Preparation method of (3, 3-dimethyl-1-butyne) cobalt hexacarbonyl

Abstract

The invention provides a preparation method of (3, 3-dimethyl-1-butyne) cobalt hexacarbonyl, which comprises the following steps: adding cobalt salt, a reducing agent, methyl formate and a catalyst into a high-pressure reaction kettle, keeping the reaction kettle in an inert gas atmosphere, and heating and stirring; cooling the high-pressure reaction kettle to room temperature, discharging gas, filtering reaction liquid, and putting filtrate into a normal-pressure reaction device in an inert gas atmosphere; 3, 3-dimethyl-1-butyne is added into the normal-pressure reaction device, stirring is conducted at normal temperature, filtering is conducted after the reaction is finished, and the obtained filtrate is subjected to aftertreatment to obtain a (3, 3-dimethyl-1-butyne) hexacarbonyl cobalt crude product. Methyl formate, formic acid 2, 4, 6-trichlorobenzene ester or diethyl oxalate is used for replacing carbon monoxide, so that the operation risk is reduced, the operation is simple, and the synthesis efficiency is high.

Description

Technical Field

[0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl. Background Art

[0002] (3,3-Dimethyl-1-butyne) dicobalt hexacarbonyl (CCTBA) is one of the cobalt-containing CVD / ALD precursors used to manufacture important functional layers of devices. It is widely used in chemical vapor deposition (CVD) or atomic layer deposition (ALD) processes, mainly used to manufacture important functional layers of devices, such as passivation layers, insulating layers, etc. As a precursor of cobalt materials, this compound has excellent volatility and can efficiently deposit cobalt films under relatively mild process conditions, ensuring the uniformity and purity of the deposited layer, thus having important industrial application value in the manufacture of microelectronic devices.

[0003] CN110818745A discloses a method for preparing (3,3-dimethyl-1-butyne) hexacarbonyl dicobalt using ionic liquid modified graphene oxide material. Under the protection of nitrogen atmosphere, carbonyl cobalt reagent and 1800g hydrocarbon solvent are added to the reactor, and then the temperature is controlled at 10°C, and then 0.1g of ionic liquid modified graphene oxide material and 25g of tert-butyl acetylene are slowly added to the system, and after the addition, the system is stirred and reacted for 5h under the protection of nitrogen atmosphere; after the reaction is completed, the filtrate is filtered, and the volatile components are distilled to obtain the crude product of (3,3-dimethyl-1-butyne) hexacarbonyl dicobalt, and then purified to obtain (3,3-dimethyl-1-butyne) hexacarbonyl dicobalt. Although the preparation method is highly operable, has few reaction by-products, and has a high yield. However, the above method has many steps, the preparation process of the ionic liquid modified graphene oxide material is complicated, and the initial material is expensive.

[0004] CN117126208A discloses a method for synthesizing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl, comprising the following steps: in a protective gas atmosphere, mixing dicobalt octacarbonyl and a solvent evenly to obtain an intermediate product; adding 3,3-dimethyl-1-butyne dropwise to the intermediate product to obtain a pre-product after reaction; and separating the pre-product to obtain (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl. Although the preparation method has simple operation steps and short time consumption, dicobalt octacarbonyl is expensive, has high synthesis cost, and is sensitive to air and difficult to store.

[0005] CN118307599A discloses a method for preparing a (3,3-dimethyl-1-butyne) hexacarbonyl dicobalt product, the specific method comprising: reacting octacarbonyl dicobalt with 3,3-dimethyl-1-butyne in an organic solvent at -10 to 40°C, under anhydrous, oxygen-free and dust-free conditions, removing the organic solvent, and distilling under reduced pressure to obtain a crude product, using an adsorbent to treat the crude product, and by controlling the amount of the adsorbent and the adsorption temperature and other parameters, effectively removing metal ion impurities and improving the quality of the product. Although the preparation method has simple operating steps and short time consumption, octacarbonyl dicobalt is expensive, has a high synthesis cost, and is sensitive to air and difficult to store.

[0006] CN118108773A discloses a method for preparing CCTBA and its application, the method comprising the following steps: continuously pumping tert-butyl acetylene into a tubular reactor containing dicobalt octacarbonyl at 10-30°C, normal pressure and nitrogen protection conditions for reaction; during the continuous pumping process, first collecting the reaction product CCTBA at 40-80°C; then collecting the unreacted tert-butyl acetylene at -20-36°C and pumping it into the reactor for further reaction; until the dicobalt octacarbonyl is completely reacted, the reaction is terminated. The invention does not involve solvents and effectively utilizes resources, but requires a corresponding reaction device, which has certain limitations.

[0007] CN119143814A discloses a method for synthesizing CCTBA using cobalt salt as raw material, the method comprising the following steps: adding activated carbon, gold chloride, cobalt salt and water into a reactor, stirring, controlling the temperature at 10-15°C, dripping 40% hydrazine hydrate aqueous solution, slowly heating to 50-55°C after the dripping is completed; dripping 30% sodium hydroxide aqueous solution into the reactor to control the pH of the reaction solution to be maintained between 7.5-8, controlling the temperature and stirring the reaction for 5-6h, filtering the reaction solution, drying the filtered solid, and then putting it into the reactor, adding dichloromethane and tert-butylacetylene, controlling the temperature at 25-30°C, introducing carbon monoxide gas to a gas phase pressure of 0.3-0.4MPa, until the reaction is completed, and distilling to obtain a pure product. This method uses cobalt salts with a wide range of sources and low prices as raw materials, which reduces costs to a certain extent, but uses precious metal catalysts, increases costs, and has strict reaction conditions and complex operations.

[0008] There are two sources of cobalt in the existing technology for synthesizing CCTBA. One method uses dicobalt octacarbonyl as the cobalt source. Although the operation is simple and time-saving, dicobalt octacarbonyl is expensive and sensitive and difficult to store, resulting in high synthesis costs. Among them, dicobalt octacarbonyl is mainly prepared by reacting cobalt salts with synthesis gas (CO, H2) under high temperature and high pressure conditions in an inert solvent, resulting in high operating conditions, complex production processes and safety risks in the synthesis process. The other method uses cobalt salts as the cobalt source. Cobalt salts are widely available and inexpensive, but the existing technology requires the use of precious metal catalysts, which increases costs, strict reaction conditions and complex operations.

[0009] In view of this, it is necessary to develop a synthesis method using cheap and readily available cobalt salts as a cobalt source, which is simple to operate, has low safety risks, and has low synthesis costs to prepare CCTBA. Summary of the invention

[0010] The invention provides a method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl, which solves the problems of high synthesis cost, complex operation or high safety risk in the prior art.

[0011] The technical solution of the present invention is achieved in this way: A method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl, the specific scheme of which is as follows: Adding cobalt salt, reducing agent, methyl formate and catalyst into a high-pressure reactor, and making the reactor into an inert gas atmosphere, heating and stirring; then cooling the high-pressure reactor to room temperature, releasing gas, filtering the reaction liquid, and putting the filtrate into a normal pressure reaction device in an inert gas atmosphere; 3,3-dimethyl-1-butyne is added into the normal pressure reaction device, stirred at room temperature, filtered after the reaction is completed, and the obtained filtrate is post-treated to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl.

[0012] In some embodiments, the cobalt salt is one of cobalt iodide, cobalt sulfide, cobalt chloride, cobalt sulfate, and cobalt acetate, preferably cobalt iodide.

[0013] In some embodiments, the reducing agent is copper, zinc or manganese, preferably zinc.

[0014] In some embodiments, the molar ratio of the cobalt salt to the reducing agent is 1:2.0-3.0, preferably 1:2.1-2.3, and most preferably 1:2.1.

[0015] In some embodiments, the methyl formate is replaced by 2,4,6-trichlorophenyl formate or diethyl oxalate, preferably methyl formate, with a concentration of 0.1M.

[0016] In some embodiments, the catalyst is [RuCl2(PPh3)3], PdCl2(PPh3)2 or Pd(OAc)2. [RuCl2(PPh3)3] is preferred, and the amount used is 0.25-0.5 mol%.

[0017] In some embodiments, the molar ratio of the cobalt salt to 3,3-dimethyl-1-butyne is 1:0.5-1.0, preferably 1:0.6-0.8, and most preferably 1:0.6.

[0018] In some embodiments, the filtration process uses a sand core filtration device.

[0019] In some embodiments, the post-treatment is performed by vacuum distillation.

[0020] In some embodiments, the reduced pressure distillation removes the front and rear fractions at a ratio of 3-5% of the (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl content, and the obtained middle fraction is the crude (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl. At a vacuum degree of 2.4 mbar, the boiling point of pure (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl is 60°C.

[0021] In some embodiments, the crude (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl is distilled to obtain a pure (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl.

[0022] In some embodiments, the temperature during the heating and stirring is 100-140°C.

[0023] In some embodiments, the heating and stirring time is 6-8 hours; and the stirring at room temperature is 3-4 hours.

[0024] In some embodiments, the cobalt salt is cobalt iodide, and the amount used is 31.2 grams; the reducing agent is zinc particles, and the amount used is 13.7 grams; the catalyst is [RuCl2(PPh3)3], and the amount used is 0.48 grams; the amount of methyl formate used is 64 mL.

[0025] Compared with the prior art, the present invention has the following beneficial effects: The present invention uses methyl formate, 2,4,6-trichlorophenyl formate or diethyl oxalate to replace carbon monoxide, which reduces the operation risk, is simple to operate and has high synthesis efficiency; carbon monoxide is flammable, toxic and environmentally unfriendly, and is also difficult to handle and store.

[0026] (2) The present invention uses cheap and readily available cobalt salt as a raw material and a relatively cheap catalyst, and the synthesis cost is low; the catalyst can also promote the redox reaction between the cobalt salt and copper, thereby promoting the reaction effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0028] Figure 1This is the H NMR spectrum of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl prepared in Example 1.

[0029] Figure 2 This is the carbon NMR spectrum of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl prepared in Example 1. DETAILED DESCRIPTION

[0030] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0031] The reagents and equipment used in the following examples are all commercially available.

[0032] Example 1 31.2 g of cobalt iodide, 13.4 g of 200 mesh copper powder, 0.24 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 100°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was subjected to reduced pressure distillation to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0033] The reaction equation of the above process is as follows: .

[0034] The filtration process uses a sand core filtration device.

[0035] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 75%.

[0036] Example 2 31.2 g of cobalt iodide, 13.7 g of zinc particles, 0.24 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 100°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was distilled under reduced pressure to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0037] The reaction equation of the above process is as follows: .

[0038] The filtration process uses a sand core filtration device.

[0039] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 90%.

[0040] Example 3 31.2 g of cobalt iodide, 11.5 g of 200 mesh manganese powder, 0.24 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 100°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was subjected to reduced pressure distillation to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0041] The reaction equation of the above process is as follows: .

[0042] The filtration process uses a sand core filtration device.

[0043] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 85%.

[0044] Example 4 31.2 g of cobalt iodide, 13.7 g of zinc particles, 0.48 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 100°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was distilled under reduced pressure to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0045] The reaction equation of the above process is as follows: .

[0046] The filtration process uses a sand core filtration device.

[0047] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 92%.

[0048] Example 5 9.1 g of cobalt sulfide, 13.7 g of zinc particles, 0.48 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 100°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was distilled under reduced pressure to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0049] The reaction equation of the above process is as follows: .

[0050] The filtration process uses a sand core filtration device.

[0051] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 87%.

[0052] Example 6 17.7 g of cobalt acetate, 13.7 g of zinc particles, 0.48 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 100°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was distilled under reduced pressure to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0053] The reaction equation of the above process is as follows: .

[0054] The filtration process uses a sand core filtration device.

[0055] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 71%.

[0056] Example 7 31.2 g of cobalt iodide, 13.7 g of zinc particles, 0.48 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 140°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was distilled under reduced pressure to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0057] The vacuum distillation removes the front and rear fractions according to the ratio of 3-5% of the content of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl, and the obtained middle fraction is the crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl. Under a vacuum degree of 2.4 mbar, the boiling point of pure (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl is 60°C.

[0058] The reaction equation of the above process is as follows: .

[0059] The filtration process uses a sand core filtration device.

[0060] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 94%.

[0061] Example 8 31.2 g of cobalt iodide, 13.7 g of zinc particles, 0.35 g of PdCl2(PPh3)2, and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 140°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was distilled under reduced pressure to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0062] The reaction equation of the above process is as follows: .

[0063] The filtration process uses a sand core filtration device.

[0064] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 82%.

[0065] Example 9 31.2 g of cobalt iodide, 13.7 g of zinc particles, 0.11 g of Pd(OAc)2, and 64 mL of methyl formate were added to a high-pressure reactor to place the reactor in an inert gas atmosphere; after the reactor was sealed, the reactor heating device was turned on, the temperature was set to 140°C, and stirring in the equipment was turned on at the same time, and the temperature was lowered after 6 hours; the temperature was lowered to room temperature, the gas in the reactor was released, the reaction liquid was filtered, and the filtrate was put into a normal pressure reaction device with an inert gas atmosphere, and 4.9 g of 3,3-dimethyl-1-butyne was added; it was stirred at room temperature for 3 hours; after the reaction was completed, it was filtered, and the obtained filtrate was subjected to reduced pressure distillation to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then the pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl was obtained by distillation.

[0066] The reaction equation of the above process is as follows: .

[0067] The filtration process uses a sand core filtration device.

[0068] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 73%.

[0069] Example 10 Add 31.2g of cobalt iodide, 13.7g of zinc particles, 0.48g of [RuCl2(PPh3)3], and 64mL of 2,4,6-trichlorophenyl formate into a high-pressure reactor, and place the reactor in an inert gas atmosphere; after the reactor is sealed, turn on the reactor heating device, set the temperature to 140°C, and start stirring in the equipment at the same time, and cool down after 6 hours; cool down to room temperature, release the gas in the reactor, filter the reaction liquid, and put the filtrate into a normal pressure reaction device with an inert gas atmosphere, add 4.9g of 3,3-dimethyl-1-butyne; stir at room temperature for 3 hours; filter after the reaction is completed, and use reduced pressure distillation to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl; and then obtain a pure product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl by distillation.

[0070] The reaction equation of the above process is as follows: .

[0071] The filtration process uses a sand core filtration device.

[0072] The yield of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl synthesized in this experiment is 88%.

[0073] The comparison components are detailed in the following table: .

[0074] In summary, when 31.2 g of cobalt iodide, 13.7 g of zinc particles, 0.48 g of [RuCl2(PPh3)3], and 64 mL of methyl formate were used, the yield reached 94%, which was the optimal ratio.

[0075] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl, characterized in that: include: Adding cobalt salt, reducing agent, methyl formate and catalyst into a high-pressure reactor, and making the reactor into an inert gas atmosphere, heating and stirring; then cooling the high-pressure reactor to room temperature, releasing gas, filtering the reaction liquid, and putting the filtrate into a normal pressure reaction device in an inert gas atmosphere; 3,3-dimethyl-1-butyne is added into the normal pressure reaction device, stirred at room temperature, filtered after the reaction is completed, and the obtained filtrate is post-treated to obtain a crude product of (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl.

2. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The cobalt salt is one of cobalt iodide, cobalt sulfide, cobalt chloride, cobalt sulfate and cobalt acetate.

3. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The reducing agent is copper, zinc or manganese.

4. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The molar ratio of the cobalt salt to the reducing agent is 1:2.1-3.0, and the preferred molar ratio is 1:2.

1.

5. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The methyl formate is replaced by 2,4,6-trichlorophenyl formate or diethyl oxalate.

6. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The catalyst is [RuCl2(PPh3)3], PdCl2(PPh3)2 or Pd(OAc)2.

7. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The molar ratio of the cobalt salt to 3,3-dimethyl-1-butyne is 1:0.5-1.0, and the preferred molar ratio is 1:0.

6.

8. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The filtering process adopts a sand core filtering device.

9. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The post-treatment is carried out by vacuum distillation.

10. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The crude (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl product is distilled to obtain a pure (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl product.

11. The method for preparing (3,3-dimethyl-1-butyne) dicobalt hexacarbonyl according to claim 1, characterized in that: The temperature during the heating and stirring is 100-140°C.

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