Preparation method and application of biomass carbon dot corrosion inhibitor

Abstract

The invention discloses a preparation method of a biomass carbon dot corrosion inhibitor, comprising the following steps: washing peanut shells, drying them naturally, crushing them and sieving them, placing them in a 1-5% NaOH solution after sieving them for reaction for 3-8 hours, filtering and rinsing them to neutrality after the reaction is completed; drying the treated peanut shells, placing them in a 1-5% NaClO2 solution, adjusting the pH of the solution to acidity with acetic acid and reacting them for 3-5 hours, filtering and rinsing them to neutrality after the reaction is completed to obtain peanut shell cellulose; sealing the peanut shell cellulose and deionized water in a stainless steel autoclave lined with polytetrafluoroethylene for heating for 10-14 hours, cooling them naturally to room temperature, centrifuging them for 8-12 minutes, filtering and removing residual large particles, and then adding 10-30 ml of 0-200 mg / L Ca 2+ The mixture is stirred evenly, and solid biomass carbon dot CDs powder is obtained by rotary evaporation and vacuum freeze drying; 1 to 10% of the CDs powder obtained in step 3 is added with 0.5 to 10% sodium molybdate, 5 to 20% polyethylene glycol, 0.5 to 5% polymethylsiloxane, 5 to 15% sodium tetraacetate and 45 to 85% water, and mixed evenly.

Description

Technical field:

[0001] The invention belongs to the technical field of photovoltaic silicon wafer cutting coolant, and in particular relates to a preparation method and application of a biomass carbon dot corrosion inhibitor. Background technology:

[0002] As a green energy, solar energy has gradually become the development direction of science and technology and industry, and the photovoltaic power generation industry is the main application form of solar energy. The photovoltaic power generation industry basically requires silicon-based materials to manufacture solar cells.

[0003] The manufacturing process involves the slicing of silicon-based materials. Currently, there are two main slicing processes for silicon-based materials: mortar cutting and diamond wire cutting. Diamond wire is made by electroplating silicon carbide powder on steel wire or resin wire, and the silicon-based material is cut through the reciprocating motion of the diamond wire. Flushing fluid is an important material used in the diamond wire cutting process, mainly including rust inhibitors, emulsifiers, defoaming agents, etc., among which rust inhibitors (also called corrosion inhibitors) are one of the main ingredients. Currently, commonly used rust inhibitors mainly use organic substances such as benzotriazoles and organic amines, but these organic substances are highly polluting and do not conform to the concept of green, environmental protection, and renewable.

[0004] Biomass materials are new materials with excellent performance and high added value, which are made from woody plants, grasses and vines and their processing residues and wastes through high-tech means such as physics, chemistry and biology. They are green, environmentally friendly and renewable materials with the characteristics of easy acquisition, low cost and abundant sources. This application proposes a biomass-based corrosion inhibitor that can meet the concepts of green, environmental protection and renewable while meeting the requirements of rust prevention and corrosion inhibition.

[0005] The information disclosed in this background technology section is only intended to enhance the understanding of the overall background of the invention and should not be regarded as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art. Summary of the invention:

[0006] The purpose of the present invention is to provide a preparation method and application of a biomass carbon dot corrosion inhibitor, thereby overcoming the defects in the above-mentioned prior art.

[0007] In order to achieve the above object, the present invention provides a method for preparing a biomass carbon dot corrosion inhibitor, comprising the following steps:

[0008] Step 1: Wash the peanut shells, dry them naturally, crush them and sieve them, place them in a 1-5% NaOH solution to react for 3-8 hours, and filter and rinse them to neutral after the reaction is completed;

[0009] Step 2: Dry the peanut shells treated in step 1 and place them in 1-5% NaClO 2 In the solution, acetic acid is used to adjust the pH of the solution to acidity and react for 3 to 5 hours. After the reaction is completed, the solution is filtered and rinsed to neutrality to obtain peanut shell cellulose;

[0010] Step 3: Heat the peanut shell cellulose and deionized water in a sealed polytetrafluoroethylene-lined stainless steel autoclave for 10 to 14 hours, cool naturally to room temperature, centrifuge for 8 to 12 minutes, filter to remove the remaining large particles, and then add 10 to 30 ml of 0 to 200 mg / L Ca 2+ The mixture was stirred evenly, and solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying;

[0011] Step 4: Take 1-10% of the CDs powder obtained in step 3, add 0.5-10% sodium molybdate, 5-20% polyethylene glycol, 0.5-5% polymethylsiloxane, 5-15% sodium tetraacetate and 45-85% water and mix well.

[0012] Furthermore, preferably, in the step 1, a 50-70 mesh sieve is used to sieve the crushed peanut shells.

[0013] Furthermore, preferably, in step 1, the weight ratio of peanut shells to NaOH solution is 1:15-25.

[0014] Furthermore, preferably, the step 1 is reacted at 95-105°C.

[0015] Furthermore, as a preferred embodiment, in the step 2, the peanut shells and NaClO 2 The weight ratio of the solution is 1:15-25.

[0016] Furthermore, preferably, the pH in step 2 is adjusted to 3-5.

[0017] Furthermore, preferably, the step 2 is reacted at 75-85°C.

[0018] Furthermore, preferably, in step three, the weight ratio of peanut shell cellulose to deionized water is 1:10-20.

[0019] Furthermore, preferably, the step three is reacted at 180-220°C.

[0020] Furthermore, preferably, in step three, a 0.1-0.3 μm filter membrane is used to remove residual large particles.

[0021] The present invention also provides an application of a biomass carbon dot corrosion inhibitor, which is used as a component in a coolant during cutting of silicon-based materials.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] (1) The present invention uses peanut shell as raw material, adds Ca 2+ Finally, a slow-release liquid with good corrosion resistance can be obtained. It does not contain organic matter such as phosphates, borates, amine salts, nitrites, benzotriazoles, organic amines, etc., will not cause eutrophication of water bodies, is environmentally friendly, and is renewable, which is of great significance to economic development and scientific research progress.

[0024] (2) In the present invention, sodium molybdate is added to the system, and the biomass and sodium molybdate produce a synergistic effect, which can improve the corrosion resistance effect. Specific implementation method:

[0025] The specific embodiments of the present invention are described in detail below, but it should be understood that the protection scope of the present invention is not limited by the specific embodiments.

[0026] A brief summary of one or more aspects is given below to provide a basic understanding of these aspects. This summary is not an exhaustive overview of all conceived aspects, and is neither intended to identify the key or critical elements of all aspects nor to define the scope of any or all aspects. Its only purpose is to give some concepts of one or more aspects in a simplified form as a prelude to a more detailed description that will be given later.

[0027] Embodiment 1:

[0028] A method for preparing a biomass carbon dot corrosion inhibitor comprises the following steps:

[0029] Step 1: Wash and naturally dry the peanut shells, crush them and sieve them with a 60-mesh sieve. After sieving, place them in a 2% NaOH solution at 100° C. for reaction for 5 hours. After the reaction is completed, filter and rinse until neutral. The weight ratio of peanut shells to NaOH solution is 1:20.

[0030] Step 2: Dry the peanut shells treated in step 1 and place them in 2% NaClO 2 The solution was adjusted to pH 4 with acetic acid, and the reaction was carried out at 80°C for 4 hours. After the reaction was completed, the solution was filtered and rinsed to neutrality, and then dried to obtain peanut shell cellulose, in which peanut shell and NaClO 2 The weight ratio of the solution is 1:20;

[0031] Step 3: 2 g peanut shell cellulose and 100 ml deionized water were sealed in a 150 ml polytetrafluoroethylene-lined stainless steel autoclave and heated to 200 ° C for 12 h. After naturally cooling to room temperature, the mixture was centrifuged at 10,000 rpm for 10 min, and then filtered through a 0.2 μm filter membrane to remove the remaining large particles. Solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying.

[0032] Step 4: Take 2% of the CDs powder obtained in step 3, add 5% sodium molybdate, 18% polyethylene glycol, 2% polymethylsiloxane, 10% sodium tetraacetate and 63% water and mix well.

[0033] Embodiment 2:

[0034] A method for preparing a biomass carbon dot corrosion inhibitor comprises the following steps:

[0035] Step 1: Wash and naturally dry the peanut shells, crush them and sieve them with a 60-mesh sieve. After sieving, place them in a 2% NaOH solution at 100° C. for reaction for 5 hours. After the reaction is completed, filter and rinse until neutral. The weight ratio of peanut shells to NaOH solution is 1:20.

[0036] Step 2: Dry the peanut shells treated in step 1 and place them in 2% NaClO 2 The solution was adjusted to pH 4 with acetic acid, and the reaction was carried out at 80°C for 4 hours. After the reaction was completed, the solution was filtered and rinsed to neutrality, and then dried to obtain peanut shell cellulose, in which peanut shell and NaClO 2 The weight ratio of the solution is 1:20;

[0037] Step 3: 2g peanut shell cellulose and 100ml deionized water were sealed in a 150ml polytetrafluoroethylene-lined stainless steel autoclave and heated to 200℃ for 12h. After cooling to room temperature naturally, the mixture was centrifuged at 10,000 rpm for 10min, and then filtered through a 0.2μm filter membrane to remove the remaining large particles. Then, 20ml of 100mg / L Ca 2+ The mixture was stirred evenly, and solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying;

[0038] Step 4: Take 4% of the CDs powder obtained in step 3, add 5% sodium molybdate, 18% polyethylene glycol, 2% polymethylsiloxane, 10% sodium tetraacetate and 61% water and mix well.

[0039] Embodiment 3:

[0040] A method for preparing a biomass carbon dot corrosion inhibitor comprises the following steps:

[0041] Step 1: Wash and naturally dry the peanut shells, crush them and sieve them with a 60-mesh sieve. After sieving, place them in a 2% NaOH solution at 100° C. for reaction for 5 hours. After the reaction is completed, filter and rinse until neutral. The weight ratio of peanut shells to NaOH solution is 1:20.

[0042] Step 2: Dry the peanut shells treated in step 1 and place them in 2% NaClO 2 The solution was adjusted to pH 4 with acetic acid, and the reaction was carried out at 80°C for 4 hours. After the reaction was completed, the solution was filtered and rinsed to neutrality, and then dried to obtain peanut shell cellulose, in which peanut shell and NaClO 2 The weight ratio of the solution is 1:20;

[0043] Step 3: 2g peanut shell cellulose and 100ml deionized water were sealed in a 150ml polytetrafluoroethylene-lined stainless steel autoclave and heated to 200℃ for 12h. After cooling to room temperature naturally, the mixture was centrifuged at 10,000 rpm for 10min, and then filtered through a 0.2μm filter membrane to remove the remaining large particles. Then, 20ml of 200mg / L Ca 2+ The mixture was stirred evenly, and solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying;

[0044] Step 4: Take 6% of the CDs powder obtained in step 3, add 5% sodium molybdate, 18% polyethylene glycol, 2% polymethylsiloxane, 10% sodium tetraacetate and 59% water and mix well.

[0045] Embodiment 4:

[0046] A method for preparing a biomass carbon dot corrosion inhibitor comprises the following steps:

[0047] Step 1: Wash and naturally dry the peanut shells, crush them and sieve them with a 60-mesh sieve. After sieving, place them in a 2% NaOH solution at 100° C. for reaction for 5 hours. After the reaction is completed, filter and rinse until neutral. The weight ratio of peanut shells to NaOH solution is 1:20.

[0048] Step 2: Dry the peanut shells treated in step 1 and place them in 2% NaClO 2 The solution was adjusted to pH 4 with acetic acid, and the reaction was carried out at 80°C for 4 hours. After the reaction was completed, the solution was filtered and rinsed to neutrality, and then dried to obtain peanut shell cellulose, in which peanut shell and NaClO 2 The weight ratio of the solution is 1:20;

[0049] Step 3: 2g peanut shell cellulose and 100ml deionized water were sealed in a 150ml polytetrafluoroethylene-lined stainless steel autoclave and heated to 200℃ for 12h. After cooling to room temperature naturally, the mixture was centrifuged at 10,000 rpm for 10min, and then filtered through a 0.2μm filter membrane to remove the remaining large particles. Then, 20ml of 100mg / L Ca 2+ The mixture was stirred evenly, and solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying;

[0050] Step 4: Take 8% of the CDs powder obtained in step 3, add 5% sodium molybdate, 18% polyethylene glycol, 2% polymethylsiloxane, 10% sodium tetraacetate and 57% water and mix well.

[0051] Embodiment 5:

[0052] A method for preparing a biomass carbon dot corrosion inhibitor comprises the following steps:

[0053] Step 1: Wash and naturally dry the peanut shells, crush them and sieve them with a 60-mesh sieve. After sieving, place them in a 2% NaOH solution at 100° C. for reaction for 5 hours. After the reaction is completed, filter and rinse until neutral. The weight ratio of peanut shells to NaOH solution is 1:20.

[0054] Step 2: Dry the peanut shells treated in step 1 and place them in 2% NaClO 2 The solution was adjusted to pH 4 with acetic acid, and the reaction was carried out at 80°C for 4 hours. After the reaction was completed, the solution was filtered and rinsed to neutrality, and then dried to obtain peanut shell cellulose, in which peanut shell and NaClO 2 The weight ratio of the solution is 1:20;

[0055] Step 3: 2g peanut shell cellulose and 100ml deionized water were sealed in a 150ml polytetrafluoroethylene-lined stainless steel autoclave and heated to 200℃ for 12h. After cooling to room temperature naturally, the mixture was centrifuged at 10,000 rpm for 10min, and then filtered through a 0.2μm filter membrane to remove the remaining large particles. Then, 20ml of 200mg / L Ca 2+ The mixture was stirred evenly, and solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying;

[0056] Step 4: Take 10% of the CDs powder obtained in step 3, add 5% sodium molybdate, 18% polyethylene glycol, 2% polymethylsiloxane, 10% sodium tetraacetate and 55% water and mix well.

[0057] Embodiment 6:

[0058] Step 1: Wash and naturally dry the peanut shells, crush them and sieve them with a 60-mesh sieve. After sieving, place them in a 2% NaOH solution at 100° C. for reaction for 5 hours. After the reaction is completed, filter and rinse until neutral. The weight ratio of peanut shells to NaOH solution is 1:20.

[0059] Step 2: Dry the peanut shells treated in step 1 and place them in 2% NaClO 2 The solution was adjusted to pH 4 with acetic acid, and the reaction was carried out at 80°C for 4 hours. After the reaction was completed, the solution was filtered and rinsed to neutrality, and then dried to obtain peanut shell cellulose, in which peanut shell and NaClO 2 The weight ratio of the solution is 1:20;

[0060] Step 3: 2g peanut shell cellulose and 100ml deionized water were sealed in a 150ml polytetrafluoroethylene-lined stainless steel autoclave and heated to 200℃ for 12h. After cooling to room temperature naturally, the mixture was centrifuged at 10,000 rpm for 10min, and then filtered through a 0.2μm filter membrane to remove the remaining large particles. Then, 20ml of 200mg / L Ca 2+ The mixture was stirred evenly, and solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying;

[0061] Step 4: Take 10% of the CDs powder obtained in step 3, add 18% polyethylene glycol, 2% polymethylsiloxane, 10% sodium tetraacetate and 60% water and mix well.

[0062] The corrosion inhibitors prepared in the above Examples 1-6 were tested, and the testing method was as follows:

[0063] 10% of the corrosion inhibitor prepared in Examples 1-6 was added to the commercially available rinsing liquid respectively, and the rinsing liquid with the corrosion inhibitor added was loaded into the rinsing tank.

[0064] The cut silicon wafers are dried and the dried silicon wafers are about 0.02m 2 The silicon wafers were sequentially passed through a 5g / L alkaline washing tank, a rinsing tank, a 5g / L hydrofluoric acid washing tank and a rinsing tank in a conveyor device rolling at 1 m / min to test the corrosion effect of the silicon wafers. Three silicon wafer samples were used for testing in each embodiment, and the average value of the three samples was taken. The test results are shown in Table 1 below:

[0065] Table 1: Silicon wafer corrosion effects

[0066]

[0067] The results showed that when Ca was added 2+ After that, the film formed on the surface of the silicon wafer is made denser, which can improve the corrosion inhibition effect of the rinse solution, and as Ca 2+As the ion concentration increases, the corrosion performance is more effectively suppressed; in addition, when sodium molybdate is added to the system, biomass can produce a synergistic effect with sodium molybdate, and the corrosion inhibition effect is more obvious.

[0068] The foregoing description of specific exemplary embodiments of the present invention is for the purpose of illustration and demonstration. These descriptions are not intended to limit the present invention to the precise form disclosed, and it is clear that many changes and variations can be made based on the above teachings. The purpose of selecting and describing the exemplary embodiments is to explain the specific principles of the present invention and its practical application, so that those skilled in the art can realize and utilize various different exemplary embodiments of the present invention and various different selections and changes. The scope of the present invention is intended to be limited by the claims and their equivalents.

Claims

1. A method for preparing a biomass carbon dot corrosion inhibitor, characterized in that: The steps include: Step 1: Wash the peanut shells, dry them naturally, crush them and sieve them. After sieving, place them in a 1-5% NaOH solution to react for 3-8 hours. After the reaction is completed, filter and rinse them until they are neutral; Step 2: Dry the peanut shells treated in step 1 and place them in a 1-5% NaClO2 solution, adjust the pH of the solution to acidity with acetic acid and react for 3-5 hours. After the reaction is completed, filter and rinse to neutrality to obtain peanut shell cellulose; Step 3: Heat the peanut shell cellulose and deionized water in a sealed PTFE-lined stainless steel autoclave for 10-14 hours, cool to room temperature, centrifuge for 8-12 minutes, filter to remove the remaining large particles, and then add 10-30 ml of 0-200 mg / L Ca 2+ The mixture was stirred evenly, and solid biomass carbon dots CDs powder was obtained by rotary evaporation and vacuum freeze drying; Step 4: Take 1-10% of the CDs powder obtained in step 3, add 0.5-10% sodium molybdate, 5-20% polyethylene glycol, 0.5-5% polymethylsiloxane, 5-15% sodium tetraacetate and 45-85% water and mix well; The step 1 is reacted at 95-105°C; The step 2 is reacted at 75-85°C; The step three is reacted at 180-220°C.

2. The method for preparing a biomass carbon dot corrosion inhibitor according to claim 1, characterized in that: In the step 1, the crushed peanut shells are sieved using a 50-70 mesh sieve.

3. The method for preparing a biomass carbon dot corrosion inhibitor according to claim 1, characterized in that: In the step 1, the weight ratio of peanut shells to NaOH solution is 1:15-25.

4. The method for preparing a biomass carbon dot corrosion inhibitor according to claim 1, characterized in that: In the step 2, the weight ratio of peanut shells to NaClO2 solution is 1:15-25.

5. The method for preparing a biomass carbon dot corrosion inhibitor according to claim 1, characterized in that: In step three, the weight ratio of peanut shell cellulose to deionized water is 1:10-20.

6. The method for preparing a biomass carbon dot corrosion inhibitor according to claim 1, characterized in that: In step three, a 0.1-0.3 μm filter membrane is used to remove residual large particles.

7. Use of the biomass carbon dot corrosion inhibitor obtained by the preparation method of the biomass carbon dot corrosion inhibitor according to any one of claims 1 to 6 as a component in a coolant when cutting silicon-based materials.

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