Method for preparing cobalt carbonyl through multi-stage dissolution and separation process
The multi-stage dissolution and separation process for COCO production addresses waste and impurity issues, achieving high recovery rates and stable storage by dissolving COCO in solvents, ensuring a green and efficient production method.
Patent Information
- Application Number
- CN202510524128.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-24
- Publication Date
- 2025-07-15
AI Technical Summary
The existing process for preparing cobalt carbonyl is prone to wastewater and impurities, and cobalt carbonyl is unstable and easy to decompose, making it difficult to store.
The multi-stage dissolution separation process is adopted, through pressurization compression, heating reaction, cooling, multi-stage dissolution separation and pressure reduction treatment, the carbonyl cobalt is dissolved with organic solvents, and the exhaust gas is treated step by step to avoid the generation of wastewater waste gas, and stored in the organic solvent.
It realizes efficient green preparation of cobalt carbonyl, improves recovery rate, avoids the generation of wastewater and waste gas, solves the problem of unstable storage, high product purity, and stable production and operation.
Smart Images
Figure CN120309019A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of carbonyl metal functional materials and catalyst preparation, and in particular to a method for preparing cobalt carbonyl through a multi-stage dissolution and separation process. Background Art
[0002] Cobalt carbonyl has shown broad application potential and prospects in the field of catalytic applications and metal organic compound research. It has shown significant practical value in many fields such as organic synthesis reactions, petrochemical processes, new energy material preparation technology, as well as cutting-edge directions such as drug delivery systems and supramolecular chemistry. In particular, it is widely used as a highly efficient catalyst in the hydroformylation reaction (i.e., the synthesis of aldehyde compounds) in the process of petroleum refining. In biomedical research, as an important precursor of carbon monoxide-releasing molecules (CORMs), cobalt carbonyl can be designed as a new type of carbon monoxide carrier, and on this basis, its efficacy in key medical applications such as anti-inflammatory treatment, vasodilation, and tissue protection is further explored.
[0003] The melting point of cobalt carbonyl is 51℃-52℃, the boiling point is 52℃, the liquid phase exists in an extremely low temperature range, and it solidifies into a solid below 51℃, and cobalt carbonyl is easily soluble in organic solvents. The present invention utilizes its characteristics and adopts a three-stage dissolution and separation process. On the one hand, multi-stage dissolution greatly improves the recovery rate; on the other hand, the tail gas is treated by step-by-step pressure reduction. The whole process is green and environmentally friendly, without wastewater and waste gas, and no by-products; at the same time, it solves the storage problem caused by the unstable and easily decomposable characteristics of cobalt carbonyl.
[0004] Most of the existing disclosed processes for preparing cobalt carbonyl use a solution for reaction, which is prone to produce wastewater and introduce impurities. Summary of the invention
[0005] In view of the above technical problems, the present invention provides a method for preparing cobalt carbonyl through a multi-stage dissolution and separation process.
[0006] In order to achieve the above object, the technical solution of the present invention is as follows: A method for preparing cobalt carbonyl by a multi-stage dissolution separation process comprises the following steps: S1. The raw gas CO is pressurized by a booster compressor, wherein the raw gas CO inlet pressure is 6-8MPa, the booster compressor inlet pressure is 6-8MPa, the outlet pressure is 20-25MPa, and the gas flow rate is 700-760Nm 3 / h; S2, adding raw materials into the cobalt carbonyl reactor, introducing heated raw gas CO, and obtaining a mixed gas of cobalt carbonyl and CO, wherein the CO is heated to a temperature of 180-220° C.; S3. Cool the mixed gas through a cooler, where the cooling temperature of the mixed gas is reduced to 80 - 120 °C; S4. Pass the cooled mixed gas into a three - stage dissolution separator filled with organic solvent to obtain an organic solution containing cobalt carbonyl and CO respectively; S5. Reduce the pressure of the dissolution separator to obtain a product of an organic solution containing cobalt carbonyl.
[0007] Among them, in step S2, electrowon cobalt is selected as the raw material, and the cobalt content > 99.9%; the proportion of cobalt carbonyl gas in the mixed gas is 3 - 6%.
[0008] Among them, in step S4, cooling coils are arranged in the dissolution separator, and the cooling temperature is up to 30 - 45 °C; a demister is arranged at the top of the dissolution separator; the pressure of the dissolution separator decreases step by step, and the pressures are 20 - 25 MPa, 7 - 8 MPa, 0.4 - 0.8 MPa respectively; the gas inlet of the dissolution separator extends below the liquid level of the organic solvent, and the gas outlet is connected to the gas inlet of the next stage.
[0009] Among them, in step S4, the organic solvent is an alkane or alkene with C12; the liquid outlet of the dissolution separator is connected to the liquid inlet of the next stage.
[0010] Among them, in step S5, the concentration of cobalt carbonyl in the organic solution product of cobalt carbonyl is 0.1% - 20%.
[0011] The beneficial effects of the present invention are: 1. Carry out a gas - solid reaction between electrowon cobalt and CO in a cobalt carbonyl reactor. The reaction is efficient, green, and pollution - free, without generating waste water, waste gas, or by - products; 2. While cooling and dissolving the cobalt carbonyl mixed gas generated by the reaction in the dissolution separator, cobalt carbonyl can be collected to a great extent, and solid cobalt carbonyl will not block the pipeline, and the failure rate of production operation is low; 3. The final product dissolves cobalt carbonyl in an organic solvent and is stored in cans, fundamentally solving the storage problem caused by the unstable and easily decomposable characteristics of cobalt carbonyl. Brief Description of the Drawings
[0012] Figure 1 It is a process flow chart of the invention. Detailed Embodiments
[0013] To make the objectives, technical solutions, and advantages of the present invention clearer and more understandable, the present invention will be further described in detail below in combination with specific embodiments. It should be understood that these descriptions are only exemplary and are not intended to limit the scope of the present invention. In addition, in the following description, the descriptions of well - known structures and technologies are omitted to avoid unnecessarily confusing the concepts of the present invention.
[0014] Example 1 like Figure 1 As shown, a method for preparing cobalt carbonyl by a multi-stage dissolution separation process comprises the following steps: S1. The raw gas CO is pressurized by a booster compressor, wherein the raw gas CO inlet pressure is 6MPa, the booster compressor inlet pressure is 6MPa, the outlet pressure is 20MPa, and the gas flow rate is 700Nm 3 / h; S2, adding raw materials into the cobalt carbonyl reactor, introducing heated raw gas CO, and obtaining a mixed gas of cobalt carbonyl and CO, wherein the CO is heated to 180° C.; S3, cooling the mixed gas through a cooler, wherein the mixed gas cooling temperature is reduced to 80° C.; S4, passing the cooled mixed gas into a three-stage dissolution separator filled with an organic solvent to obtain an organic solution containing carbonyl cobalt and CO respectively; S5. Reduce the pressure of the dissolution separator to obtain an organic solution product containing dissolved cobalt carbonyl.
[0015] Wherein, in step S2, the raw material is electrolytic cobalt, and the cobalt content is greater than 99.9%; the carbonyl cobalt gas accounts for 3% of the mixed gas.
[0016] Among them, in the step S4, a cooling coil is provided in the dissolution separator, and the cooling temperature is set to 30°C; a foam catcher is provided on the top of the dissolution separator; the pressure of the dissolution separator decreases step by step, and the pressures are 20MPa, 7MPa, and 0.4MPa respectively; the air inlet of the dissolution separator is deep below the liquid surface of the organic solvent, and the air outlet is connected to the air inlet of the next stage.
[0017] Wherein, in step S4, the organic solvent is selected from C12 alkanes or alkenes; the liquid outlet of the dissolution separator is connected to the liquid inlet of the next stage.
[0018] Wherein, in the step S5, the concentration of cobalt carbonyl in the organic solution of the product cobalt carbonyl is 0.1%.
[0019] Example 2 like Figure 1 As shown, a method for preparing cobalt carbonyl by a multi-stage dissolution separation process comprises the following steps: S1. The raw gas CO is pressurized by a booster compressor, wherein the raw gas CO inlet pressure is 8MPa, the booster compressor inlet pressure is 8MPa, the outlet pressure is 25MPa, and the gas flow rate is 760Nm 3 / h; S2, adding raw materials into the cobalt carbonyl reactor, introducing heated raw gas CO, and obtaining a mixed gas of cobalt carbonyl and CO, wherein the CO is heated to 220° C.; S3, cooling the mixed gas through a cooler, wherein the mixed gas cooling temperature is reduced to 120° C.; S4, passing the cooled mixed gas into a three-stage dissolution separator filled with an organic solvent to obtain an organic solution containing carbonyl cobalt and CO respectively; S5. Reduce the pressure of the dissolution separator to obtain an organic solution product containing dissolved cobalt carbonyl.
[0020] Wherein, in step S2, the raw material is electrolytic cobalt, and the cobalt content is greater than 99.9%; the carbonyl cobalt gas accounts for 6% of the mixed gas.
[0021] Among them, in step S4, a cooling coil is installed in the dissolution separator, and the cooling temperature is 45°C; a foam catcher is set on the top of the dissolution separator; the pressure of the dissolution separator decreases step by step, and the pressures are 25MPa, 8MPa, and 0.8MPa respectively; the air inlet of the dissolution separator is deep below the liquid level of the organic solvent, and the air outlet is connected to the air inlet of the next level.
[0022] Wherein, in step S4, the organic solvent is selected from C12 alkanes or alkenes; the liquid outlet of the dissolution separator is connected to the liquid inlet of the next stage.
[0023] Wherein, in step S5, the concentration of cobalt carbonyl in the organic solution of the product cobalt carbonyl is 20%.
[0024] Example 3 like Figure 1 As shown, a method for preparing cobalt carbonyl by a multi-stage dissolution separation process, the key steps of the treatment process include: 1) The raw gas CO is pressurized by a booster compressor; the raw gas CO inlet pressure is 6MPa, the booster compressor inlet pressure is 6MPa, the outlet pressure is 20MPa, and the gas flow rate is 712Nm 3 / h; 2) Add the raw materials into the cobalt carbonyl reactor, and introduce the heated raw gas CO to obtain a mixed gas of cobalt carbonyl and CO; the raw material is electrolytic cobalt, and the cobalt content is greater than 99.9%; the CO is heated to 189°C; the cobalt carbonyl gas accounts for 3% of the mixed gas; 3) Cool the mixed gas through a cooler; the mixed gas cooling temperature is reduced to 90°C; 4) The cooled mixed gas is passed into a three-stage dissolution separation system filled with an organic solvent to obtain an organic solution containing carbonyl cobalt and CO respectively; dodecene is selected as the organic solvent, and the cooling temperature is 30°C; the pressure of the dissolution separator is gradually reduced, and the pressures are 20MPa, 7MPa, and 0.6MPa respectively; 5) The dissolution separator is depressurized to obtain an organic solution product containing carbonyl cobalt. The concentration of carbonyl cobalt in the organic solution of the product carbonyl cobalt is 12%.
[0025] Example 4 like Figure 1 As shown, a method for preparing cobalt carbonyl by a multi-stage dissolution separation process, the key steps of the treatment process include: 1) The raw gas CO is pressurized by a booster compressor; the raw gas CO inlet pressure is 8MPa, the booster compressor inlet pressure is 8MPa, the outlet pressure is 25MPa, and the gas flow rate is 756Nm 3 / h; 2) Add the raw materials into the cobalt carbonyl reactor, and introduce the heated raw gas CO to obtain a mixed gas of cobalt carbonyl and CO; the raw material is electrolytic cobalt, and the cobalt content is >99.9%; the CO is heated to 200°C; the cobalt carbonyl gas accounts for 6% of the mixed gas; 3) Cool the mixed gas through a cooler; the mixed gas cooling temperature is reduced to 110°C; 4) The cooled mixed gas is passed into a three-stage dissolution separation system filled with an organic solvent to obtain an organic solution containing carbonyl cobalt and CO respectively; tetrapropylene is selected as the organic solvent, and the cooling temperature is 40°C; the pressure of the dissolution separator is gradually reduced, and the pressures are 25MPa, 8MPa, and 0.8MPa respectively; 5) The dissolution separator is depressurized to obtain an organic solution product containing carbonyl cobalt. The concentration of carbonyl cobalt in the organic solution of the product carbonyl cobalt is 5%.
[0026] Example 5 like Figure 1 As shown, a method for preparing cobalt carbonyl by a multi-stage dissolution separation process, the key steps of the treatment process include: 1) The raw gas CO is pressurized by a booster compressor; the raw gas CO inlet pressure is 7MPa, the booster compressor inlet pressure is 7MPa, the outlet pressure is 23MPa, and the gas flow rate is 760Nm 3 / h; 2) Add the raw materials into the cobalt carbonyl reactor, and introduce the heated raw gas CO to obtain a mixed gas of cobalt carbonyl and CO; the raw material is electrolytic cobalt, and the cobalt content is greater than 99.9%; the CO is heated to 220°C; the cobalt carbonyl gas accounts for 4% of the mixed gas; 3) Cool the mixed gas through a cooler; the mixed gas cooling temperature is reduced to 100°C; 4) The cooled mixed gas is passed into a three-stage dissolution separation system filled with an organic solvent to obtain an organic solution containing carbonyl cobalt and CO respectively; dodecane is selected as the organic solvent, and the cooling temperature is 32°C; the pressure of the dissolution separator is gradually reduced, and the pressures are 23MPa, 7MPa, and 0.6MPa respectively; 5) Depressurize the dissolution separator to obtain an organic solution product containing cobalt carbonyl. The concentration of cobalt carbonyl in the organic solution product of cobalt carbonyl is 0.5%.
[0027] It should be understood that the above specific embodiments of the present invention are only used for exemplary illustration or explanation of the principle of the present invention, and do not constitute a limitation on the present invention. Therefore, any modifications, equivalent replacements, improvements, etc. made without departing from the spirit and scope of the present invention shall be included within the protection scope of the present invention. In addition, the appended claims of the present invention are intended to cover all variations and modification examples falling within the scope and boundaries of the appended claims, or equivalent forms of such scope and boundaries.
Claims
1. A method for preparing cobalt carbonyl through a multi-stage dissolution and separation process, characterized in that, It includes the following steps: S1. The raw gas CO is pressurized by a booster compressor, wherein the raw gas CO inlet pressure is 6-8MPa, the booster compressor inlet pressure is 6-8MPa, the outlet pressure is 20-25MPa, and the gas flow rate is 700-760Nm 3 / h; S2. Add the raw materials into the cobalt carbonyl reactor, and introduce the heated raw material gas CO to obtain a mixed gas of cobalt carbonyl and CO, where the heating temperature of CO is 180 - 220°C; S3. Cool the mixed gas through a cooler, where the cooling temperature of the mixed gas is reduced to 80 - 120°C; S4. Pass the cooled mixed gas into a three-stage dissolution separator filled with an organic solvent to obtain an organic solution containing dissolved cobalt carbonyl and CO respectively; S5. Reduce the pressure of the dissolution separator to obtain an organic solution product containing dissolved cobalt carbonyl.
2. The method for preparing cobalt carbonyl by a multi-stage dissolution and separation process according to claim 1, characterized in that: In step S2, the raw material is selected as electrowon cobalt with a cobalt content > 99.9%; the proportion of cobalt carbonyl gas in the mixed gas is 3 - 6%.
3. The method for preparing cobalt carbonyl by a multi-stage dissolution and separation process according to claim 1, wherein: In step S4, a cooling coil is provided in the dissolution separator with a cooling temperature of 30 - 45°C; a demister is provided at the top of the dissolution separator; the pressure of the dissolution separator decreases step by step, with pressures of 20 - 25 MPa, 7 - 8 MPa, and 0.4 - 0.8 MPa respectively; the inlet of the dissolution separator extends below the liquid level of the organic solvent, and the outlet is connected to the inlet of the next stage.
4. A method for preparing cobalt carbonyl by a multi-stage dissolution and separation process according to claim 1, characterized in that: In step S4, the organic solvent is selected as an alkane or alkene with C12; the liquid outlet of the dissolution separator is connected to the liquid inlet of the next stage.
5. A method for preparing cobalt carbonyl by a multi-stage dissolution and separation process according to claim 1, characterized in that: In step S5, the concentration of cobalt carbonyl in the organic solution of the product cobalt carbonyl is 0.1% - 20%.