Device and method for quantitatively detecting content of nickel carbonyl in rectification residual liquid

Abstract

The invention relates to the technical field of metallurgy, in particular to a device and method for quantitatively detecting the content of nickel carbonyl in rectification residual liquid, and aims to solve the problem that the purity of nickel carbonyl is limited due to the fact that the current detection situation that nickel carbonyl can be indirectly and qualitatively judged only according to carbon monoxide generated through decomposition of nickel carbonyl for a long time at present. According to the device and the method, the rectification raffinate enters the ice water liquid seal tank in advance, so that the rectification raffinate is prevented from contacting with air, leaking out and being decomposed into CO to harm the health of personnel; meanwhile, the liquid level drop volume number of the rectification residual liquid can be directly read through the metering transparent U-shaped pipe with scales, metering is accurate, and the multi-metal recovery rate can be further calculated conveniently; the metal powder after reaction is collected by using a ground combustion bottle with the same caliber as a spray head, the product in the combustion bottle is subjected to acid dissolution and repeated washing, the contents of nickel, iron and cobalt in the residual liquid are directly detected, and an accurate metal quantitative result can be obtained by combining the pre-read volume of the rectification residual liquid; therefore, the purpose of directly obtaining quantitative detection data of the metal in the rectification residual liquid is achieved.

Description

Technical Field

[0001] The present invention relates to the technical field of metallurgy, and particularly relates to a device and method for quantitatively detecting the content of nickel carbonyl in rectification residue. Background Art

[0002] Nickel carbonyl was invented by C. Langer and L. Mond in 1898. By using the reaction of metals such as nickel and iron with CO to generate gaseous carbonyl complexes, in essence, nickel in various nickel-containing materials is highly selectively extracted once to become a highly pure gaseous metal complex, and then it is thermally decomposed to separate high-purity metal products and carbon monoxide returned to the process system. The high-purity nickel powder prepared by this process has unique properties and has been widely used in fields such as batteries, national defense, aerospace, chemical industry, atomic energy, electronic communication, and high-performance magnetic materials. Nevertheless, during the carbonylation reaction process, the properties of the same-group metals iron, cobalt, and nickel element are similar, and a small amount will react and enter the carbonylation complex. If the rectification separation is incomplete, it will seriously affect the purity and grade of nickel powder during subsequent decomposition. Therefore, it is particularly important to study the actual recovery rates of various metals during the rectification process in the laboratory, which determines whether it is necessary to adjust the rectification process parameters to further improve the refined and purified requirements. For a long time, due to the highly toxic and easily decomposable characteristics of nickel carbonyl, most detection methods either indirectly qualitatively determine nickel carbonyl by detecting the CO concentration in the working environment, or estimate the situation of nickel carbonyl by measuring the indicators of nickel powder at the end of the process. The former cannot accurately measure the CO concentration data, and the latter involves relatively complex process parameters of the thermal decomposition process, making it difficult to directly and timely measure the content of nickel carbonyl in the rectification residue. Therefore, the current detection means for liquid nickel carbonyl still have the problem of low accuracy. Summary of the Invention

[0003] The present invention provides a device and method for quantitatively detecting the content of nickel carbonyl in rectification residue to solve the problems existing in the above background.

[0004] To achieve the above object, the present invention adopts the following technical solutions: A device for quantitatively detecting the content of nickel carbonyl in rectification residue includes a liquid seal tank. The top of the liquid seal tank is communicated with a rectification residue inlet. The side of the rectification residue inlet is provided with an ice water inlet. The bottom of the liquid seal tank is communicated with a metering transparent U-shaped tube, and an electronic ignition nozzle is connected to the end of the metering transparent U-shaped tube.

[0005] Further, a liquid inlet pipe is provided in the rectification residue inlet, and a three-way valve is provided on the liquid inlet pipe.

[0006] Further, a stop valve is provided at the liquid outlet of the bottom of the liquid seal tank, and the stop valve is connected to the metering transparent U-shaped tube.

[0007] It also includes a method for quantitatively detecting the content of nickel carbonyl in the rectification residue, comprising the following steps: Step 1: Utilize the density difference between the ice water and nickel carbonyl in the liquid seal tank. First, add ice water to the liquid seal tank to a height of 20 mm - 30 mm, allowing the rectification residue to safely enter the liquid seal tank without contacting air. Then, use a three-way valve to blow air through the pipeline to ensure that the rectification residue has no contact with air.

[0008] Step 2: Then, control the rectification residue to fill the metering transparent U-shaped tube to the zero scale line, facilitating the reading of the liquid level change after combustion.

[0009] Step 3: Ignite with an electronic ignition nozzle, and completely collect the combustion products into a combustion bottle with the same caliber.

[0010] Step 4: Then, repeatedly wash the combustion bottle with hydrochloric acid 3 - 4 times, combine the washing solutions, use atomic absorption to test the nickel and iron contents, and calculate the contents of nickel and iron based on the drop in the liquid level of the metering transparent U-shaped tube, thereby calculating the recovery rate of nickel carbonyl.

[0011] The present invention has the following beneficial effects: The device of the present invention has a simple structure and low cost, is more accurate than the previous method of indirectly detecting nickel carbonyl through CO, and is safer and more user-friendly for operators. When the present invention is used for detection, the rectification residue first enters the ice water liquid seal tank, avoiding its contact with air and leakage and decomposition to generate CO, which is harmful to the health of test personnel. When the present invention is used for detection, the rectification residue can directly read the volume of the liquid level drop through the graduated U-shaped conduit, with accurate measurement, facilitating the calculation of the recovery rate of multiple metals in the next step. When the present invention is used for detection, a ground glass combustion bottle with the same caliber as the nozzle is used to collect the metal powder after the reaction, and the products in the combustion bottle are acid-dissolved and repeatedly washed to directly detect the nickel, iron, and cobalt contents in the residue. Combining with the previous volume of the rectification residue, accurate metal quantitative results can be obtained.

[0012] The present invention is an effective, safe, and direct solution for determining the nickel-based and impurity element contents in the rectification residue, which can be widely used in the laboratory research of nickel carbonyl and the optimization and adjustment of production line parameters. Moreover, a small amount of rectification residue is synchronously extracted for detection after the rectification process, providing relatively direct and accurate quantitative experimental data for the metal recovery rate in the rectification process, and providing reliable technical support for the metal recovery rate of the rectification process and the subsequent material purification in the laboratory research. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0014] The meanings of the reference numerals are as follows: 1. Three-way valve; 2. Globe valve; 3. Liquid seal tank; 4. Entrance for rectification residue liquid; 5. Entrance for ice water; 6. Measuring transparent U-shaped tube; 7. Electronic ignition nozzle; 8. Liquid inlet pipe. Detailed implementation manners

[0015] The present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0016] As Figure 1 shown, a device for quantitatively detecting the content of nickel carbonyl in rectification residue liquid includes a liquid seal tank 3. The top of the liquid seal tank 3 is communicated with an entrance 4 for rectification residue liquid. A side part of the entrance 4 for rectification residue liquid is provided with an entrance 5 for ice water. The bottom of the liquid seal tank 3 is communicated with a measuring transparent U-shaped tube 6, and an end of the measuring transparent U-shaped tube 6 is connected with an electronic ignition nozzle 7. An inlet pipe 8 is arranged in the entrance 4 for rectification residue liquid, and a three-way valve 1 is arranged on the inlet pipe 8. A globe valve 2 is arranged at an outlet of the bottom of the liquid seal tank 3, and the globe valve 2 is connected with the measuring transparent U-shaped tube 6.

[0017] The size of the liquid seal tank 3 is a stainless steel cylinder with a diameter of φ50 - 100 mm and equipped with a liquid level gauge. There are two openings on the upper cover. The center is an entrance 4 for rectification residue liquid with a diameter of φ10 mm and an insertion depth of 80 mm. The other is an entrance 5 for ice water with a diameter of φ10 mm and an insertion depth of 30 mm. A central outlet is left on the lower bottom cover, and a globe valve 2 is connected at the outlet to control the flow rate of the rectification residue liquid entering the measuring transparent U-shaped tube 6. The combustion bottle is an inverted 125 mL brown quartz ground joint bottle. The inner diameter of the bottle mouth is 31 mm, which is the same as the outer diameter of the electronic ignition nozzle 7, and the nozzle can just be clamped into the bottle mouth of the combustion bottle to avoid the leakage of metal powder after combustion decomposition.

[0018] When detecting the components of the rectification residue liquid, first, close the three-way valve 1 and the globe valve 2. Add a 0 °C ice water mixture to the liquid seal tank 3 through the entrance 5 for ice water until it reaches 50 mm in the liquid seal tank 3. Then, open the three-way valve 1. The rectification residue liquid enters the liquid seal tank 3 filled with ice water through the entrance 4 for rectification residue liquid. When the liquid level in the storage tank reaches two-thirds, close the three-way valve 1, and then open the globe valve 2 to make the mixed rectification residue liquid enter the measuring transparent U-shaped tube 6. When the liquid level shows zero position on the left straight tube scale, close the globe valve 2, and open the electronic ignition nozzle 7 device. Invert the combustion bottle above the nozzle. After the flame burns for a certain time, the air in the bottle is consumed and it goes out naturally. Remove the inverted combustion bottle, wash the combustion bottle with hydrochloric acid three times repeatedly, combine the washing solutions, use atomic absorption to test the nickel and iron contents, and calculate the content of nickel and iron in the material according to the liquid level drop amount, so as to calculate the recovery rate of nickel carbonyl.

[0019] When detecting the components of the rectification residue liquid, it is achieved through the following specific steps: First, close the stop valve 2, connect the three-way valve 1 to the atmosphere, and add ice water into the liquid seal tank 3 through the ice water inlet 5 until it reaches 30 mm; then turn the three-way valve 1 to the carbonyl nickel raw material, and the material enters the liquid seal tank 3 filled with ice water. When the liquid level rises to 45 mm, turn the three-way valve 1 to the air direction, and use the air flow to blow the residual liquid in the pipe into the liquid seal tank 3; then open the stop valve 2, and the rectification residue liquid at the lower part of the liquid seal tank 3 enters the metering transparent U-shaped tube 6. When the liquid level shows the zero position of the left straight tube scale, close the stop valve 2; then weigh the brown combustion bottle and place it upside down above the electronic ignition nozzle 7; then turn on the electronic ignition nozzle 7 device in the ventilation device. The flame burns for a certain period of time. After the air in the bottle is burned out, it will go out by itself. Immediately cover the combustion bottle after removing it, and weigh it after cooling; then open the stop valve 2 again to lower the liquid level in the liquid seal tank 3 below 30 mm, and part of the water also enters the metering transparent U-shaped tube 6. At this time, it can be observed that there is an interface between two liquid phases in the metering transparent U-shaped tube 6. Ensure that the rectification residue liquid in the liquid seal tank 3 completely flows into the metering transparent U-shaped tube 6, and close the stop valve 2; then ignite again, place another combustion bottle upside down, and ignite the residual liquid in the metering transparent U-shaped tube 6 in the ventilation device. Burn until the ice water in the liquid seal tank 3 drops to the position of the electronic ignition nozzle 7, and the flame goes out naturally; finally, repeatedly wash the first combustion bottle with dilute hydrochloric acid three times, combine the solutions, measure the nickel, iron, and cobalt contents in it by atomic absorption, and calculate the nickel, iron, and cobalt contents in the material according to the liquid level drop, so as to calculate the recovery rate of carbonyl nickel. This method can directly measure the metal content in the rectification residue liquid synchronously and in a timely manner, calculate and evaluate the actual recovery rate of carbonyl nickel in the rectification process. After clarifying the contents of each component in the rectification residue liquid, it provides a reliable basis for adjusting the rectification process parameters in real time and improving the purity of carbonyl nickel.

Claims

1. An apparatus for quantitatively detecting the content of nickel carbonyl in rectification residue liquid, comprising a liquid seal tank (3), characterized in that: The top of the liquid seal tank (3) is communicatively provided with a rectification residue inlet (4). A chilled water inlet (5) is arranged on the side of the rectification residue inlet (4). The bottom of the liquid seal tank (3) is communicatively provided with a metering transparent U-shaped tube (6), and an electronic ignition spray head (7) is connected to the end of the metering transparent U-shaped tube (6).

2. The device for quantitatively detecting the content of nickel carbonyl in rectification residue according to claim 1, wherein: A liquid inlet pipe (8) is arranged in the rectification residue inlet (4), and a three-way valve (1) is arranged on the liquid inlet pipe (8).

3. The device for quantitatively detecting the content of nickel carbonyl in the rectification residue according to claim 1, wherein: A stop valve (2) is arranged at the liquid outlet of the bottom of the liquid seal tank (3), and the stop valve (2) is connected to the metering transparent U-shaped tube (6).

4. It also includes a method for quantitatively detecting the content of nickel carbonyl in the rectification residue, characterized in that, It includes the following steps: Step 1: Utilize the density difference between the chilled water and nickel carbonyl in the liquid seal tank (3). First, add chilled water to the liquid seal tank (3) to a height of 20 mm - 30 mm, allowing the rectification residue to safely enter the liquid seal tank (3) without contacting air. Then, use the three-way valve (1) to conduct air purging on the pipeline to ensure that the rectification residue has no contact with air; Step 2: Then, control the rectification residue to fill the metering transparent U-shaped tube (6) up to the zero scale line to facilitate reading the change in liquid level after combustion; Step 3: Ignite with the electronic ignition spray head (7) to completely collect the combustion products into a combustion bottle with the same caliber; Step 4: Then, repeatedly wash the combustion bottle with hydrochloric acid 3 - 4 times, combine the washing solutions, use atomic absorption to test the nickel and iron contents, and calculate the contents of nickel and iron based on the decrease in the liquid level of the metering transparent U-shaped tube (6), thereby calculating the recovery rate of nickel carbonyl.

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