NiB binary alloy raw material mixing device and method

Abstract

The invention relates to the technical field of alloy raw material mixing, and discloses a NiB binary alloy raw material mixing device, the raw material mixing device comprises a reaction kettle, a stirrer and a filler port, the stirrer is installed at the bottom of the reaction kettle, stirring and mixing are generated in the reaction kettle, the filler port is formed in the side wall of the reaction kettle, and the filler port is communicated with the stirrer. A temperature control assembly capable of switching heating and cooling is arranged on the outer side of the reaction kettle, a temperature control system capable of switching a circulating medium is constructed on the outer side of the reaction kettle on the basis of the jacket, and compared with a single temperature control medium in conventional equipment, a very stable effect can be achieved during temperature control; the chemical nickel plating process requiring accurate temperature change is more friendly, in addition, the setting form that the jacket wraps the medium for temperature conduction is adopted, so that the acting part is very uniform during temperature control, more accurate temperature control can be provided, and good product production is ensured.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of alloy raw material mixing, in particular to a NiB binary alloy raw material mixing device. BACKGROUND

[0002] Ni-P alloy generally refers to a plating layer formed by electroless nickel plating, and raw material mixing is a core link in the electroless nickel plating process and directly determines the quality of the plating layer, the deposition rate and the stability of the solution.

[0003] During Ni-P alloy raw material mixing, precise temperature control is required, and the performance of the Ni-P alloy plating layer, such as hardness, corrosion resistance and magnetic performance, is directly determined by the phosphorus (P) content, and the phosphorus content is extremely sensitive to temperature. The medium temperature range (about 88 DEG C): usually a medium phosphorus (6-9% P) plating layer is obtained, and the best balance between corrosion resistance and hardness is achieved, and the application is the most extensive; The low temperature range (<80 DEG C): tends to form a high phosphorus (10-12% P) plating layer, non-magnetic, excellent corrosion resistance, but low hardness; The high temperature range (> 90 DEG C): tends to form a low phosphorus (2-5% P) plating layer, high hardness, good wear resistance, but poor corrosion resistance; In addition, the chemical plating process itself is a strong exothermic reaction, and if there is no effective cooling, the plating bath temperature will continue to rise, resulting in faster and faster reaction and more and more heat release, eventually falling into a vicious cycle and causing spontaneous decomposition of the plating solution.

[0004] The existing mixing reaction equipment has certain improvement space in temperature regulation, and usually adopts a single temperature control medium, and the covered parts are not uniform during temperature control, which can easily lead to inaccurate temperature control, so that the phosphorus content of the same batch or even different parts of the same workpiece is different, resulting in inconsistent and unreliable product performance. SUMMARY

[0005] The application provides a NiB binary alloy raw material mixing device, which solves the technical problems of uneven temperature control coverage and product performance imbalance caused by single temperature control medium in the related art.

[0006] The application provides a NiB binary alloy raw material mixing device, which comprises a reaction kettle, a stirrer and a filling port, the stirrer is installed at the bottom of the reaction kettle, stirring and mixing are generated in the reaction kettle, the filling port is arranged on the side wall of the reaction kettle, and a heating and cooling switchable temperature control assembly is arranged outside the reaction kettle. The temperature control assembly comprises a jacket, which is fixedly sleeved around the outer periphery of the reaction kettle to form a cavity for the temperature control medium to pass through on the outer wall of the reaction kettle, the top of the jacket is connected with the liquid inlet pipe, and the bottom of the jacket is connected with the liquid outlet pipe, the outer portion of the reaction kettle is provided with a heat conduction supply end and a cooling supply end, and the liquid inlet pipe and the liquid outlet pipe are both communicated with the heat conduction supply end and the cooling supply end through three-way valves respectively.

[0007] As a further scheme of the present application, the heat conduction supply end comprises a heat conduction oil boiler, a heat conduction oil storage tank and an oil pump, the top of the three-way valve on one side of the liquid inlet pipe is connected with the heat conduction oil boiler, the top of the three-way valve on one side of the liquid outlet pipe is connected with the heat conduction oil storage tank, and the pipeline connected between the heat conduction oil boiler and the heat conduction oil storage tank is provided with the oil pump, so that the heat conduction oil is pushed from the heat conduction oil storage tank to the heat conduction oil boiler.

[0008] As a further scheme of the present application, the cooling supply end comprises a cold water machine, a cooling tower and a water pump, the bottom of the three-way valve on one side of the liquid inlet pipe is connected with the cold water machine, the bottom of the three-way valve on one side of the liquid outlet pipe is connected with the cooling tower, and the pipeline connected between the cold water machine and the cooling tower is provided with the water pump, so that the cooling water is pushed from the cooling tower to the cold water machine.

[0009] As a further scheme of the present application, the top of the reaction kettle is provided with a pushing assembly matched with the temperature control assembly, the pushing assembly comprises an electric push rod and a pressing plate, the electric push rod is fixedly installed on the top of the reaction kettle, the pressing plate is slidably arranged in the jacket, and the output end of the electric push rod is fixedly connected with the pressing plate.

[0010] As a further scheme of the present application, the pressing plate is in the form of a ring and has a cross section equal to that of the cavity enclosed by the jacket and the outer wall of the reaction kettle.

[0011] A method for mixing NiB binary alloy raw materials, comprising the following steps: S1, water injection and preheating: a certain amount of deionized water is injected into the reaction kettle from the filling port, the stirrer and the temperature control assembly are started, and heating is performed until the set temperature (55°C) is reached; S2, raw material addition: solid complexing agent is added through the filling port, nickel salt is dissolved, pre-diluted stabilizer solution is added, and sodium hypophosphite solution is dissolved in advance for reduction reaction; S3, constant volume and pH coarse adjustment: deionized water is supplemented to the final volume, and ammonia water is added to the mixed solution to reach the target pH range; S4, aging: the temperature control assembly raises the solution to the working temperature (88°C), and the stirring is continued at this temperature for a period of time; S5, sampling detection: the plating solution after mixing is sampled and analyzed, and the plating solution is adjusted to the preparation requirements according to the analysis results.

[0012] In step S2, lactic acid and citric acid are slowly added as complexing agents and acetic acid and boric acid are slowly added as buffering agents under stirring.

[0013] In step S2, the sodium hypophosphite is dissolved in an appropriate amount of warm water (<60°C) before being added.

[0014] In step S3, the pH of the plating solution is accurately adjusted to 4.6-5.2 using ammonia water using a pH meter.

[0015] In step S4, the prepared plating solution is subjected to circulating filtration using a filter with a pore size of 1-5 microns to remove solid impurities generated during the reaction.

[0016] The beneficial effects of the present application are: The present application uses a jacket on the outside of the reaction kettle to build a temperature control system that can switch the circulating medium. Compared with the single temperature control medium in conventional equipment, it can achieve very stable results when temperature control is performed, and is more friendly to the chemical nickel plating process that requires accurate temperature changes. In addition, the setting form of the jacket wrapped medium for temperature conduction makes the action site very uniform when temperature control is performed, providing more accurate temperature control and ensuring good production.

[0017] In the switching stage, the electric push rod pushes the pressing plate, which can speed up the switching speed and quickly empty the original medium in the jacket, and the blocking of the pressing plate can minimize the mixing of cooling water and heat conducting oil in the jacket to avoid interference with temperature control. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 is a first perspective view of the overall structure of the NiB binary alloy raw material mixing device according to the present application; Figure 2 is a second perspective view of the overall structure of the NiB binary alloy raw material mixing device according to the present application; Figure 3 is a schematic view of the overall structure of the temperature control assembly in the NiB binary alloy raw material mixing device according to the present application; Figure 4 is a schematic view of the detailed structure of the temperature control assembly in the NiB binary alloy raw material mixing device according to the present application; Figure 5 is a first state schematic view of the propulsion assembly in the NiB binary alloy raw material mixing device according to the present application; Figure 6 is a second state schematic view of the propulsion assembly in the NiB binary alloy raw material mixing device according to the present application.

[0019] In the drawings: 1, reactor; 2, stirrer; 3, filler port; 4, temperature control assembly; 41, jacket; 42, liquid inlet pipe; 43, liquid outlet pipe; 44, three-way valve; 451, heat conduction oil boiler; 452, heat conduction oil storage tank; 453, oil pump; 461, water chiller; 462, cooling tower; 463, water pump; 5, propulsion assembly; 51, electric push rod; 52, pressing plate. DETAILED DESCRIPTION

[0020] The subject matter described herein will now be discussed with reference to example implementations. It should be understood that discussions of these implementations are merely provided to enable those skilled in the art to better understand so as to be able to implement the subject matter described herein, and variations of elements discussed can be made by one skilled in the art, without departing from the scope of the present specification. Various examples can omit, substitute, or add various processes or components in addition to those described or in place of those described. Also, some of the described features can be combined in a single example.

[0021] The application discloses a NiB binary alloy raw material mixing device, as shown in the figure, comprising a reactor 1, a stirrer 2 and a filler port 3, the bottom of the reactor 1 is provided with the stirrer 2, and stirring and mixing are generated in the reactor 1, the filler port 3 is arranged on the side wall of the reactor 1, and a temperature control assembly 4 capable of switching heating and cooling is arranged outside the reactor 1. Figure 1 Figure 6 As shown in the figure, comprising a reactor 1, a stirrer 2 and a filler port 3, the bottom of the reactor 1 is provided with the stirrer 2, and stirring and mixing are generated in the reactor 1, the filler port 3 is arranged on the side wall of the reactor 1, and a temperature control assembly 4 capable of switching heating and cooling is arranged outside the reactor 1. The temperature control assembly 4 comprises a jacket 41, the jacket 41 is fixedly sleeved around the outer periphery of the reactor 1, a cavity for passing a temperature control medium is formed on the outer wall of the reactor 1, the top of the jacket 41 is connected with a liquid inlet pipe 42, and the bottom of the jacket 41 is connected with a liquid outlet pipe 43, a heat conduction supply end and a cooling supply end are arranged outside the reactor 1, and the liquid inlet pipe 42 and the liquid outlet pipe 43 are respectively communicated with the heat conduction supply end and the cooling supply end through three-way valves 44.

[0022] Temperature control during the mixing reaction can be divided into a heating stage and a cooling stage. In the heating stage, the three-way valves 44 are controlled to switch to communication between the heat conduction supply end and the jacket 41, and circulation of heat conduction oil in the cavity is established. Specifically: The heat conduction supply end comprises a heat conduction oil boiler 451, a heat conduction oil storage tank 452 and an oil pump 453, the top of the three-way valve 44 on one side of the liquid inlet pipe 42 is connected with the heat conduction oil boiler 451, the top of the three-way valve 44 on one side of the liquid outlet pipe 43 is connected with the heat conduction oil storage tank 452, and the oil pump 453 is arranged on the pipeline connected between the heat conduction oil boiler 451 and the heat conduction oil storage tank 452, and the heat conduction oil is pushed from the heat conduction oil storage tank 452 to the heat conduction oil boiler 451.

[0023] ​The heat conducting oil boiler 451 inputs the heat conducting oil heated to the suitable temperature from the liquid inlet pipe 42 and outputs from the liquid outlet pipe 43, and is introduced into the heat conducting oil storage tank 452, and the oil pump 453 is turned on to establish the heating cycle of "the heat conducting oil boiler 451 - the jacket 41 - the heat conducting oil storage tank 452", and provide the temperature rising condition for the mixed reaction.

[0024] In the cooling stage, the three-way valve 44 is controlled to switch to the cooling supply end in communication with the jacket 41 to establish the circulation of the cooling water in the cavity, and specifically: The cooling supply end comprises a water chiller 461, a cooling tower 462 and a water pump 463, the bottom of the three-way valve 44 on one side of the liquid inlet pipe 42 is connected to the water chiller 461, the bottom of the three-way valve 44 on one side of the liquid outlet pipe 43 is connected to the cooling tower 462, and the water pump 463 is arranged on the pipeline connected between the water chiller 461 and the cooling tower 462 to push the cooling water from the cooling tower 462 to the water chiller 461.

[0025] The water chiller 461 inputs the cooling water from the liquid inlet pipe 42 and outputs from the liquid outlet pipe 43, and is introduced into the cooling tower 462, and the water pump 463 is turned on to establish the cooling cycle of "the water chiller 461 - the jacket 41 - the cooling tower 462", and provide the temperature lowering condition for the mixed reaction.

[0026] According to the above implementation, the temperature control system capable of switching the circulating medium (heat conducting oil and cooling water) is constructed based on the jacket 41 outside the reaction kettle 1, compared with the single temperature control medium in the conventional equipment, the temperature control can be very stable, and the process of electroless nickel plating requiring accurate temperature change is more friendly. In addition, the jacket 41 wraps the medium for temperature conduction, so that the action part is very uniform during temperature control, and more accurate temperature control can be provided to ensure good products.

[0027] It should be noted that when the above implementation is adopted, the cooling water and the heat conducting oil will inevitably mix in the common temperature control action part (the jacket 41). In order to solve the adverse effects caused by the mixing, the following implementation is carried out: The top of the reaction kettle 1 is provided with a pushing assembly 5 matched with the temperature control assembly 4, the pushing assembly 5 comprises an electric push rod 51 and a pressing plate 52, the electric push rod 51 is fixedly installed on the top of the reaction kettle 1, the pressing plate 52 is slidingly arranged in the jacket 41, and the output end of the electric push rod 51 is fixedly connected with the pressing plate 52.

[0028] In the switching stage, the electric push rod 51 pushes the pressing plate 52, which can accelerate the switching speed and quickly empty the original medium in the jacket 41, and the blocking of the pressing plate 52 can minimize the mixing of the cooling water and the heat conducting oil in the jacket 41 to avoid interference with the temperature control action.

[0029] The pressing plate 52 is annular, and the cross section of the cavity surrounded by the jacket 41 and the outer wall of the reactor 1 is equal to that of the pressing plate 52.

[0030] A method for mixing NiB binary alloy raw materials, comprising the following steps: S1, water injection and preheating: quantitative deionized water is injected into the reactor 1 from the filling port 3, the stirrer 2 and the temperature control assembly 4 are started, and heating is performed to a set temperature (55°C); S2, raw material addition: solid complexing agent is added through the filling port 3, nickel salt solution is added, pre-diluted stabilizer solution is added, and pre-dissolved sodium hypophosphite solution is added for reduction reaction; S3, constant volume and pH coarse adjustment: deionized water is supplemented to the final volume, and ammonia water is added to the mixed solution to the target pH range; S4, aging: the temperature control assembly 4 raises the solution to the working temperature (88°C), and continues to stir at this temperature for a period of time; S5, sampling detection: the plating solution after mixing is sampled and analyzed, and the plating solution is adjusted to the preparation requirements according to the analysis results.

[0031] The above describes the embodiments of the present application, but the embodiments are not limited to the above specific embodiments, and the above specific embodiments are only illustrative and not restrictive. Those skilled in the art can also make more forms of equivalent embodiments under the inspiration of the embodiments, which are all within the protection scope of the embodiments.

Claims

1. A NiB binary alloy raw material mixing device, comprising a reactor (1), a stirrer (2), and a packing port (3), wherein the stirrer (2) is installed at the bottom of the reactor (1) to generate stirring and mixing in the reactor (1), and the packing port (3) is opened on the side wall of the reactor (1), characterized in that, The reaction kettle (1) is provided with a heating and cooling switchable temperature control assembly (4) outside; The temperature control assembly (4) comprises a jacket (41), the jacket (41) is fixedly sleeved around the outer periphery of the reaction kettle (1), and a cavity for passing the temperature control medium is formed on the outer wall of the reaction kettle (1), the top of the jacket (41) is connected with a liquid inlet pipe (42), and the bottom is connected with a liquid outlet pipe (43), the outer part of the reaction kettle (1) is provided with a heat conduction supply end and a cooling supply end, and the liquid inlet pipe (42) and the liquid outlet pipe (43) are respectively communicated with the heat conduction supply end and the cooling supply end through three-way valves (44).

2. The NiB binary alloy raw material mixing device according to claim 1, characterized in that, The heat conduction supply end comprises a heat conduction oil boiler (451), a heat conduction oil storage tank (452) and an oil pump (453), the top of the three-way valve (44) on one side of the liquid inlet pipe (42) is connected with the heat conduction oil boiler (451), the top of the three-way valve (44) on one side of the liquid outlet pipe (43) is connected with the heat conduction oil storage tank (452), and an oil pump (453) is arranged on the pipeline connected between the heat conduction oil boiler (451) and the heat conduction oil storage tank (452), and the heat conduction oil is pushed from the heat conduction oil storage tank (452) to the heat conduction oil boiler (451).

3. The NiB binary alloy raw material mixing device according to claim 1, characterized in that, The cooling supply end comprises a water chiller (461), a cooling tower (462) and a water pump (463), the bottom of the three-way valve (44) on one side of the liquid inlet pipe (42) is connected with the water chiller (461), the bottom of the three-way valve (44) on one side of the liquid outlet pipe (43) is connected with the cooling tower (462), and a water pump (463) is arranged on the pipeline connected between the water chiller (461) and the cooling tower (462), and the cooling water is pushed from the cooling tower (462) to the water chiller (461).

4. The NiB binary alloy raw material mixing device according to claim 2, characterized in that, The top of the reaction kettle (1) is provided with a pushing assembly (5) matched with the temperature control assembly (4), the pushing assembly (5) comprises an electric push rod (51) and a pressing plate (52), the electric push rod (51) is fixedly installed on the top of the reaction kettle (1), and the pressing plate (52) is slidably arranged in the jacket (41), and the output end of the electric push rod (51) is fixedly connected with the pressing plate (52).

5. The NiB binary alloy raw material mixing device according to claim 4, characterized in that, The pressing plate (52) is annular, and the cross section of the cavity surrounded by the jacket (41) and the outer wall of the reaction kettle (1) is equal to that of the pressing plate (52).

6. A method for mixing raw materials of a NiB binary alloy, the raw material mixing device for a NiB binary alloy according to any one of claims 1 to 5, characterized by, The method comprises the following steps: S1, water injection and preheating: a certain amount of deionized water is injected into the reaction kettle (1) from the filling port (3), the stirrer (2) and the temperature control assembly (4) are started, and heating is carried out until the set temperature (55℃) is reached; S2, raw material addition: solid complexing agent is added through the filling port (3) in sequence, nickel salt solution is added, pre-diluted stabilizer solution is added, and sodium hypophosphite solution is added for reduction reaction; S3, constant volume and pH coarse adjustment: deionized water is supplemented to the final volume, and ammonia water is added to the mixed solution to reach the target pH range; S4, aging: the temperature control assembly (4) raises the solution to the working temperature (88°C), and continues to stir at this temperature for a period of time; S5, sampling detection: the plating solution after mixing is sampled and analyzed, and the plating solution is adjusted to the preparation requirements according to the analysis results.

7. The method of claim 6, wherein the NiB binary alloy raw material is mixed by a method of, In step S2, lactic acid and citric acid are added slowly as complexing agents and acetic acid and boric acid are added slowly as buffering agents under stirring.

8. The method of claim 6, wherein the NiB binary alloy raw material is mixed by using a ball mill. In step S2, the sodium hypophosphite is dissolved in a suitable amount of warm water (<60°C) before being added.

9. The method of claim 6, wherein the NiB binary alloy raw material is mixed by using a ball mill. In step S3, the pH of the plating solution is adjusted to 4.6-5.2 using ammonia.

10. The method of claim 6, wherein the NiB binary alloy raw material is mixed by using a ball mill. In step S4, the prepared plating solution is filtered using a filter with a pore size of 1-5 microns to remove solid impurities generated during the reaction.

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