Process for controlling distillation of high-purity nickel carbonyl component
The separation of high-purity carbonyl nickel in a distillation column through a distillation process solves the problems of insufficient purity and efficiency in existing technologies, realizes the production of high-purity carbonyl nickel, and improves product quality and corporate benefits.
Patent Information
- Application Number
- CN202511261847.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-05
- Publication Date
- 2026-01-16
AI Technical Summary
Existing technologies are insufficient to produce high-purity carbonyl nickel, resulting in a shortage in market supply, and production efficiency and product added value are insufficient to meet demand.
Distillation is carried out in a distillation column using a distillation process. By controlling the temperature, pressure, and pressure difference, high-purity carbonyl nickel and heavy components are separated. High-purity carbonyl nickel is extracted by utilizing gas-liquid phase exchange and temperature adjustment.
It improves the purity and yield of carbonyl nickel, reduces energy consumption and investment costs, simplifies the process, reduces the floor space required, and enhances the economic benefits of enterprises.
Smart Images
Figure CN121344378A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the fields of powder metallurgy and metal materials technology, and in particular to a process for controlling the distillation of high-purity carbonyl nickel components. Background Technology
[0002] In recent years, market research has shown that the domestic and international markets for nickel carbonyl are performing well, with existing supply falling far short of market demand and production efficiency failing to meet development needs. Given the current situation of enterprises, the purity of tetracarbonyl nickel is insufficient to reach the levels required for higher value-added new materials. Therefore, this invention proposes a process for controlling the distillation of high-purity nickel carbonyl components. Summary of the Invention
[0003] This invention provides a process for controlling the distillation of high-purity carbonyl nickel components, thereby obtaining a high-purity carbonyl nickel powder raw material liquid through a distillation process.
[0004] According to one aspect of this disclosure, a process for controlling the distillation of high-purity nickel carbonyl components is provided, the process comprising: The first material output from the raw material synthesis unit is transported to a preheating device for heating. The second material output from the preheating equipment is conveyed to the distillation column; The second stream is distilled in a distillation column; The third stream at the top of the tower is cooled by a condenser and then enters a gas-liquid separator. The sixth stream separated from the gas-liquid separator flows into the distillation column and the high-purity tank, respectively. The material from the bottom of the distillation column flows into the reboiler and the low-purity tank, respectively. The material in the low-purity tank is either sent to the next process or recycled. The reboiler heats the incoming stream and returns it to the distillation column as a vapor-liquid phase stream.
[0005] In one possible implementation, the first stream comprises: nickel carbonyl, iron carbonyl, carbon monoxide or nitrogen, and dust impurities.
[0006] In one possible implementation, the components in the first material are characterized by the following proportions: nickel carbonyl 98.83%, iron carbonyl 0.627%, carbon monoxide or nitrogen 0.198%, and dust impurities 0.345%.
[0007] In one possible implementation, the pressure of the first material before it enters the preheating equipment is controlled to be an absolute pressure of 0.3 MPa and the temperature is 25°C. The preheating equipment is then controlled to heat the first material to 40°C to obtain the second material.
[0008] In one possible implementation, the pressure at the top of the column is controlled by a regulating valve and a flow meter installed at the top vapor line of the distillation column. Liquid level control inside the column: The liquid level inside the distillation column is controlled by a regulating valve and a flow meter installed at the bottom of the distillation column; Top temperature control: The top temperature of the distillation column is controlled by a regulating valve and flow meter installed on the top reflux line of the distillation column. Bottom temperature control: The temperature at the bottom of the tower is controlled by regulating valves and flow meters installed on the heat medium pipeline of the reboiler.
[0009] In one possible implementation, the distillation column operates at a gauge pressure of 12 kPa, has two sections of structured packing, and has a diameter of 400 mm.
[0010] In one possible implementation, the feed rate is 580 kg / h.
[0011] In one possible implementation, the distillation column is equipped with a differential pressure controller. The differential pressure controller compares the pressure difference between the top and bottom of the column and feeds the comparison result back to the distillation column control system. The control system controls the regulating valve and flow meter installed on the top reflux line of the column to adjust the temperature.
[0012] Compared with the prior art, the beneficial effects of the present invention are: The process described in this application removes heavy components from nickel-iron carbonyl within a single distillation column. The nickel-iron carbonyl feedstock is fed into the middle of a distillation column, where it is operated under pressure. After cooling the overhead gas, the top product is high-purity nickel carbonyl. The heavy components at the bottom of the column are processed in a downstream evaporator.
[0013] This invention incorporates a temperature controller in the distillation column to adjust product quality. The temperature controller adjusts the temperature at the top of the column, ensuring that the extraction rate of the top product remains stable at a set point to guarantee product quality.
[0014] This invention takes into account the special characteristics of the materials and incorporates a differential pressure controller in the distillation column to adjust operating parameters. The differential pressure controller adjusts the temperature of the top product by comparing the pressure difference between the top and bottom of the column, thereby ensuring product quality by maintaining the extraction rate of the top product at a stable set point.
[0015] Obtaining high-purity carbonyl nickel powder feedstock solution through distillation is essential for increasing product added value and improving enterprise economic benefits. This method offers advantages such as low investment, small footprint, low energy consumption, and high yield of high-purity products.
[0016] (1) High yield of high-purity carbonyl nickel component Using the method of extracting from the top of the distillation column allows for sufficient gas-liquid phase exchange of the material within the column. Simultaneously, through precise control of temperature and pressure difference, the yield of high-purity carbonyl nickel can be increased by 0.5% to 1%.
[0017] (2) Low energy consumption The temperature of the extract from the distillation column is relatively low (below 50°C), which allows for full utilization of suitable heat sources, reduces utility consumption, and lowers energy consumption. By reducing the column operating pressure and controlling the reflux temperature at the top of the column, less reboiling heat and condensation are required, and the accuracy of feed liquid fractionation can be achieved with a small number of supporting facilities.
[0018] (3) Investment savings Reducing equipment investment and operating energy consumption is crucial. This invention adopts a distillation process, uses only one column, and does not employ a vacuum system, thus significantly reducing investment costs.
[0019] (4) Small footprint The single-tower distillation process simplifies the process and reduces the floor space required. Attached Figure Description
[0020] Figure 1 A process flow diagram illustrating the controlled distillation of high-purity carbonyl nickel components according to an embodiment of this disclosure is shown.
[0021] Figure 2 A schematic diagram of a process for controlling the distillation of high-purity carbonyl nickel components according to an embodiment of the present disclosure is shown. Detailed Implementation
[0022] Various exemplary embodiments, features, and aspects of this disclosure will now be described in detail with reference to the accompanying drawings. The same reference numerals in the drawings denote elements that have the same or similar functions. Although various aspects of the embodiments are shown in the drawings, they are not necessarily drawn to scale unless specifically indicated otherwise.
[0023] The term “exemplary” as used herein means “serving as an example, embodiment, or illustration.” Any embodiment illustrated herein as “exemplary” is not necessarily to be construed as superior to or better than other embodiments.
[0024] Furthermore, to better illustrate this disclosure, numerous specific details are set forth in the following detailed description. Those skilled in the art will understand that this disclosure can be practiced without certain specific details. In some instances, methods, means, components, and circuits well known to those skilled in the art have not been described in detail in order to highlight the main points of this disclosure.
[0025] According to one aspect of this disclosure, a process for controlling the distillation of high-purity nickel carbonyl components is provided, the process comprising: S01, the first material output from the raw material synthesis unit is transported to the preheating equipment for heating; S02, the second material output from the preheating equipment is conveyed to the distillation column; S03, the second stream is distilled in a distillation column; S04, the third stream at the top of the tower is cooled by the condenser and then enters the gas-liquid separator. S05, control the sixth stream separated from the gas-liquid separator to flow into the distillation column and the high-purity tank respectively; S06, the material from the bottom of the distillation column flows into the reboiler and the low-purity tank respectively, and the material in the low-purity tank enters the next process or is recycled. S07, the reboiler heats the incoming stream and returns it to the distillation column as a vapor-liquid phase stream.
[0026] For example, the carbonyl nickel-iron liquid (first stream) from the carbonyl nickel powder synthesis unit enters the middle of a distillation column, where it is separated into a high-purity carbonyl nickel fraction (top) and a heavier fraction (bottom). The high-purity carbonyl nickel at the top is cooled and enters a gas-liquid separator at the top. A portion of the liquid at the bottom is heated in a reboiler and returned to the distillation column as reflux, while the remainder is cooled and sent as product to downstream processes. The heavier fraction at the bottom of the distillation column enters a storage tank and is sent to downstream processes or prepared for reprocessing.
[0027] In one possible implementation, the first stream comprises: nickel carbonyl, iron carbonyl, carbon monoxide or nitrogen, and dust impurities.
[0028] In one possible implementation, the components in the first material are characterized by the following proportions: nickel carbonyl 98.83%, iron carbonyl 0.627%, carbon monoxide or nitrogen 0.198%, and dust impurities 0.345%.
[0029] In one possible implementation, the pressure of the first material before it enters the preheating equipment is controlled to be an absolute pressure of 0.3 MPa and the temperature is 25°C. The preheating equipment is then controlled to heat the first material to 40°C to obtain the second material.
[0030] In one possible implementation, the pressure at the top of the column is controlled by a regulating valve and a flow meter installed at the top vapor line of the distillation column. Liquid level control inside the column: The liquid level inside the distillation column is controlled by regulating valves and flow meters installed at the bottom of the distillation column; for example, the liquid level is controlled at 60%-70% of the distillation column.
[0031] Top temperature control: The top temperature of the distillation column is controlled by a regulating valve and flow meter installed on the top reflux line of the distillation column. Bottom temperature control: The temperature at the bottom of the tower is controlled by regulating valves and flow meters installed on the heat medium pipeline of the reboiler.
[0032] In one possible implementation, the distillation column operates at a gauge pressure of 12 kPa, has two sections of structured packing, and has a diameter of 400 mm.
[0033] In one possible implementation, the feed rate (first stream) is 580 kg / h. In this case, the high-purity nickel carbonyl extraction rate from the top of the column is 562 kg / h. The yield of high-purity nickel carbonyl can be increased by 0.5–1%.
[0034] In one possible implementation, the distillation column is equipped with a differential pressure controller. The differential pressure controller compares the pressure difference between the top and bottom of the column (the total differential pressure of the column is controlled within 2 kPa (gauge pressure), and then controls the temperature at the top of the column). The comparison result is fed back to the distillation column control system. The control system controls the regulating valve and flow meter set on the top reflux line of the column to adjust the temperature.
[0035] Application example: The distillation column operates at a pressure of 12 kPa (g) and contains two sections of structured packing. The feed liquid F01 from the synthesis unit enters the unit at a pressure of 0.3 MPa (A) and a temperature of 25°C. It is heated to 40°C in the preheating equipment 10 and then fed into the distillation column 40 as the feed stream F02. After being cooled by condenser 20, the top stream F03 enters gas-liquid separator 30. The gas phase stream F05 separated by gas-liquid separator 30 is connected to the downstream process for processing. A portion of the liquid component F06 separated by gas-liquid separator 30 is separated as liquid stream F07 and enters distillation column 40 from the top. The other portion is sent to the downstream section as product liquid stream F08. A thermosiphon reboiler 50 is provided at the bottom of the column. Part of the bottom stream F10 is heated by the reboiler 50 and returned to the distillation column 40 as a vapor-liquid phase stream F11. The other stream is sent to the temporary storage tank as a low-purity stream F09 and sent to the downstream process, or is prepared for reprocessing.
[0036] The various embodiments of this disclosure have been described above. These descriptions are exemplary and not exhaustive, nor are they limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen to best explain the principles, practical application, or technical improvements to the embodiments in the market, or to enable others skilled in the art to understand the embodiments disclosed herein.
Claims
1. A process for controlling the distillation of a high purity nickel carbonyl component, characterized in that the process The application relates to a method for purifying a first stream output by a raw material synthesis unit. The first stream output by the raw material synthesis unit is sent to a preheating device for heating; The second stream output by the preheating device is sent to the middle part of a rectifying tower; The second stream is distilled in the rectifying tower; The third stream at the top of the rectifying tower is cooled by a condenser and then enters a gas-liquid separation tank; The sixth stream separated from the gas-liquid separation tank is sent to the rectifying tower and a high-purity tank respectively; The stream at the bottom of the rectifying tower is sent to a reboiler and a low-purity tank respectively, and the stream in the low-purity tank is sent to a next process or is recycled; The reboiler heats the stream flowing in and returns the stream to the rectifying tower as a gas-liquid phase stream.
2. The process of claim 1, wherein the process is characterized by, The first stream comprises carbonyl nickel, carbonyl iron, carbon monoxide or nitrogen and dust impurities.
3. The process of claim 1, wherein the process is characterized by, The proportions of the components in the first stream are as follows: 98.83% of carbonyl nickel, 0.627% of carbonyl iron, 0.198% of carbon monoxide or nitrogen and 0.345% of dust impurities.
4. The process of claim 1, wherein the process is characterized by, The pressure of the first stream before entering the preheating device is controlled to be 0.3 MPa (absolute pressure) and the temperature is controlled to be 25 DEG C, and the preheating device heats the first stream to 40 DEG C to obtain the second stream.
5. The process of claim 1, wherein the process is characterized by, The pressure at the top of the rectifying tower is controlled by an adjusting valve and a flowmeter arranged on a gas phase line at the top of the rectifying tower; The liquid level in the rectifying tower is controlled by an adjusting valve and a flowmeter arranged at the bottom of the rectifying tower; The temperature at the top of the rectifying tower is controlled by an adjusting valve and a flowmeter arranged on a reflux line at the top of the rectifying tower; The temperature at the bottom of the rectifying tower is controlled by an adjusting valve and a flowmeter arranged on a heat medium pipeline of the reboiler.
6. The process of claim 1, wherein the process is characterized by, The operating pressure of the rectifying tower is 12 KPa (gauge pressure), two regular fillers are arranged in the rectifying tower, and the diameter of the rectifying tower is 400 mm.
7. The process of claim 1, wherein the process is characterized by, The feeding speed is 580 kg / h.
8. The process of claim 1, wherein the process is characterized by, The rectifying tower is provided with a differential pressure controller, the differential pressure controller compares the pressure difference between the top and the bottom of the rectifying tower, feeds back the comparison result to a control system of the rectifying tower, and controls an adjusting valve and a flowmeter arranged on a reflux line at the top of the rectifying tower or an adjusting valve and a flowmeter arranged on the reflux line at the top of the rectifying tower to realize temperature adjustment.