A method for preparing dicarbonyl cyclopentadienyl cobalt

Abstract

The present application relates to the field of metal organic source synthesis, and particularly relates to a preparation method of dicarbonyl cyclopentadienyl cobalt, which comprises the following steps: under the protection of inert gas, raw material dicobalt octacarbonyl and tetrahydrofuran solvent are added into a reaction bottle, a normal pressure reflux device is arranged, and stirring is started; tetrahydrofuran solution of cyclopentadienyl sodium is added dropwise into the reaction bottle, after the dropwise addition is completed, stirring reaction is kept at 70-80 DEG C for 6-10 h; after the stirring reflux is completed, the solvent tetrahydrofuran is distilled out through normal pressure distillation; then a reduced pressure distillation device is arranged, and crude dicarbonyl cyclopentadienyl cobalt is obtained through reduced pressure distillation; the obtained crude dicarbonyl cyclopentadienyl cobalt is subjected to reduced pressure rectification to obtain finished product dicarbonyl cyclopentadienyl cobalt; all the above steps are carried out in the environment of inert gas. The preparation method has the advantages of simple synthesis route, easy raw material, short reaction time, high synthesis efficiency, high product yield, less raw material residue, high product purity, and can be used for industrial production, and can meet the growing market demand.

Description

Technical Field

[0001] This invention relates to the field of organometallic source synthesis, and more particularly to a method for preparing dicarbonylcyclopentadienyl cobalt. Background Technology

[0002] Dicarbonylcyclopentadienylcobalt is an organometallic compound with the chemical formula CpCo(CO)2, widely used in chemistry. It can be used as a reagent in intramolecular cycloaddition reactions to synthesize compounds with cyclopentadiene structures. It can also act as a catalyst in various organic reactions, catalyzing carbonylation reactions to convert carbonyl compounds into corresponding alcohols, aldehydes, or ketones. Furthermore, in chip manufacturing, dicarbonylcyclopentadienylcobalt is commonly used as a metal-organic precursor material in metal deposition steps such as metal-organic chemical vapor deposition (MOCVD). It can provide cobalt atoms or ions to form cobalt-related thin films or structures, such as metal wires, electrodes, resistors, and magnetic materials. By controlling the deposition conditions of dicarbonylcyclopentadienylcobalt, the thickness, crystallinity, and electrical properties of the cobalt film can be regulated to meet the requirements of chip manufacturing.

[0003] Because dicarbonylcyclopentadienyl cobalt can be used in chip manufacturing, electronic components, magnetic materials and other fields, the demand for high-performance chips and electronic components is constantly increasing with the rapid development of emerging technologies such as 5G communication, artificial intelligence, and the Internet of Things. Therefore, the demand for dicarbonylcyclopentadienyl cobalt is showing a steady growth trend. The current synthesis process uses cyclopentadiene monomer and octacarbonyl cobalt to react under reflux for 48 hours. This method has two disadvantages: first, the reaction time is too long and the energy consumption is high; second, the raw material cyclopentadiene monomer will contain some dimers or even polymers. These dimers and polymers have boiling points close to those of the product dicarbonylcyclopentadienyl cobalt, making them difficult to remove completely and difficult to obtain high-purity dicarbonylcyclopentadienyl cobalt. Summary of the Invention

[0004] To address the problems of long reaction time, high energy consumption, and raw material residue in the existing technologies, this invention provides a method for preparing dicarbonylcyclopentadienyl cobalt.

[0005] To achieve the above objectives, the present invention provides a method for preparing dicarbonylcyclopentadienyl cobalt, comprising the following steps:

[0006] S1. Under the protection of an inert gas, add the raw material octacarbonyl dicobalt and tetrahydrofuran solvent to the reaction flask, set up an atmospheric pressure reflux device, and start stirring;

[0007] S2. Add the tetrahydrofuran solution of sodium cyclopentadienyl to the reaction flask dropwise. After the addition is complete, keep the mixture at 70-80°C and stir for 6-10 hours.

[0008] S3, after the stirring reflux, first normal pressure distillation is used to distill the solvent tetrahydrofuran;

[0009] S4, the reduced pressure distillation device is changed again, and the crude di-carbonyl cyclopentadienyl cobalt is obtained through the reduced pressure distillation;

[0010] S5, the crude di-carbonyl cyclopentadienyl cobalt is obtained through the reduced pressure distillation, and the di-carbonyl cyclopentadienyl cobalt product is obtained;

[0011] All the above steps are carried out in the inert gas environment.

[0012] Preferably, the tetrahydrofuran is used after being dried and water is removed.

[0013] Preferably, the molar ratio of the amount of the octacarbonyldicobalt and the amount of the sodium cyclopentadienyl is 1: (1.05-1.8).

[0014] Preferably, the molar ratio of the amount of the octacarbonyldicobalt and the amount of the sodium cyclopentadienyl is 1:1.5.

[0015] Preferably, the stirring reaction is 6-10h, and the temperature is increased to 70-80℃.

[0016] Preferably, the stirring reaction is 6-10h, and the temperature is increased to 70-80℃.

[0017] Preferably, the reduced pressure distillation is controlled at a pressure of 30 Torr, and the distillate at 90-95℃ is received.

[0018] Preferably, the reduced pressure distillation is controlled at a pressure of 30 Torr, and the distillate at 90-95℃ is received.

[0019] Preferably, the di-carbonyl cyclopentadienyl cobalt product needs to be detected by nuclear magnetic resonance and ICP to confirm the purity.

[0020] Preferably, the inert gas has a water and oxygen content of less than 1ppm.

[0021] The application provides a preparation method of di-carbonyl cyclopentadienyl cobalt, which comprises the following steps:

[0022]

[0023] Compared with the prior art, the application has the following beneficial effects:

[0024] 1. The application provides a preparation method of dicarbonyl cyclopentadienyl cobalt, the synthesis route is simple, raw materials are easy to obtain, compared with the reaction of traditional cyclopentadiene monomer and octacarbonyldicobalt, the reaction time is greatly shortened, the production efficiency is greatly improved, the production energy consumption is saved, and the method is suitable for industrial production.

[0025] 2. The cyclopentadiene monomer is not used as a reaction raw material, the impurities such as cyclopentadiene dimers and polymers brought by the raw material and having a boiling point close to that of the product dicarbonyl cyclopentadienyl cobalt and being difficult to remove are avoided, the product yield is high, and the purity is high. BRIEF DESCRIPTION OF DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments described in the application, and for those skilled in the art, other drawings obtained according to these drawings without creative labor also belong to the protection scope of the application.

[0027] Figure 1 It is a process step of a method for preparing dicarbonyl cyclopentadienyl cobalt according to an embodiment of the application.

[0028] Figure 2 It is a nuclear magnetic hydrogen spectrum of dicarbonyl cyclopentadienyl cobalt according to an embodiment of the application.

[0029] Figure 3 It is a nuclear magnetic carbon spectrum of dicarbonyl cyclopentadienyl cobalt according to an embodiment of the application. DETAILED DESCRIPTION

[0030] In order to make the objects, technical solutions and advantages of the application clearer, the application will be further described in combination with the following specific embodiments.

[0031] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in the application should be the general meanings understood by those skilled in the art. The words such as "first", "second" and the like used in the application do not represent any order, number or importance, but are only used to distinguish different components. The words such as "include" or "contain" and the like mean that the elements or objects before the words cover the elements or objects listed after the words and their equivalents, and do not exclude other elements or objects. The words such as "connect" or "connected" and the like are not limited to physical or mechanical connection, but can include electrical connection, whether direct or indirect. The words such as "up", "down", "left", "right" and the like are only used to represent relative positional relationship, when the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0032] As Figure 1 shown, the embodiment of the present application provides a preparation method of dicarbonyl cyclopentadienyl cobalt, comprising:

[0033] S1, under the protection of inert gas, raw material dicobalt octacarbonyl and tetrahydrofuran solvent are added to the reaction bottle, and the stirring is started with the normal pressure reflux device;

[0034] S2, the tetrahydrofuran solution of cyclopentadienyl sodium is added dropwise to the reaction bottle, and after the dropwise addition is completed, the stirring reaction is maintained at 70~80℃ for 6~10h;

[0035] S3, after the stirring reflux is completed, the solvent tetrahydrofuran is distilled out at normal pressure;

[0036] S4, then the reduced pressure distillation device is changed, and the crude product of dicarbonyl cyclopentadienyl cobalt is obtained by reduced pressure distillation;

[0037] S5, the crude product of dicarbonyl cyclopentadienyl cobalt is obtained by reduced pressure distillation to obtain the finished product of dicarbonyl cyclopentadienyl cobalt;

[0038] All the above steps are carried out in the environment of inert gas.

[0039] In some optional embodiments, the tetrahydrofuran can be used only after drying and removing water.

[0040] In some optional embodiments, the molar ratio of the use amount of dicobalt octacarbonyl and cyclopentadienyl sodium is 1:(1.05~1.8).

[0041] In some optional embodiments, the molar ratio of the use amount of dicobalt octacarbonyl and cyclopentadienyl sodium is 1:1.5.

[0042] In some optional embodiments, the stirring reaction of 6~10h is started to count time when the temperature rises to 70~80℃.

[0043] In some optional embodiments, the stirring reaction of 6~10h is preferably stirring reaction of 8h.

[0044] In some optional embodiments, the reduced pressure distillation controls the pressure of 30Torr, and receives the distillate of 90~95℃.

[0045] In some optional embodiments, the reduced pressure distillation removes the front and rear distillates according to the proportion of 3~5% of the content of dicarbonyl cyclopentadienyl cobalt, and the middle distillate obtained is the finished product of dicarbonyl cyclopentadienyl cobalt.

[0046] In some optional embodiments, the finished product of dicarbonyl cyclopentadienyl cobalt needs to be detected and confirmed for purity by nuclear magnetic resonance and ICP.

[0047] In some alternative embodiments, the inert gas has a water and oxygen content of less than 1 ppm.

[0048] The following provides eight sets of embodiments:

[0049] Example One

[0050] Under the protection of inert gas, 171 g of octacarbonyldicobalt and 300 mL of tetrahydrofuran solvent were added to a 1 L reaction bottle, a normal pressure reflux device was assembled, and stirring was started; then 262.5 mL of a tetrahydrofuran solution (2.0 M) of sodium cyclopentadienyl was added dropwise to the reaction bottle, after the dropwise addition was completed, the temperature was raised to 75°C, and the stirring reaction was maintained at 75°C for 6 h; after the stirring reflux was completed, the solvent tetrahydrofuran was first distilled out at normal pressure, then a reduced pressure distillation device was assembled, the pressure was controlled at 30 Torr, and a fraction of 79.2 g at 90-95°C was received, which was a crude dicarbonylcyclopentadienylcobalt; the crude dicarbonylcyclopentadienylcobalt was subjected to reduced pressure distillation: according to a proportion of 3-5% of the content of dicarbonylcyclopentadienylcobalt, the front and rear fractions were removed, and the middle fraction obtained was a dicarbonylcyclopentadienylcobalt with higher purity.

[0051] All the above steps were performed in an inert gas environment (water and oxygen content less than 1 ppm), and the tetrahydrofuran solvent was used after being dried to remove water, and the product sample was detected by nuclear magnetic resonance and ICP to confirm the purity.

[0052] The crude dicarbonylcyclopentadienylcobalt in this case had a synthesis yield of 88%, and the product was detected by nuclear magnetic resonance spectrometer to confirm that it was dicarbonylcyclopentadienylcobalt; the inductively coupled plasma emission spectrometer (Optima 8000) detected that all inorganic elements were <1 ppm, and the purity reached 6N.

[0053] Example Two

[0054] Under the protection of inert gas, 171 g of octacarbonyldicobalt and 300 mL of tetrahydrofuran solvent were added to a 1 L reaction bottle, a normal pressure reflux device was assembled, and stirring was started; then 262.5 mL of a tetrahydrofuran solution (2.0 M) of sodium cyclopentadienyl was added dropwise to the reaction bottle, after the dropwise addition was completed, the temperature was raised to 75°C, and the stirring reaction was maintained at 75°C for 6 h; after the stirring reflux was completed, the solvent tetrahydrofuran was first distilled out at normal pressure, then a reduced pressure distillation device was assembled, the pressure was controlled at 30 Torr, and a fraction of 79.2 g at 90-95°C was received, which was a crude dicarbonylcyclopentadienylcobalt; the crude dicarbonylcyclopentadienylcobalt was subjected to reduced pressure distillation: according to a proportion of 3-5% of the content of dicarbonylcyclopentadienylcobalt, the front and rear fractions were removed, and the middle fraction obtained was a dicarbonylcyclopentadienylcobalt with higher purity.

[0055] The steps were performed under the protection of inert gas (water and oxygen content less than 1 ppm), and the tetrahydrofuran solvent was used after being dried to remove water, and the product sample was detected by nuclear magnetic resonance and ICP to confirm the purity.

[0056] The crude product of the example was confirmed to be dicarbonyl cyclopentadienyl cobalt by nuclear magnetic resonance spectrometer. The content of all inorganic elements was less than 1 ppm, and the purity reached 6N, as detected by inductively coupled plasma emission spectrometer (Optima 8000).

[0057] Example 3

[0058] Under the protection of inert gas, 171 g of octacarbonyldicobalt and 300 mL of tetrahydrofuran solvent were added to a 1 L reaction bottle, and a normal pressure reflux device was connected, and stirring was started. Then 375 mL of a tetrahydrofuran solution (2.0 M) of cyclopentadienyl sodium was added dropwise to the reaction bottle, after the dropwise addition was completed, the temperature was raised to 75°C, and the stirring reaction was kept at 75°C for 6 h. After the stirring reflux was completed, the solvent tetrahydrofuran was distilled out at normal pressure, then a reduced pressure distillation device was connected, and the pressure was controlled at 30 Torr, and a fraction of 82.8 g at 90-95°C was collected, which was the crude product of dicarbonyl cyclopentadienyl cobalt. The crude product of dicarbonyl cyclopentadienyl cobalt was subjected to reduced pressure distillation, and the front and rear fractions were removed according to the content of dicarbonyl cyclopentadienyl cobalt at a ratio of 3-5%, and the middle fraction was the dicarbonyl cyclopentadienyl cobalt with higher purity.

[0059] The steps were all carried out under the protection of inert gas (the water and oxygen contents were all less than 1 ppm), and the tetrahydrofuran solvent was used after drying and removing water, and the product sample was subjected to nuclear magnetic and ICP detection to confirm the purity.

[0060] The crude product of the example was confirmed to be dicarbonyl cyclopentadienyl cobalt by nuclear magnetic resonance spectrometer. The content of all inorganic elements was less than 1 ppm, and the purity reached 6N, as detected by inductively coupled plasma emission spectrometer (Optima 8000).

[0061] Example 4

[0062] Under the protection of inert gas, 171 g of octacarbonyldicobalt and 300 mL of tetrahydrofuran solvent were added to a 1 L reaction bottle, and a normal pressure reflux device was connected, and stirring was started. Then 375 mL of a tetrahydrofuran solution (2.0 M) of cyclopentadienyl sodium was added dropwise to the reaction bottle, after the dropwise addition was completed, the temperature was raised to 75°C, and the stirring reaction was kept at 75°C for 6 h. After the stirring reflux was completed, the solvent tetrahydrofuran was distilled out at normal pressure, then a reduced pressure distillation device was connected, and the pressure was controlled at 30 Torr, and a fraction of 82.8 g at 90-95°C was collected, which was the crude product of dicarbonyl cyclopentadienyl cobalt. The crude product of dicarbonyl cyclopentadienyl cobalt was subjected to reduced pressure distillation, and the front and rear fractions were removed according to the content of dicarbonyl cyclopentadienyl cobalt at a ratio of 3-5%, and the middle fraction was the dicarbonyl cyclopentadienyl cobalt with higher purity.

[0063] The steps are all carried out under the protection of inert gas (water oxygen content is less than 1 ppm), and the tetrahydrofuran solvent is used after drying and removing water, and the product sample is detected by nuclear magnetic resonance and ICP to confirm the purity.

[0064] The crude product of the example is bis(cyclopentadienyl) cobalt, the synthesis yield of which is 92%, the product is detected by nuclear magnetic resonance spectrometer to confirm that it is bis(cyclopentadienyl) cobalt, and the inorganic elements are all less than 1 ppm detected by inductively coupled plasma emission spectrometer (Optima 8000), and the purity reaches 6N.

[0065] Example five

[0066] Under the protection of inert gas, 341.9g of bis(cyclooctadienyl) dicobalt and 600mL of tetrahydrofuran solvent are added into a 2L reaction bottle, a normal pressure reflux device is connected, and stirring is started; then 750mL of cyclopentadienyl sodium tetrahydrofuran solution (2.0M) is added dropwise into the reaction bottle, after the dropwise addition is completed, the temperature is increased to 70°C, and the stirring reaction is kept at 70°C for 6h; after the stirring reflux is completed, the solvent tetrahydrofuran is distilled out at normal pressure, then a reduced pressure distillation device is connected, the pressure is controlled to be 30 Torr, and the fraction of 165.2g at 90-95°C is received as the crude product of bis(cyclopentadienyl) cobalt; the obtained crude product of bis(cyclopentadienyl) cobalt is subjected to reduced pressure distillation: the front and rear fractions are removed according to the proportion of 3-5% of the content of bis(cyclopentadienyl) cobalt, and the middle fraction obtained is the bis(cyclopentadienyl) cobalt with higher purity.

[0067] The steps are all carried out under the protection of inert gas (water oxygen content is less than 1 ppm), and the tetrahydrofuran solvent is used after drying and removing water, and the product sample is detected by nuclear magnetic resonance and ICP to confirm the purity.

[0068] The crude product of the example is bis(cyclopentadienyl) cobalt, the synthesis yield of which is 92%, the product is detected by nuclear magnetic resonance spectrometer to confirm that it is bis(cyclopentadienyl) cobalt; the inorganic elements are all less than 1 ppm detected by inductively coupled plasma emission spectrometer (Optima 8000), and the purity reaches 6N.

[0069] Example six

[0070] Into a 2L reaction flask, 341.9g of dicobalt octacarbonyl and 600mL of tetrahydrofuran solvent were added under the protection of inert gas, and a normal pressure reflux device was connected and stirring was started; then 750mL of sodium cyclopentadienyl tetrahydrofuran solution (2.0M) was added dropwise into the reaction flask, after the dropwise addition was completed, the temperature was raised to 80°C, and the stirring reaction was kept at 80°C for 6h; after the stirring reflux was completed, the solvent tetrahydrofuran was first distilled out under normal pressure, then a reduced pressure distillation device was connected, and the pressure was controlled at 30Torr, and a fraction of 165.7g was received at 90~95°C, which was the crude dicarbonyl cyclopentadienyl cobalt; the obtained crude dicarbonyl cyclopentadienyl cobalt was subjected to reduced pressure distillation: according to the proportion of 3~5% of the content of dicarbonyl cyclopentadienyl cobalt, the front and rear fractions were removed, and the middle fraction obtained was the dicarbonyl cyclopentadienyl cobalt with higher purity.

[0071] The steps were all carried out under the protection of inert gas (the water and oxygen content was all less than 1ppm), and the tetrahydrofuran solvent was used after drying and removing water, and the product sample was subjected to nuclear magnetic and ICP detection to confirm the purity.

[0072] The synthesis yield of the crude dicarbonyl cyclopentadienyl cobalt in this case was 92%, and the product was confirmed to be dicarbonyl cyclopentadienyl cobalt by nuclear magnetic resonance spectrometer detection; the inductively coupled plasma emission spectrometer (Optima8000) detected that all inorganic elements were <1ppm, and the purity reached 6N.

[0073] Example Seven

[0074] Into a 2L reaction flask, 341.9g of dicobalt octacarbonyl and 600mL of tetrahydrofuran solvent were added under the protection of inert gas, and a normal pressure reflux device was connected and stirring was started; then 750mL of sodium cyclopentadienyl tetrahydrofuran solution (2.0M) was added dropwise into the reaction flask, after the dropwise addition was completed, the temperature was raised to 75°C, and the stirring reaction was kept at 75°C for 8h; after the stirring reflux was completed, the solvent tetrahydrofuran was first distilled out under normal pressure, then a reduced pressure distillation device was connected, and the pressure was controlled at 30Torr, and a fraction of 171g was received at 90~95°C, which was the crude dicarbonyl cyclopentadienyl cobalt; the obtained crude dicarbonyl cyclopentadienyl cobalt was subjected to reduced pressure distillation: according to the proportion of 3~5% of the content of dicarbonyl cyclopentadienyl cobalt, the front and rear fractions were removed, and the middle fraction obtained was the dicarbonyl cyclopentadienyl cobalt with higher purity.

[0075] The steps were all carried out under the protection of inert gas (the water and oxygen content was all less than 1ppm), and the tetrahydrofuran solvent was used after drying and removing water, and the product sample was subjected to nuclear magnetic and ICP detection to confirm the purity.

[0076] The synthesis yield of the crude dicarbonyl cyclopentadienyl cobalt in this case was 95%, and the product was confirmed to be dicarbonyl cyclopentadienyl cobalt by nuclear magnetic resonance spectrometer detection; the inductively coupled plasma emission spectrometer (Optima8000) detected that all inorganic elements were <1ppm, and the purity reached 6N.

[0077] Example 8

[0078] Under the protection of inert gas, 341.9 g of octacarbonyldicobalt and 600 mL of tetrahydrofuran solvent were added into a 2 L reaction bottle, which was equipped with a normal pressure reflux device and was started to stir. Then 750 mL of sodium cyclopentadienyl tetrahydrofuran solution (2.0 M) was added dropwise into the reaction bottle, after the dropwise addition was completed, the temperature was increased to 75°C, and the stirring reaction was kept at 75°C for 10 h. After the stirring reflux was completed, the solvent tetrahydrofuran was distilled out at normal pressure, then the pressure was controlled to 30 Torr by changing the reduced pressure distillation device, and the fraction of 90-95°C was received, which was 171.1 g of the crude dicarbonylcyclopentadienyl cobalt. The crude dicarbonylcyclopentadienyl cobalt was subjected to reduced pressure distillation, and the front and rear fractions were removed according to the proportion of 3-5% of the dicarbonylcyclopentadienyl cobalt content, and the middle fraction was the dicarbonylcyclopentadienyl cobalt with higher purity.

[0079] The steps were all carried out under the protection of inert gas (the water oxygen content was less than 1 ppm), and the tetrahydrofuran solvent was used after being dried to remove water, and the product sample was subjected to nuclear magnetic and ICP detection to confirm the purity.

[0080] The crude dicarbonylcyclopentadienyl cobalt in the case has a synthesis yield of 95%, and the product is confirmed to be dicarbonylcyclopentadienyl cobalt by nuclear magnetic resonance spectrometer detection. The inductively coupled plasma emission spectrometer (Optima 8000) detects that all inorganic elements are less than 1 ppm, and the purity reaches 6N.

[0081] It can be seen that the present application provides a preparation method of dicarbonylcyclopentadienyl cobalt. Under the protection of inert gas, tetrahydrofuran is used as a solvent, sodium cyclopentadienyl and octacarbonyldicobalt are reacted to generate dicarbonylcyclopentadienyl cobalt. The product is confirmed to be dicarbonylcyclopentadienyl cobalt by nuclear magnetic resonance spectrometer detection, wherein, Figure 2 The nuclear magnetic hydrogen spectrum of the dicarbonylcyclopentadienyl cobalt is as follows: 1 H NMR (C6D6): δ = 4.42 (5H, -C5H5), Figure 3 The nuclear magnetic carbon spectrum of the dicarbonylcyclopentadienyl cobalt is as follows: 13 C NMR (C6D6): δ = 84.06 (-C5H5).

[0082] The preparation method has the advantages of simple synthesis route, easy-to-obtain raw materials, short reaction time, high synthesis efficiency, high product yield, less raw material residue, high product purity, and can be used for industrial production, and can meet the increasing market demand.

[0083] Those skilled in the art should understand that the above discussion of any embodiment is merely exemplary in nature and is not intended to imply that the present application, including the claims, is limited to these examples; the technical features among the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other changes of different aspects of the present application as described above, which are not provided in details for the sake of brevity.

[0084] The present application is intended to cover all such alternatives, modifications, and variations as come within the scope of the broadest possible interpretation of the appended claims. Accordingly, any and all such alternations, modifications, equivalents, improvements and the like are intended to be encompassed by the present application.

Claims

1. A method for preparing dicarbonylcyclopentadienyl cobalt, characterized in that, Includes the following steps: S1. Under the protection of an inert gas, add the raw material octacarbonyl dicobalt and tetrahydrofuran solvent to the reaction flask, set up an atmospheric pressure reflux device, and start stirring; S2. Add the tetrahydrofuran solution of sodium cyclopentadienyl to the reaction flask dropwise. After the addition is complete, keep the mixture at 70-80°C and stir for 6-10 hours. S3. After stirring and reflux, distill off the solvent tetrahydrofuran at atmospheric pressure. S4. Then, a vacuum distillation apparatus was used to obtain crude dicarbonylcyclopentadienyl cobalt by vacuum distillation. S5. The crude dicarbonylcyclopentadienyl cobalt obtained was subjected to vacuum distillation to obtain the finished dicarbonylcyclopentadienyl cobalt product. All of the above steps were carried out in an inert gas environment; The stirring reaction time of 6-10 hours begins when the temperature reaches 70-80°C.

2. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The tetrahydrofuran can only be used after it has been dried and dehydrated.

3. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The molar ratio of the amounts of octacarbonyl cobalt and cyclopentadienyl sodium is 1:(1.05~1.8).

4. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The molar ratio of the amounts of octacarbonyl cobalt and cyclopentadienyl sodium is 1:1.

5.

5. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The stirring reaction lasted for 8 hours.

6. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The reduced pressure distillation is controlled at 30 Torr, and the fraction collected is at 90~95°C.

7. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The reduced pressure distillation process removes the front and rear fractions at a ratio of 3-5% for the dicarbonylcyclopentadienyl cobalt content, and the resulting middle fraction is the dicarbonylcyclopentadienyl cobalt product.

8. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The purity of the dicarbonylcyclopentadienyl cobalt product needs to be confirmed by NMR and ICP testing.

9. The method for preparing dicarbonylcyclopentadienyl cobalt according to claim 1, characterized in that, The inert gas contains less than 1 ppm of water and oxygen.

Images