Reaction kettle for chemical plating and chemical nickel plating method for diamond micro powder
By using a chemical plating reactor in the process of electroless nickel plating of diamond micropowder, combined with stirring and ultrasonic technology, the problems of low plating efficiency and poor plating effect are solved, and efficient and stable nickel plating effect are achieved.
Patent Information
- Application Number
- CN202411952134.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-02-18
AI Technical Summary
The existing diamond powder electroless nickel plating process has low plating efficiency, small single plating amount, and poor plating effect.
The chemical plating reactor is used to drive the stirring blades to stir the liquid and diamond powder in the kettle body through the first motor. The adhesion of diamond powder is controlled by combining ultrasonic waves and stirring. The sodium hypophosphite is continuously transported into the kettle body through the conveying pump to control the reaction. process.
It effectively improves the plating efficiency, increases the amount of diamond powder treated in a single time, reduces leakage plating and agglomeration, and ensures the quality stability of the electroless nickel plating process.
Smart Images
Figure CN119465113A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of diamond micropowder processing, and in particular relates to a reaction kettle for chemical plating and a diamond micropowder chemical nickel plating method. Background Art
[0002] In the process of preparing diamond micropowder for diamond wire sanding, the chemical plating is to coat a layer of nickel on the surface of the diamond micropowder, which can give the diamond micropowder better performance and application characteristics. At present, the diamond micropowder is mostly mixed with the required liquid medicine in a barrel, and the staff needs to stir it at all times to ensure the plating effect of chemical nickel plating. There are problems such as low plating efficiency, small single plating amount, and poor plating effect. Summary of the invention
[0003] The present invention aims to solve the problems of low plating efficiency, small single plating amount, poor plating effect and the like in the existing diamond micropowder chemical nickel plating method, in which the diamond micropowder is mixed with the required liquid in a small barrel and stirred. A reaction kettle for chemical plating and a diamond micropowder chemical nickel plating method are provided. The liquid and the diamond micropowder in the kettle are stirred by a first motor driving a stirring blade, the plating temperature is ensured by circulating hot oil between the inner layer and the outer layer of the kettle, the adhesion between the diamond micropowders is controlled by ultrasonic wave and stirring, and sodium hypophosphite is continuously transported into the kettle by a delivery pump. The present invention can control the reaction process, so that the overall reaction is controlled in a stable and controllable state, and the effects of plating leakage, agglomeration and the like occurring in the process of mass production of diamond micropowder chemical nickel plating are solved.
[0004] In order to achieve the above object, the technical solution of the present invention is: A reaction kettle for chemical plating, comprising a mounting frame, a kettle body and a cover body are arranged on the mounting frame, the kettle body comprises an inner layer and an outer layer, there is a gap between the inner layer and the outer layer, a circulation inlet is arranged at the lower end of the kettle body, and a circulation outlet is arranged at the upper end, the circulation inlet and the circulation outlet are both connected to the gap between the inner layer and the outer layer, and the circulation inlet and the circulation outlet are both connected to a feed box through a pipeline. Preferably, the feed box contains hot oil, and the hot oil is circulated in the gap between the inner and outer layers of the kettle body through the circulation inlet and the circulation outlet, effectively controlling the temperature of the kettle body to 85°C to 95°C, ensuring the smooth progress of the reaction.
[0005] The cover body is connected to the mounting frame for sliding up and down movement, and a stirring assembly, an ultrasonic assembly and a dosing assembly are arranged on the cover body. The stirring assembly is used to stir the liquid in the kettle body, the ultrasonic assembly is used to emit ultrasonic waves into the kettle body, and the dosing assembly is used to transport medicine into the kettle body. By sliding the cover body up and down, the stirring assembly, the ultrasonic assembly and the dosing assembly are synchronously moved away from the kettle body, so that the cover body is opened to stop working or the cover body is closed to start working.
[0006] Preferably, the stirring assembly includes a first motor, a stirring shaft and a stirring blade. The first motor is fixedly arranged above the cover body, the output end of the first motor is fixedly connected to the stirring shaft, the lower end of the stirring shaft extends to the lower inner part of the kettle body, and the stirring blade is arranged on the stirring shaft. The first motor drives the stirring shaft to rotate, which drives the stirring blade to rotate, thereby stirring the diamond powder and liquid in the kettle body.
[0007] Preferably, the stirring shaft is fixedly sleeved with a plurality of connection seats spaced apart from each other, and each connection seat is circumferentially fixed with a plurality of stirring blades. The spiral blades on the plurality of connection seats rotate synchronously to ensure the stirring effect on the kettle body.
[0008] Preferably, the ultrasonic component includes at least one ultrasonic generator, the lower end of which penetrates the cover body and extends into the kettle body, and is used to emit ultrasonic waves to the liquid in the kettle body. The ultrasonic generator further enhances the dispersion effect of diamond micropowder in the liquid in the kettle body and controls the adhesion between diamond micropowders.
[0009] Preferably, the drug adding component includes a drug inlet pipe, which passes through the cover body and extends into the kettle body. The drug inlet pipe is connected to a delivery pump, which is connected to a storage box. The storage box contains medicine. The medicine is continuously delivered to the kettle body by the delivery pump to control the reaction in the kettle body to proceed at a uniform speed, thereby ensuring the chemical plating effect.
[0010] Preferably, the drug inlet pipe is provided in plurality, the plurality of drug inlet pipes are circumferentially arranged on the cover body, the plurality of drug inlet pipes are commonly connected to the delivery pump, and the plurality of drug inlet pipes simultaneously deliver the medicine into the kettle body to ensure rapid diffusion of the medicine in the kettle body.
[0011] Preferably, the mounting frame includes a support plate and a vertical pole, the vertical pole is fixedly arranged above the support plate, a second motor is fixedly arranged on the upper side of the vertical pole, one side of the vertical pole is fixedly connected to the kettle body, the support plate corresponds to the kettle body up and down, a slide groove is downwardly provided at the upper end of the vertical pole, a screw is fixedly connected to the output end of the second motor, the screw extends into the slide groove, a mounting seat is provided in the slide groove for sliding up and down, the screw is threadedly connected to the mounting seat, the mounting seat extends out of one side of the vertical pole and is fixedly connected to the cover body, the screw is driven to rotate by the second motor, and the mounting seat and the cover body are driven to rise and fall.
[0012] Preferably, a discharge pipe is fixedly provided at the lower end of the kettle body, and the discharge pipe penetrates the outer layer and the inner layer and extends into the kettle body. A valve is provided on the discharge pipe. After the nickel plating of the diamond powder is completed, the valve is opened, and the diamond powder and liquid are discharged from the kettle body through the discharge pipe.
[0013] The present invention also provides a diamond powder chemical nickel plating method, using the above-mentioned chemical plating reactor, the chemical nickel plating method comprises the following steps: Step 1: Weigh diamond micropowder according to the measurement to prepare reagent No. 1 and reagent No. 2; The No. 1 reagent is prepared by mixing the following raw materials: nickel sulfate, sodium citrate, lactic acid, dispersant and ammonia water, and the solvent is water; The No. 2 agent is prepared by mixing the following raw materials: sodium hypophosphite and sodium hydroxide, and the solvent is water; The ratio of the total volume of diamond powder to the No. 1 agent and the No. 2 agent is (25-65) g:1 L, and the volume ratio of the No. 1 agent to the No. 2 agent is (1-4):1; Step 2: Add reagent No. 1 into the kettle body, add diamond powder into the kettle body at the same time, heat the kettle body to a predetermined temperature, the predetermined temperature is 85°C to 95°C, turn on the ultrasonic generator and turn on the stirring component to stir the liquid in the kettle body, and after stirring evenly, slowly add reagent No. 2, and add reagent No. 2 into the kettle body through the dosing component, the dosing speed is 30 to 80 ml / min, the dosing time is 2.5 to 3 hours, and after the addition of reagent No. 2, continue to stir and react for 20 to 40 minutes. After the reaction is completed, the liquid in the kettle body is precipitated and washed to obtain nickel-plated diamond powder.
[0014] Furthermore, the mass of the diamond powder is 2000-5000 g, the sum of the volumes of agent No. 1 and agent No. 2 is 80-100 L, and the volume ratio of agent No. 1 to agent No. 2 is (3-4):1; The No. 1 agent is prepared by mixing the following raw materials: 4900-12250 g of nickel sulfate, 1460-3650 g of sodium citrate (complexing agent), 200-300 ml of lactic acid (complexing agent), 100-250 ml of dispersant and 6.2-15.5 liters of ammonia water (ammonia water concentration is 28%, used as pH control and complexing agent), the solvent is water, wherein the amount of water added is such that the volume ratio of the No. 1 agent to the No. 2 agent is (3-4):1; The No. 2 agent is prepared by mixing the following raw materials: 6750-16875 grams of sodium hypophosphite (reducing agent) and 40-100 grams of sodium hydroxide (pH control), and the solvent is water, wherein the amount of water added is such that the volume ratio of the No. 1 agent to the No. 2 agent is (3-4):1.
[0015] Further, in step 2, the predetermined temperature is 90° C., and the stirring speed is 200 to 600 rpm; The mass of the diamond powder is 2000g, the volume of the No. 1 reagent is 60L, and the volume of the No. 2 reagent is 20L; The No. 1 reagent is prepared by mixing the following raw materials: 4900 g of nickel sulfate, 1460 g of sodium citrate, 200 ml of lactic acid, 100 ml of dispersant and 6.2 liters of ammonia water, the solvent is water, and the amount of water added makes the volume of the No. 1 reagent 60 L; The No. 2 agent is prepared by mixing the following raw materials: 6750 grams of sodium hypophosphite and 40 grams of sodium hydroxide, and the solvent is water, wherein the amount of water added makes the volume of the No. 2 agent 20L.
[0016] Preferably, the dosing speed of agent No. 2 is gradually increased, the initial dosing speed is 30 ml / min, and the dosing speed increases by 8 ml / min every half hour. As the dosing time increases, the volume of the liquid in the kettle increases. If the initial dosing speed is maintained, the reaction speed decreases. Therefore, as time goes by, the dosing speed needs to be increased to keep the reaction speed balanced.
[0017] Preferably, when diamond powder and agent No. 1 are mixed, the stirring speed is 200 rpm. When agent No. 2 is added, the stirring speed is adjusted to 250-300 rpm, and then the stirring speed is increased by 50 rpm every half hour. As the dosing time increases, the volume of the liquid in the kettle increases, so it is necessary to increase the stirring speed to keep the reaction speed balanced.
[0018] Through the above technical solution, the beneficial effects of the present invention are: 1. The present invention stirs the diamond micropowder and liquid in the kettle, emits ultrasonic waves, and controls the reaction temperature by heating in an oil bath, thereby ensuring that the chemical nickel plating reaction of the diamond micropowder proceeds smoothly, effectively reducing or even avoiding the adhesion between the diamond micropowders, thereby greatly increasing the processing amount of the diamond micropowder participating in the reaction at a single time.
[0019] 2. The present invention drives the stirring blade to rotate by the first motor to achieve stirring of the solution, effectively reduce the adhesion between diamond micropowders, effectively increase the amount of diamond micropowder processed in a single time, and reduce the labor intensity of the staff.
[0020] 3. The present invention emits ultrasonic waves into the solution through an ultrasonic generator, and under the action of ultrasound, the adhesion between diamond micropowders is further reduced, and the phenomenon of plating leakage and agglomeration is avoided.
[0021] 4. The delivery pump of the present invention continuously delivers reagent No. 2 to the kettle through the dosing pipe, thereby controlling the reaction process in the kettle and ensuring the quality stability of the diamond micropowder chemical plating process.
[0022] 5. The present invention effectively controls the temperature inside the kettle body through oil bath heating, that is, hot oil is transported from the feed box pipeline and enters the gap between the inner layer and the outer layer of the kettle body through the circulation inlet, and is transported to the feed box from the circulation outlet pipeline, thereby ensuring that the temperature inside the kettle body is controlled at 85°C to 95°C, and more preferably controlled at about 90°C. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] Figure 1 The structure of the present invention is schematically shown Figure 1 .
[0024] Figure 2 The structure of the present invention is schematically shown Figure 2 .
[0025] Figure 3 It is a schematic structural diagram of the kettle body of the present invention.
[0026] Figure 4 This is a particle size test report of diamond micropowder after nickel plating in Example 2 of the present invention.
[0027] Figure 5 This is a SEM image of diamond powder after nickel plating in Example 2 of the present invention.
[0028] Figure 6 This is a SEM image of diamond powder after nickel plating in Example 3 of the present invention.
[0029] Figure 7 This is a SEM image of diamond powder after nickel plating in Example 4 of the present invention.
[0030] Figure 8 This is one of the SEM images of diamond powder after nickel plating in the prior art.
[0031] Fig. 9 This is the second SEM image of diamond powder after nickel plating in the prior art.
[0032] The numbers in the accompanying drawings are: 1 is a mounting frame, 2 is a kettle body, 3 is a cover body, 4 is a circulation inlet, 5 is a circulation outlet, 6 is a first motor, 7 is a stirring shaft, 8 is a stirring blade, 9 is an ultrasonic generator, 10 is a medicine inlet pipe, 11 is a second motor, 12 is a slide chute, 13 is a screw, 14 is a mounting seat, 15 is a discharge pipe, and 16 is a valve. DETAILED DESCRIPTION
[0033] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments: The missed plating mentioned in the present invention refers to the fact that the surface of the diamond powder is not plated with nickel or 50% or more of the surface is not plated with nickel.
[0034] Agglomeration refers to the situation where two or more diamond powders stick together under the action of the nickel layer due to untimely dispersion of diamond powder during the nickel plating process.
[0035] Example 1 like Figure 1 to Figure 3As shown, this embodiment provides a chemical plating reactor, including a mounting frame 1, on which a reactor body 2 and a cover body 3 are arranged. Before the chemical plating starts, diamond powder, No. 1 reagent, etc. are added to the reactor body 2, and then the cover body 3 is covered. A through hole is opened on the cover body 3 for connecting the inside and outside of the reactor body 2 to ensure that the inside of the reactor body 2 is connected to the outside during the chemical plating process. The mounting frame 1 includes a support plate and a vertical pole, the vertical pole is fixedly arranged above the support plate, and a second motor 11 is fixedly arranged on the upper side of the vertical pole. One side of the vertical rod is fixedly connected to the kettle body 2, the support plate corresponds to the kettle body 2 up and down, the upper end of the vertical rod is provided with a slide groove 12 downward, the output end of the second motor 11 is fixedly connected with a screw rod 13, the screw rod 13 extends into the slide groove 12, a mounting seat 14 is provided in the slide groove 12 for sliding up and down, the screw rod 13 is threadedly connected to the mounting seat 14, the mounting seat 14 extends out of one side of the vertical rod and is fixedly connected to the cover body 3, the second motor 11 drives the screw rod to rotate, drives the mounting seat 14 to move up and down, and drives the cover body 3 to move up and down.
[0036] The kettle body 2 includes an inner layer and an outer layer, and there is a gap between the inner layer and the outer layer. A circulation inlet 4 is arranged at the lower end of the kettle body 2, and a circulation outlet 5 is arranged at the upper end. The circulation inlet 4 and the circulation outlet 5 are both connected to the gap between the inner layer and the outer layer. The circulation inlet 4 and the circulation outlet 5 are both connected to a supply box (not shown in the figure) through pipelines. The supply box can provide hot water, hot steam or hot oil, etc. into the gap. In this embodiment, the supply box is filled with hot oil. The hot oil in the supply box enters the gap between the inner layer and the outer layer along the circulation inlet 4. As the hot oil level in the gap continues to rise, when it reaches the position of the circulation outlet 5, the hot oil basically covers the kettle body 2. Then the hot oil is discharged from the circulation outlet 5 and transported to the supply box through a pipeline to complete the circulation of the hot oil. Then, the kettle body 2 is heated in an oil bath through the circulation of the hot oil to ensure that the temperature of the kettle body 2 is controlled at 85°C to 95°C, thereby ensuring the smooth progress of the chemical plating reaction.
[0037] The cover body 3 is connected to the mounting frame 1 in an up-and-down sliding manner, and a stirring component, an ultrasonic component and a dosing component are arranged on the cover body 3 .
[0038] The stirring assembly is used to stir the liquid in the kettle body 2, and the stirring assembly includes a first motor 6, a stirring shaft 7 and a stirring blade 8. The first motor 6 is fixedly arranged above the cover body 3, and the output end of the first motor 6 is fixedly connected to the stirring shaft 7. The first motor 6 drives the stirring shaft 7 to rotate. The lower end of the stirring shaft 7 extends to the lower part of the kettle body 1. The stirring blade 8 is arranged on the stirring shaft 7. The stirring shaft 7 is fixedly sleeved with a plurality of connecting seats arranged at intervals up and down, and each connecting seat is circumferentially fixed with a plurality of stirring blades 8. The rotation of the stirring shaft 7 drives the plurality of connecting seats to rotate, and drives the plurality of stirring blades 8 to rotate, and then the stirring blades 8 stir the solution in the kettle body 2, effectively reducing the adhesion of diamond micropowder in the solution.
[0039] The ultrasonic component is used to emit ultrasonic waves into the kettle body 2. The ultrasonic component includes at least one ultrasonic generator 9. The ultrasonic generator 9 adopts an ultrasonic liquid processing device with a model of GBS-SCF30A. The lower end of the ultrasonic generator 9 penetrates the cover body 3 and extends into the kettle body 2. It is used to emit ultrasonic waves to the liquid in the kettle body 2 to further reduce the adhesion between the diamond micropowders.
[0040] The dosing assembly is used to deliver medicine to the kettle body 2. The dosing assembly includes a medicine feed pipe 10. The medicine feed pipe 10 penetrates the cover body 3 and extends into the kettle body 2. The medicine is delivered to the kettle body 2 through the medicine feed pipe 10. The medicine feed pipe 10 is connected to a delivery pump. The delivery pump is a diaphragm pump. The medicine feed pipe 10 is provided in plurality. The plurality of medicine feed pipes 10 are circumferentially arranged on the cover body 3. The plurality of medicine feed pipes 10 are connected to the delivery pump together. Through the provision of the plurality of medicine feed pipes 10, the medicine enters the kettle body 2 from a plurality of different positions and diffuses rapidly in the kettle body 2. The delivery pump is connected to a storage box. The storage box is provided with No. 2 medicine. The kettle body 2 After the internal solution is prepared, the cover 3 is closed, the stirring blade 8 and the ultrasonic emission position of the ultrasonic generator 9 are immersed in the solution, the first motor 6 is started, the stirring blade 8 is driven to stir the solution and the diamond powder therein, the ultrasonic generator 9 is started, and the ultrasonic power is set to 70% to 90% when in use, and ultrasonic waves are emitted into the solution, and then the delivery pump is started to deliver agent No. 2 to the kettle body 2, so that the chemical plating reaction starts, and at the same time, through the setting of multiple drug inlet pipes 10, the agent No. 2 quickly diffuses after entering the kettle body 2, and the delivery rate of the agent No. 2 is effectively controlled by the delivery pump, and the reaction rate in the kettle body 2 is controlled.
[0041] A discharge pipe 15 is fixedly provided at the lower end of the kettle body 2, and the discharge pipe 15 penetrates the outer layer and the inner layer and extends into the kettle body 2. A valve 16 is provided on the discharge pipe 15. After the chemical plating reaction is completed, the valve 16 is opened, and the solution and the diamond powder after the nickel plating are discharged from the kettle body 2 through the discharge pipe 15. The ammonia generated by the chemical plating reaction can be collected and transported to the absorption tower for treatment.
[0042] It should be noted that the capacity of the kettle body 2 in this embodiment is 100L, which can be further increased as needed.
[0043] When in use, firstly, the cover 3 is driven upward by the second motor 11, and then when the stirring shaft 7 and the stirring blades 8 and the ultrasonic generator 9 on it are all out of the kettle 2, the No. 1 agent is added to the kettle 2, and the diamond powder is added, and then the second motor 11 drives the cover 3 to descend until the cover 3 and the upper end of the kettle 2 are attached, and the first motor 6 and the ultrasonic generator 9 are started to stir the solution and emit ultrasonic waves into the kettle 2 to avoid the adhesion of the diamond powder during the chemical plating reaction. At the same time, hot oil is circulated into the gap between the outer layer and the inner layer through the feed box for oil bath heating to ensure that the temperature in the kettle 2 is 85°C to 95°C, and the delivery pump is started, and then the No. 2 agent is continuously delivered to the kettle 2 through multiple drug inlet pipes 10, so that the chemical nickel plating reaction starts, and the speed of delivering the No. 2 agent to the kettle 2 is adjusted at any time by the delivery pump to ensure that the reaction speed is uniform. After the chemical nickel plating of the diamond powder is completed, the liquid and the diamond powder that has completed the nickel plating are discharged through the discharge pipe 15.
[0044] Example 2 The present invention provides a diamond micropowder chemical nickel plating method, using the chemical plating reactor of embodiment 1, the chemical nickel plating method comprises the following steps: Step 1: Weigh 10,000 carats of diamond powder according to the measurement. 1 carat is equal to 0.2 g, so the diamond powder is 2,000 grams. Prepare reagent No. 1 and reagent No. 2. The total volume of reagent No. 1 and reagent No. 2 is 80L; The No. 1 reagent has a volume of 60 L and is prepared by mixing the following raw materials: 4900 g of nickel sulfate, 1460 g of sodium citrate, 200 ml of lactic acid, 100 ml of dispersant (F-350) and 6.2 liters of ammonia water, the solvent is water, and the amount of water added is such that the volume of the No. 1 reagent prepared after mixing all the raw materials is 60 L; The No. 2 reagent has a volume of 20 L and is prepared by mixing the following raw materials: 6750 g of sodium hypophosphite and 40 g of sodium hydroxide, the solvent is water, and the amount of water added is such that the volume of the No. 2 reagent prepared after mixing all the raw materials is 20 L; Step 2: Add agent No. 1 into kettle 2, and add diamond powder into kettle 2 at the same time. At the same time, the gap between the inner layer and the outer layer of kettle 2 is filled with oil to heat the liquid in kettle 2 to 90°C, turn on the ultrasonic generator power to 70%, stir the liquid in kettle 2 for 10 minutes with a stirring speed of 200 rpm, and slowly add agent No. 2 after stirring evenly. At this time, the stirring speed is adjusted to 250 rpm. Agent No. 2 is added to kettle 2 through the dosing component at a dosing speed of 30 ml / min, and then the dosing speed is increased by 8 ml / min every half an hour, and the stirring speed is increased by 50 rpm every half an hour. After the addition of agent No. 2, continue to stir and react for 30 minutes. After the reaction is completed, pour the liquid in kettle 2 into the container, precipitate for more than 30 minutes, pour out the supernatant, and avoid spilling and loss of powder. Then move the precipitated diamond powder to the cleaning area and wash it with clean water 5 times to obtain nickel-plated diamond powder.
[0045] Test the diamond powder after nickel plating. The particle size test report of diamond powder can be found in Figure 4 It can be seen that the D50 of diamond powder after nickel plating is 7.511μm, see SEM picture Figure 5 The indicators all meet the production requirements. The device and method can be used in large-scale production to improve production efficiency and reduce production costs.
[0046] Example 3 The method is basically the same as Example 2, except that, step 1: 15,000 carats of diamond powder are weighed, 1 carat equals 0.2 g, therefore, the diamond powder is 3,000 g, and reagent No. 1 and reagent No. 2 are prepared, and the total volume of reagent No. 1 and reagent No. 2 is 80 L; The No. 1 reagent has a volume of 60 L and is prepared by mixing the following raw materials: 7350 g of nickel sulfate, 2190 g of sodium citrate, 300 ml of lactic acid, 150 ml of dispersant (F-350) and 8.06 liters of ammonia water, the solvent is water, and the amount of water added is such that the volume of the No. 1 reagent prepared after mixing all the raw materials is 60 L; The volume of the No. 2 agent is 20L, and it is prepared by mixing the following raw materials: 10125 grams of sodium hypophosphite and 60 grams of sodium hydroxide, the solvent is water, and the amount of water added is such that the volume of the No. 2 agent prepared after mixing all the raw materials is 20L.
[0047] In step 2, the ultrasonic generator power is increased to 90%.
[0048] See the SEM image of diamond powder after nickel plating. Figure 6 .
[0049] Example 4 The method is basically the same as Example 2, except that in step 1, 25,000 carats of diamond powder are weighed, 1 carat equals 0.2 g, and therefore, the diamond powder is 5,000 g, and reagent No. 1 and reagent No. 2 are prepared, and the total volume of reagent No. 1 and reagent No. 2 is 100 L; The No. 1 reagent has a volume of 80 L and is prepared by mixing the following raw materials: 12250 g of nickel sulfate, 3650 g of sodium citrate, 250 ml of lactic acid, 250 ml of dispersant (F-350) and 15.5 liters of ammonia water, the solvent is water, and the amount of water added is such that the volume of the No. 1 reagent prepared after mixing all the raw materials is 80 L; The No. 2 reagent has a volume of 20 L and is prepared by mixing the following raw materials: 16875 g of sodium hypophosphite and 100 g of sodium hydroxide, the solvent is water, and the amount of water added is such that the volume of the No. 2 reagent prepared after mixing all the raw materials is 20 L; In step 2, the power of the ultrasonic generator is increased to 80%.
[0050] See the SEM image of diamond powder after nickel plating. Figure 7 .
[0051] from Figures 5 to 7 It can be seen that after adopting the chemical plating reactor and nickel plating method of the present invention, the dispersibility of diamond micropowder is better, and the plating leakage and agglomeration are reduced.
[0052] Before using the chemical plating reactor of the present invention, diamond micropowder is mixed with the required liquid medicine in a barrel, and the staff stirs it to obtain nickel-plated diamond micropowder, such as Figure 8 and Fig. 9 As shown in Figure 2, due to manual stirring, the stability of different batches is poor, such as Figure 8 The batch shown has incomplete plating and missing plating. Fig. 9 The batch shown had agglomerated particles.
[0053] The embodiments described above are only preferred embodiments of the present invention and are not intended to limit the scope of implementation of the present invention. Therefore, any equivalent changes or modifications made according to the structures, features and principles described in the patent scope of the present invention should be included in the scope of the patent application of the present invention.
Claims
1. A reaction kettle for chemical plating, characterized in that: The invention comprises a mounting frame (1), wherein a kettle body (2) and a cover body (3) are arranged on the mounting frame (1), wherein the kettle body (2) comprises an inner layer and an outer layer, wherein a gap is provided between the inner layer and the outer layer, wherein a circulation inlet (4) is provided at the lower end of the kettle body (2), and a circulation outlet (5) is provided at the upper end, wherein the circulation inlet (4) and the circulation outlet (5) are both connected to the gap between the inner layer and the outer layer, and wherein the circulation inlet (4) and the circulation outlet (5) are both connected to a feed box via a pipeline; The cover body (3) is slidably connected to the mounting frame (1) up and down, and a stirring component, an ultrasonic component and a dosing component are arranged on the cover body (3), the stirring component is used to stir the liquid in the kettle body (2), the ultrasonic component is used to emit ultrasonic waves into the kettle body (2), and the dosing component is used to transport medicine into the kettle body (2).
2. A chemical plating reactor according to claim 1, characterized in that: The stirring assembly comprises a first motor (6), a stirring shaft (7) and a stirring blade (8); the first motor (6) is fixedly arranged above the cover body (3); the output end of the first motor (6) is fixedly connected to the stirring shaft (7); the lower end of the stirring shaft (7) extends to the lower part of the kettle body (1); and the stirring blade (8) is arranged on the stirring shaft (7).
3. A chemical plating reactor according to claim 1, characterized in that: The ultrasonic component comprises at least one ultrasonic generator (9), the lower end of which penetrates the cover body (3) and extends into the kettle body (2), and is used to emit ultrasonic waves to the liquid in the kettle body (2).
4. A chemical plating reactor according to claim 1, characterized in that: The medicine adding assembly comprises a medicine feeding pipe (10), the medicine feeding pipe (10) passes through the cover body (3) and extends into the kettle body (2), the medicine feeding pipe (10) is connected to a delivery pump, and the delivery pump is connected to a storage box, and the storage box is provided with medicine.
5. A chemical plating reactor according to claim 4, characterized in that: The drug inlet pipes (10) are provided in plurality, the plurality of drug inlet pipes (10) are circumferentially arranged on the cover body (3), and the plurality of drug inlet pipes (10) are commonly connected to the delivery pump.
6. A chemical plating reactor according to claim 1, characterized in that: The mounting frame (1) comprises a support plate and a vertical pole, the vertical pole being fixedly arranged above the support plate, a second motor (11) being fixedly arranged on the upper side of the vertical pole, one side of the vertical pole being fixedly connected to the kettle body (2), the support plate and the kettle body (2) corresponding to each other up and down, a slide groove (12) being downwardly provided at the upper end of the vertical pole, an output end of the second motor (11) being fixedly connected to a screw rod (13), the screw rod (13) extending into the slide groove (12), a mounting seat (14) being slidably arranged in the slide groove (12), the screw rod (13) being threadedly connected to the mounting seat (14), the mounting seat (14) extending out from one side of the vertical pole and fixedly connected to the cover body (3).
7. A chemical plating reactor according to claim 1, characterized in that: A discharge pipe (15) is fixedly arranged at the lower end of the kettle body (2); the discharge pipe (15) penetrates the outer layer and the inner layer and extends into the kettle body (2); a valve (16) is arranged on the discharge pipe (15).
8. A diamond powder chemical nickel plating method, characterized in that: Using the chemical plating reactor according to any one of claims 1 to 7, the chemical nickel plating method comprises the following steps: Step 1: Weigh diamond micropowder according to the measurement to prepare reagent No. 1 and reagent No. 2; The No. 1 reagent is prepared by mixing the following raw materials: nickel sulfate, sodium citrate, lactic acid, dispersant and ammonia water, and the solvent is water; The No. 2 agent is prepared by mixing the following raw materials: sodium hypophosphite and sodium hydroxide, and the solvent is water; The ratio of the total volume of diamond powder to the No. 1 agent and the No. 2 agent is (25-65) g:1 L, and the volume ratio of the No. 1 agent to the No. 2 agent is (1-4):1; Step 2: Add reagent No. 1 into the kettle (2), and at the same time add diamond powder into the kettle (2), heat the kettle (2) to a predetermined temperature, the predetermined temperature being 85° C. to 95° C., turn on the ultrasonic generator (9) and turn on the stirring component to stir the liquid in the kettle (2), and after stirring evenly, slowly add reagent No. 2, and add reagent No. 2 into the kettle (2) through the dosing component, the dosing speed is 30 to 80 ml / min, and the dosing time is 2.5 to 3 hours. After the addition of reagent No. 2 is completed, continue stirring and reacting for 20 to 40 minutes; after the reaction is completed, precipitate the liquid in the kettle (2), wash it, and obtain the nickel-plated diamond powder.
9. A diamond powder chemical nickel plating method according to claim 8, characterized in that: The mass of the diamond powder is 2000-5000 g, the sum of the volumes of agent No. 1 and agent No. 2 is 80-100 L, and the volume ratio of agent No. 1 to agent No. 2 is (3-4):1; The No. 1 agent is prepared by mixing the following raw materials: 4900-12250 g of nickel sulfate, 1460-3650 g of sodium citrate, 200-300 ml of lactic acid, 100-250 ml of dispersant and 6.2-15.5 liters of ammonia water, the solvent is water, wherein the amount of water added is such that the volume ratio of the No. 1 agent to the No. 2 agent is (3-4):1; The No. 2 agent is prepared by mixing the following raw materials: 6750-16875 grams of sodium hypophosphite and 40-100 grams of sodium hydroxide, and the solvent is water, wherein the amount of water added is such that the volume ratio of the No. 1 agent to the No. 2 agent is (3-4):
1.
10. The method for chemical nickel plating of diamond powder according to claim 8, characterized in that: In step 2, the predetermined temperature is 90° C. and the stirring speed is 200 to 600 rpm; The mass of the diamond powder is 2000g, the volume of the No. 1 reagent is 60L, and the volume of the No. 2 reagent is 20L; The No. 1 reagent is prepared by mixing the following raw materials: 4900 g of nickel sulfate, 1460 g of sodium citrate, 200 ml of lactic acid, 100 ml of dispersant and 6.2 liters of ammonia water, the solvent is water, and the amount of water added makes the volume of the No. 1 reagent 60 L; The No. 2 agent is prepared by mixing the following raw materials: 6750 grams of sodium hypophosphite and 40 grams of sodium hydroxide, and the solvent is water, wherein the amount of water added makes the volume of the No. 2 agent 20L.