous polyvinyl alcohol defoaming agent, and 1 part of an organic amine TPP anticorrosive agent to the uniformly dispersed aqueous solution obtained in step (4), keep the stirrer speed unchanged, and continue stirring for 5 minutes to obtain a uniformly dispersed aqueous solution;

[0107] Step (6): Add 2 parts of sodium hydroxide as a pH regulator to the uniformly dispersed aqueous solution obtained in step (5), replenish the pure aqueous solution until the total content of all additives and the aqueous solution is 100 parts, keep the agitator speed unchanged, and continue stirring for 30 minutes to obtain a uniformly dispersed diamond polishing liquid with a pH value of 9.

[0108] Example 7

[0109] Preferably, an environmentally friendly water-based diamond grinding liquid comprises the following raw materials in parts by weight: 10 parts of diamond micropowder with a particle size of 0.5um, 2 parts of propylene glycol, 1 part of acrylic monomer polymer thickener, 1 part of modified polyurea N-methylpyrrolidone, 2 parts of polyvinyl alcohol defoamer, 1 part of organic amine TPP, 10 parts of sodium hydroxide and 73 parts of pure water.

[0110] The preparation method of the diamond grinding liquid of the present invention comprises the following steps:

[0111] Step (1): adding 5 parts of diamond micropowder with a particle size of 0.5 μm to 10 parts of pure water solution, adding 2 parts of propylene glycol, and ultrasonically treating for 5 minutes to obtain a uniformly dispersed diamond micropowder solution;

[0112] Step (2): adding 1 part of acrylic acid derivative thickener to 70 parts of water, stirring with a stirrer for 30 minutes at a speed of 800 r / min to evenly disperse the thickener to form an evenly dispersed thickening solution;

[0113] Step (3): Keep the stirrer in the second step running, add the evenly dispersed diamond micro-solution prepared in the first step into the thickened solution, keep the speed unchanged, and continue stirring for 5 minutes to obtain a solution with evenly dispersed abrasives;

[0114] Step (4): add 1 part of modified polyurea N-methylpyrrolidone anti-settling agent to the solution obtained in step (3), stir for 5 minutes at a constant stirrer speed to obtain a uniformly dispersed aqueous solution;

[0115] Step (5): add 2 parts of a defoaming agent, aqueous polyvinyl alcohol defoaming agent, and 1 part of an organic amine TPP anticorrosive agent to the uniformly dispersed aqueous solution obtained in step (4), keep the stirrer speed unchanged, and continue stirring for 5 minutes to obtain a uniformly dispersed aqueous solution;

[0116] Step (6): Add 2 parts of sodium hydroxide as a pH regulator to the uniformly dispersed aqueous solution obtained in step (5), replenish the pure aqueous solution until the total content of all additives and the aqueous solution is 100 parts, keep the agitator speed unchanged, and continue stirring for 30 minutes to obtain a uniformly dispersed diamond polishing liquid with a pH value of 9.

[0117] The data in Table 1 show that the present invention can achieve stronger and more stable grinding quality, the grinding liquid has moderate viscosity and stable dispersion, surface scratches are avoided during grinding and polishing, and the grinding liquid has good suspension effect.

[0118] Table 1: Particle size distribution and viscosity values ​​of the products prepared in Examples 1-5

[0119] D10 D50 D90 Viscosity (25℃) Example 1 0.275μm 0.496μm 0.865μm 80.2mPa*S Example 2 16.19μm 20.25μm 24.86μm 60.5mPa*S Example 3 1.985μm 2.993μm 4.441 μm 225.7mPa*S Example 4 0.664μm 1.021μm 1.565 μm 168.2mPa*S Example 5 8.39μm 11.92μm 16.88 μm 406.5mPa*S Example 6 15.79μm 20.13μm 25.06μm 9814.2mPa*S Example 7 0.262μm 0.518μm 0.886 μm 11542mPa*S

[0120] from Figure 2 and Figure 3 The microscope images in the figure are microscope images of the samples of Example 3 and Example 4 respectively. It can be seen from the figure that the dispersion effect of the diamond single crystal in the grinding liquid is good and no agglomeration occurs.

[0121] Example 8

[0122] The recovery method of diamond grinding liquid of the present invention comprises the following steps:

[0123] Step (1): add 0.5% sodium dodecylbenzene sulfonate to the diamond polishing liquid prepared in any one of Examples 1 to 7, stir evenly to completely dissolve the sodium dodecylbenzene sulfonate, and leave for 2 hours until all the diamond powder in the solution agglomerates and precipitates;

[0124] Step (2): pour the upper layer solution in the first step into the wastewater tank, retain the precipitate, and add clean water to wash the precipitate twice;

[0125] Step (3): adding water and hydrogen peroxide solution in a ratio of 1:10 to the washed precipitate, and reacting for 2 hours to allow the hydrogen peroxide to completely degrade the sodium dodecylbenzene sulfonate, and the micropowder is redispersed to obtain a micropowder solution without a treatment agent, thereby realizing the recycling of the micropowder.

[0126] The embodiment of the present invention discloses a method for recovering diamond polishing liquid, referring to Figure 4 As shown, the recycling method comprises the following steps:

[0127] Step (1): adding a treatment agent to the used diamond polishing liquid or expired polishing liquid to agglomerate the diamond powder in the polishing liquid, and leaving it for a period of time until all the agglomerates are precipitated;

[0128] Step (2): pour the upper solution into a wastewater treatment tank, retain the precipitated powder, and wash the precipitated material with clean water 1-2 times;

[0129] Step (3): adding water and hydrogen peroxide solution to the cleaned precipitate and reacting for 1-3 hours to allow the hydrogen peroxide to completely degrade the treatment agent added in step (1), thereby obtaining a micropowder solution without the treatment agent, thereby completing the complete recovery of the diamond micropowder.

[0130] Furthermore, the dosage of sodium dodecylbenzene sulfonate is 0.5-5%.

[0131] Furthermore, the ratio of water to hydrogen peroxide is 10:1-2.

[0132] Furthermore, the hydrogen peroxide concentration was 30%.

[0133] The method for recovering micropowder in diamond polishing liquid provided by the present invention is not only applicable to the polishing liquid formula described in the present invention, but has been verified to be also applicable to the recovery of micropowder in various water-based polishing liquids.

[0134] In a specific embodiment, the steps of performing a method for recovering diamond slurry are:

[0135] Step (1): add 0.5% sodium dodecylbenzene sulfonate to the diamond polishing liquid prepared in Example 3, stir evenly to completely dissolve the sodium dodecylbenzene sulfonate, and leave for 2 hours until all the diamond micropowders in the solution are aggregated and precipitated;

[0136] Step (2): pour the upper layer solution in the first step into the wastewater tank, retain the precipitate, and add clean water to wash the precipitate twice;

[0137] Step (3): adding water and hydrogen peroxide solution in a ratio of 1:10 to the washed precipitate, reacting for 2 hours, hydrogen peroxide completely degrades sodium dodecylbenzene sulfonate, and the micropowder is redispersed to obtain a micropowder solution without a treatment agent, thereby realizing the recycling of the micropowder.

[0138] In another specific embodiment, the steps of performing a method for recovering diamond slurry are:

[0139] Step (1): Add 2% sodium dodecylbenzene sulfonate to the diamond polishing liquid prepared in Example 3, stir evenly to completely dissolve the sodium dodecylbenzene sulfonate, and leave for 1 hour until all the diamond micropowders in the solution are aggregated and precipitated;

[0140] Step (2): pour the upper layer solution in the first step into the wastewater tank, retain the precipitate, and add clean water to wash the precipitate twice;

[0141] Step (3): adding water and hydrogen peroxide solution in a ratio of 1:10 to the washed precipitate, reacting for 2 hours, hydrogen peroxide completely degrades sodium dodecylbenzene sulfonate, and the micropowder is redispersed to obtain a micropowder solution without a treatment agent, thereby realizing the recycling of the micropowder.

[0142] In another specific embodiment, the steps of performing a method for recovering diamond slurry are:

[0143] Step (1): Add 5% sodium dodecylbenzene sulfonate to the diamond polishing liquid prepared in Example 3, stir evenly to completely dissolve the sodium dodecylbenzene sulfonate, and leave for 0.5 h until all the diamond micropowders in the solution are aggregated and precipitated;

[0144] Step (2): pour the upper layer solution in the first step into the wastewater tank, retain the precipitate, and add clean water to wash the precipitate twice;

[0145] Step (3): adding water and hydrogen peroxide solution in a ratio of 1:10 to the washed precipitate, reacting for 2 hours, hydrogen peroxide completely degrades sodium dodecylbenzene sulfonate, and the micropowder is redispersed to obtain a micropowder solution without a treatment agent, thereby realizing the recycling of the micropowder.

[0146] Figure 5 This is a particle size distribution diagram of the 3 μm diamond polishing liquid prepared in Example 1 of the present invention, Figure 6 This is the appearance of the diamond polishing liquid in Example 1 of the present invention after natural sedimentation for one month. Figure 7 This is the appearance of the diamond polishing liquid in Example 1 of the present invention after natural sedimentation for 6 months. Figure 8 The particle size distribution diagram of the product obtained after being treated by the recovery method of the present invention in Example 3. As can be seen from the above figure, the grinding liquid has not precipitated or agglomerated, and is still in a good state with stable quality. In addition, the particle size distribution of the product obtained by recovery is concentrated, and there is no agglomerated large particles, and the recovery effect is good.

[0147] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. An environmentally friendly water-based diamond grinding liquid, characterized in that: The raw material composition comprises the following parts by weight: 1-10 parts of abrasive, 0.1-2 parts of wetting agent, 0.1-1 parts of thickener, 0.1-1 parts of anti-settling agent, 1-10 parts of pH regulator, 0.1-2 parts of defoaming agent, 0.1-1 parts of anti-corrosion agent and 73-97.5 parts of water; The abrasive is single crystal diamond powder; The wetting agent is one or more of ethanol, glycerol, and polyethylene glycol; The thickener is one or more of acrylic acid monomer polymers, acrylic acid derivatives, alkali-soluble anionic thickeners, and anionic polymer thickeners; The anti-settling agent is modified polyurea N-methylpyrrolidone; The pH regulator is sodium hydroxide or hydrogen peroxide; The defoamer is one of a water-based polyvinyl alcohol defoamer and a polyether siloxane copolymer; The anti-corrosion agent is one of sodium benzoate, organic amine TPP, and silicated triethanolamine.

2. The environmentally friendly water-based diamond grinding liquid according to claim 1, characterized in that: The particle size of the single crystal diamond powder is 0.5-20 μm.

3. The environmentally friendly water-based diamond grinding liquid according to claim 1, characterized in that: The pH value range of diamond polishing fluid is 7-11.

4. The environmentally friendly water-based diamond grinding liquid according to claim 1, characterized in that: The water used as the matrix is ​​purified pure water.

5. A process for preparing a water-based diamond grinding liquid according to any one of claims 1 to 4, characterized in that: The preparation process comprises the following steps: Step (1): mixing diamond micropowder and water and stirring evenly, adding a dispersant and a wetting agent and stirring evenly, and ultrasonically treating for 5-20 minutes to obtain a surface-modified diamond micropowder solution; Step (2): adding the thickener to pure water and stirring with a stirrer for 10-30 minutes to obtain a uniformly dispersed viscous solution; Step (3): pouring the uniformly dispersed diamond powder solution obtained in step (1) into the uniformly dispersed viscous solution in step (2), and continuing to stir with a stirrer for 10-30 minutes; Step (4): adding an anti-settling agent to the solution obtained in step (3), stirring for 5-10 minutes to obtain a uniformly dispersed aqueous solution 1; Step (5): adding a defoamer and an anti-corrosion agent to the uniformly dispersed aqueous solution 1 obtained in step (4), and continuing stirring for 5-10 minutes to obtain a uniformly dispersed aqueous solution 2; Step (6): Add a pH regulator to the uniformly dispersed aqueous solution obtained in step (5) to adjust the pH value of the grinding liquid, and continue stirring for 10-30 minutes to obtain a uniformly dispersed diamond grinding liquid.

6. A method for recovering micropowder in water-based diamond grinding liquid, characterized in that: The method includes: Step (1): adding a treatment agent to the used diamond polishing liquid or expired polishing liquid to agglomerate the diamond powder in the polishing liquid, and leaving it for a period of time until all the agglomerates are precipitated; Step (2): pour the upper solution into a wastewater treatment tank, retain the precipitated powder, and wash the precipitated material with clean water 1-2 times; Step (3): adding water and hydrogen peroxide solution to the cleaned precipitate and reacting for 1-3 hours to allow the hydrogen peroxide to completely degrade the treatment agent added in step (1), thereby obtaining a micropowder solution without the treatment agent, thereby completing the complete recovery of the diamond micropowder.

7. The method for recovering micro powder in water-based diamond grinding liquid according to claim 6, characterized in that: The treating agent in step (1) is sodium dodecylbenzene sulfonate.

8. The method for recovering micro powder in water-based diamond grinding liquid according to claim 7, characterized in that: The dosage of the sodium dodecylbenzene sulfonate is 0.5-5%.

9. The method for recovering micro powder in water-based diamond grinding liquid according to claim 6, characterized in that: In step (3), the ratio of water to hydrogen peroxide is 10:1-2.

10. The method for recovering fine powder in water-based diamond grinding liquid according to claim 9, characterized in that: The concentration of hydrogen peroxide is 30%.

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