Synthesis method of high-purity cobalt complex precursor

The reaction method of urea and choline chloride is used to prepare a deep eutectic solvent, combined with cobalt chloride, 2,2,6,6-tetramethyl-3,5-heptadene, triethylamine and hydrogen peroxide, the problems of low yield, high cost and unenvironmental synthesis of cobalt tris(2,2,6,6-tetramethyl-3,5-heptadene) in the prior art are solved, and the synthesis of high-purity cobalt complex precursors is achieved.

CN119504390APending Publication Date: 2025-02-25ANHUI ARGOSUN NEW ELECTRONIC MATERIALS CO LTD +1
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Patent Information

Application Number
CN202411427211.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-14
Publication Date
2025-02-25

AI Technical Summary

Technical Problem

In the prior art, the method of synthesizing tris(2,2,6,6-tetramethyl-3,5-heptanedione) cobalt has low yield, high cost, insufficient environmental protection, and large solvent usage and many by-products.

Method used

The deep eutectic solvent was prepared by reacting urea and choline chloride, and cobalt chloride, 2,2,6,6-tetramethyl-3,5-heptanedione, triethylamine and hydrogen peroxide were added to the system in turn for reaction. After filtration, the filtrate was recycled and reused, and the solid was dried and sublimated to obtain the target product.

Benefits of technology

It greatly reduces the use of conventional organic solvents, is more environmentally friendly, and reduces production costs. The deep eutectic solvent can be reused 5 times without significant changes in the product yield, the reaction process is calm, the energy consumption is low, and the safety is high.

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Abstract

The invention discloses a synthesis method of a high-purity cobalt complex precursor, which comprises the following steps: reacting urea with choline chloride to prepare a deep eutectic solvent, sequentially adding cobalt chloride, 2, 2, 6, 6-tetramethyl-3, 5-heptadione, triethylamine, hydrogen peroxide and other raw materials into the system, reacting, filtering after the reaction is finished, and recycling the filtrate, thereby obtaining the high-purity cobalt complex precursor. The solid is dried and sublimated to obtain a target product, and the deep eutectic solvent is used for replacing a traditional organic reagent, so that the use amount of the conventional organic solvent is greatly reduced, the method is more environment-friendly and can be repeatedly used, and the production cost is reduced; the deep eutectic solvent is recycled for 5 times, the product yield is not obviously changed, the operation conditions of the whole process are convenient, and the target product is obtained by a one-pot method; the reaction process is mild, low in energy consumption and high in safety; the raw materials are wide and cheap, the product yield is high, and the process stability is good; and other metal ions are not introduced in the whole reaction system except the metal cobalt, so that the product metal purity is high.
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Description

Technical Field

[0001] The invention relates to the technical field of organometallic compound synthesis, and in particular to a method for synthesizing a high-purity cobalt complex precursor. Background Art

[0002] As a semiconductor functional material, cobalt oxide (CoOx) is often used to make gas sensor materials, electromagnetic equipment materials, lithium-ion battery negative electrode materials, etc. due to its stable chemical properties, unique magnetic properties and high electrochemical energy storage capacity. In recent years, ultra-thin CoOx films have attracted more and more attention due to their excellent electrochemical catalytic properties.

[0003] Many methods for preparing CoOx thin films have been reported, including chemical vapor deposition (CVD), physical vapor deposition (PVD), laser pulse deposition (PLD), atomic layer deposition (ALD) and other methods. Among them, the atomic layer deposition method has been increasingly recognized due to its self-limiting characteristics and excellent three-dimensional structural conformality. Tris(2,2,6,6-tetramethyl-3,5-heptanedione)cobalt [Co(tmhd)3], as a source precursor for depositing cobalt oxide thin films, has gradually come into people's field of vision in recent years.

[0004] At present, in the prior art, the methods for synthesizing tris(2,2,6,6-tetramethyl-3,5-heptanedione)cobalt mainly include:

[0005] 1. Using cobalt carbonate or cobalt dichloride hexahydrate as raw material and hydrogen peroxide as oxidant, the yield is only 13%-25% [3,4], which is relatively low.

[0006] 2. First synthesize the di(2,2,6,6-tetramethyl-3,5-heptanedione)cobalt intermediate Co(tmhd)2, and then react it with oxygen in the air or directly with oxygen in n-hexane or ethanol solvent. The yield is 45%-75%. If 2,2,6,6-tetramethyl-3,5-heptanedione is used as both a reactant and a solvent, the yield can be increased to 95%. The amount of solvent used is relatively high, there are many by-products, and it is not environmentally friendly.

[0007] 3. Using cobalt oxide as raw material, 2,2,6,6-tetramethyl-3,5-heptanedione as solvent and reactant, and oxygen as oxidant, the yield can reach 85%. 2,2,6,6-tetramethyl-3,5-heptanedione is expensive and the cost is too high. Summary of the invention

[0008] The purpose of the present invention is to provide a method for synthesizing a high-purity cobalt complex precursor to solve the above-mentioned deficiencies in the prior art.

[0009] In order to achieve the above object, the present invention provides the following technical solutions:

[0010] A method for synthesizing a high-purity cobalt complex precursor, the method comprising the following steps:

[0011] S1: Add urea (125 g, 2.08 mol)-(375 g, 6.24 mol) and choline chloride (387.2 g, 2.77 mol)-(193.6 g, 1.39 mol) into the reaction bottle, and heat to 80°C. The system slowly turns into a colorless transparent solution and then slowly returns to room temperature;

[0012] S2: Cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6 g, 0.23 mol) and triethylamine (15.6 g, 0.15 mol) were added to the reaction system in sequence, and the temperature was raised to 60-90°C;

[0013] S3: add 10% hydrogen peroxide (6.8 g, 0.02 mol)-(34 g, 0.1 mol) dropwise, and react for 12 hours;

[0014] S4: Filter, set aside the filtrate, wash the solid with 20 ml of n-hexane three times, dry, and sublime the crude product (120° / 0.5 mm) to obtain tris(2,2,6,6-tetramethyl-3,5-heptanedione)cobalt;

[0015] S5: Add cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6 g, 0.23 mol) and triethylamine (15.6 g, 0.15 mol) to the filtrate filtered during treatment, and heat to 60-90°C;

[0016] S6: dropwise add 10% hydrogen peroxide (6.8 g, 0.02 mol)-(34 g, 0.1 mol), react at room temperature for 12 hours, filter through a funnel, recycle the filtrate, wash the solid with n-hexane, dry, and sublime;

[0017] The funnel includes a shaking component, which is used to shake the filtered solids to improve the filtering efficiency.

[0018] Preferably, in step S2 and step S5, the temperature is raised to 80°C.

[0019] Preferably, in steps S3 and S6, hydrogen peroxide (20.4 g, 0.06 mol) with a mass fraction of 10% is added dropwise.

[0020] Preferably, it comprises a funnel body and a straight tube, the straight tube is detachably provided with filter paper, and the shaking assembly comprises a shaking frame slidably provided on the straight tube;

[0021] The straight tube is provided with a locking groove, a supporting block is fixedly provided on the funnel body, a locking block is fixedly provided on the supporting block, and the locking block is engaged and connected with the locking groove;

[0022] Also included is a clamping assembly, which is used to clamp the filter paper.

[0023] Preferably, a rotating block is rotatably provided on the straight tube, a guide groove is provided on the rotating block, a lifting block is fixedly provided on the shaking frame, and the lifting block is slidably provided in the guide groove.

[0024] Preferably, a sliding rod is slidably provided on the straight tube, a polygonal rod is rotatably provided on the sliding rod, and the polygonal rod is slidably connected to the rotating block.

[0025] Preferably, the clamping assembly comprises a clamping rod rotatably arranged on a straight tube, a round tube is slidably arranged on the straight tube, a protrusion is fixedly arranged on the round tube, a limiting groove is arranged on the clamping rod, and the protrusion is slidably arranged in the limiting groove.

[0026] Preferably, a lifting rod is fixedly provided on the polygonal rod, and the lifting rod is rotatably connected to the circular tube.

[0027] Preferably, a spring is provided between the straight tube and the sliding rod, and two ends of the spring are fixedly connected to the straight tube and the sliding rod respectively.

[0028] Preferably, a driving motor is fixedly provided on the sliding rod, and an output shaft of the driving motor is fixedly connected to the polygonal rod.

[0029] In the above technical scheme, the method for synthesizing a high-purity cobalt complex precursor provided by the present invention has the beneficial effects of:

[0030] A deep eutectic solvent is prepared by the reaction of urea and choline chloride, and then raw materials such as cobalt chloride, 2,2,6,6-tetramethyl-3,5-heptanedione, triethylamine, hydrogen peroxide, etc. are added into the system in sequence for reaction. After the reaction is completed, the filtrate is filtered, the filtrate is recovered and reused, and the solid is dried and sublimated to obtain the target product. In addition, the deep eutectic solvent is recycled for 5 times without significant change in product yield, which greatly reduces the use of conventional organic solvents, is more green and environmentally friendly, and can be reused to reduce production costs.

[0031] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.

[0032] This application document provides an overview of various implementations or examples of the technology described in the present disclosure, and is not a comprehensive disclosure of the entire scope or all features of the disclosed technology. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0034] Figure 1 A schematic diagram of the funnel main body structure provided by an embodiment of the present invention;

[0035] Figure 2 A cross-sectional view of a funnel body provided by an embodiment of the present invention;

[0036] Figure 3 The embodiment of the present invention provides Figure 2 A in the enlarged view;

[0037] Figure 4 A schematic diagram of the support block and the locking slot structure provided by an embodiment of the present invention;

[0038] Figure 5 A schematic diagram of a circular tube structure provided by an embodiment of the present invention;

[0039] Figure 6 A statistical graph showing the yield and the number of deep eutectic solvent cycles provided in an embodiment of the present invention.

[0040] Description of reference numerals:

[0041] 1. Funnel body; 2. Filter paper; 3. Shaking frame; 31. Lifting block; 4. Support block; 41. Locking block; 5. Straight tube; 51. Rotating block; 52. Guide groove; 53. Clamping rod; 54. Limiting groove; 55. Locking groove; 6. Sliding rod; 61. Polygonal rod; 62. Spring; 63. Driving motor; 64. Lifting rod, 7. Round tube; 71. Bump. DETAILED DESCRIPTION

[0042] In order to make the purpose, technical solution and advantages of the embodiments of the present disclosure clearer, the technical solution of the embodiments of the present disclosure will be clearly and completely described below in conjunction with the drawings of the embodiments of the present disclosure. Obviously, the described embodiments are part of the embodiments of the present disclosure, not all of the embodiments. Based on the described embodiments of the present disclosure, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present disclosure.

[0043] Please refer to 1-6, a method for synthesizing a high-purity cobalt complex precursor, characterized in that the method for synthesizing a high-purity cobalt complex precursor comprises the following steps:

[0044] S1: Add urea (125 g, 2.08 mol)-(375 g, 6.24 mol) and choline chloride (387.2 g, 2.77 mol)-(193.6 g, 1.39 mol) into the reaction bottle, and heat to 80°C. The system slowly turns into a colorless transparent solution and then slowly returns to room temperature;

[0045] S2: Cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6 g, 0.23 mol) and triethylamine (15.6 g, 0.15 mol) were added to the reaction system in sequence, and the temperature was raised to 60-90°C;

[0046] S3: add 10% hydrogen peroxide (6.8 g, 0.02 mol)-(34 g, 0.1 mol) dropwise, and react for 12 hours;

[0047] S4: Filter, set aside the filtrate, wash the solid with 20 ml of n-hexane three times, dry, and sublime the crude product (120° / 0.5 mm) to obtain tris(2,2,6,6-tetramethyl-3,5-heptanedione)cobalt;

[0048] S5: Add cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6 g, 0.23 mol) and triethylamine (15.6 g, 0.15 mol) to the filtrate filtered during treatment, and heat to 60-90°C;

[0049] S6: dropwise add 10% hydrogen peroxide (6.8 g, 0.02 mol)-(34 g, 0.1 mol), react at room temperature for 12 hours, filter through a funnel, recycle the filtrate, wash the solid with n-hexane, dry, and sublime;

[0050] The funnel includes a shaking component, which is used to shake the filtered solids to improve the filtering efficiency.

[0051] In step S2 and step S5, the temperature is raised to 80°C.

[0052] In the steps S3 and S6, hydrogen peroxide (20.4 g, 0.06 mol) with a mass fraction of 10% is added dropwise;

[0053] Embodiment 1:

[0054] Add urea (125g, 2.08mol) and choline chloride (387.2g, 2.77mol) to the reaction bottle, heat to 80°C, the system slowly becomes a colorless transparent solution, and then slowly returns to room temperature. Add cobalt chloride (10g, 0.08mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6g, 0.23mol) and triethylamine (15.6g, 0.15mol) to the reaction system in sequence, heat to 60°C, add 10% hydrogen peroxide (6.8g, 0.02mol) by mass fraction, react at room temperature for 12 hours, filter, and set aside the filtrate. Wash the solid with 20 ml of n-hexane 3 times, dry, and sublimate the crude product (120° / 0.5mm) to obtain 30.7 grams of the product with a yield of 63%.

[0055] Embodiment 2:

[0056] Add urea (250 g, 4.16 mol) and choline chloride (290.6 g, 2.08 mol) to the reaction bottle, heat to 80 ° C, the system slowly turns into a colorless transparent solution, and then slowly returns to room temperature. Add cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6 g, 0.23 mol) and triethylamine (15.6 g, 0.15 mol) to the reaction system in sequence. The temperature was raised to 80°C, and 10% hydrogen peroxide (20.4 g, 0.06 mol) was added dropwise. After the addition was completed, the mixture was reacted at room temperature for 12 hours, filtered, and the filtrate was reserved. The solid was washed three times with 20 ml of n-hexane and dried. The crude product was sublimated (120° / 0.5 mm) to obtain 44.8 g of the product with a yield of 92%. The purity of the product was detected by inductively coupled plasma mass spectrometry (ICP-MS), and the results showed that the metal purity of the product was 5N.

[0057] Embodiment 3:

[0058] Add urea (375g, 6.24mol) and choline chloride (193.6g, 1.39mol) to the reaction bottle, heat to 80°C, the system slowly becomes a colorless transparent solution, and then slowly returns to room temperature. Add cobalt chloride (10g, 0.08mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6g, 0.23mol) and triethylamine (15.6g, 0.15mol) to the reaction system in sequence, heat to 90°C, add 10% hydrogen peroxide (34g, 0.1mol) dropwise, react at room temperature for 12 hours, filter, and set aside the filtrate. Wash the solid with 20 ml of n-hexane 3 times, dry, and sublimate the crude product (120° / 0.5mm) to obtain 35.1 grams of the product with a yield of 72%.

[0059] Comparative Example 1:

[0060] To the reaction flask, cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptane (42.6 g, 0.23 mol), triethylamine (15.6 g, 0.15 mol) and 200 ml of n-hexane were added in sequence, the temperature was raised to 80°C, 10% hydrogen peroxide (20.4 g, 0.06 mol) was added dropwise, the reaction was continued at room temperature for 12 hours, filtered, and the filtrate was reserved. The solid was washed 3 times with 20 ml of n-hexane, dried, and the crude product was sublimed (120° / 0.5 mm) to obtain 38 g of product with a yield of 78%.

[0061] Comparative Example 2:

[0062] Add urea (250g, 4.16mol) and choline chloride (290.6g, 2.08mol) to the reaction bottle, heat to 80°C, the system slowly becomes a colorless transparent solution, and then slowly returns to room temperature. Add cobalt chloride (10g, 0.08mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6g, 0.23mol) and sodium hydroxide (6g, 0.15mol) to the reaction system in sequence, heat to 80°C, add 10% hydrogen peroxide (20.4g, 0.06mol) dropwise, react at room temperature for 12 hours, filter, and set aside the filtrate. Wash the solid with 20 ml of n-hexane 3 times, dry, and sublimate the crude product (120° / 0.5mm) to obtain 43.3 grams of the product with a yield of 89%. The purity of the product was tested using inductively coupled plasma mass spectrometry (ICP-MS), and the results showed that the sodium residue was 74 ppm and the metal purity of the product was 4N.

[0063] In summary, a deep eutectic solvent is prepared by the reaction of urea and choline chloride, and then raw materials such as cobalt chloride, 2,2,6,6-tetramethyl-3,5-heptanedione, triethylamine, hydrogen peroxide, etc. are added to the system in turn for reaction. After the reaction is completed, the reaction is filtered, the filtrate is recovered and reused, and the solid is dried and sublimated to obtain the target product. The deep eutectic solvent is used to replace the traditional organic reagent, which greatly reduces the use of conventional organic solvents, is more environmentally friendly, and can be reused to reduce production costs. The deep eutectic solvent is recycled 5 times without a significant change in product yield. The operating conditions of the entire process are convenient, and the target product is obtained by a one-pot method. The reaction process is gentle, energy consumption is low, and safety is high. The raw materials are widely available and cheap, the product yield is high, and the process stability is good. In addition to metallic cobalt, no other metal ions are introduced into the entire reaction system, and the product metal purity is high, which meets the requirements of the semiconductor field for product metal purity.

[0064] Yield (%) Example 1 63 Example 2 92 Example 3 72 Comparative Example 1 78

[0065] It can be seen from the data in the above table that the synthesis method of the high-purity cobalt complex precursor provided by the present invention not only reduces the usage of conventional organic solvents, but also ensures the product yield. At the same time, the deep eutectic solvent prepared by the reaction of urea and choline chloride can be repeatedly recycled, and the effect of repeated use on the yield is shown in the attached Figure 6 ;

[0066] At the same time, in combination with Example 2 and Comparative Example 2, it is concluded that by replacing sodium hydroxide with an equivalent amount of triethylamine, the product yield and purity can be effectively improved, and the acid produced in the reaction is absorbed by triethylamine to prevent it from having a negative impact on the reaction, thereby ensuring the smooth progress of the reaction, thereby improving the recycling effect of the deep eutectic solvent.

[0067] Specifically, it includes a funnel body 1 and a straight tube 5, on which a filter paper 2 is detachably arranged, and a shaking assembly includes a shaking frame 3 slidably arranged on the straight tube 5; the straight tube 5 is provided with a locking groove 55, and a support block 4 is fixedly arranged on the funnel body 1, and a locking block 41 is fixedly arranged on the support block 4, and the locking block 41 is engaged and connected with the locking groove 55; it also includes a clamping assembly, which is used to clamp the filter paper 2. By setting the filter paper 2 on the straight tube 5, the filter paper 2 can be lifted and can be more portable when separating the generated solid and liquid. Replacement is carried out, and a shaking frame 3 is set to prevent solid precipitation when the shaking frame 3 slides up and down. After the filtration is completed, the liquid adhering to the solid can be further separated by shaking the shaking frame 3, which causes clogging of the filter paper 2 and affects the filtration efficiency. At the same time, the straight tube 5 is fixed by the engagement of the locking block 41 and the locking groove 55, and the filter paper 2 is clamped by the clamping assembly, which improves the stability of the filter paper 2 during the filtration process and prevents the filter paper 2 from being offset, which affects the filtration effect.

[0068] In an embodiment further provided by the present invention, a rotating block 51 is rotatably provided on the straight tube 5, a guide groove 52 is provided on the rotating block 51, a lifting block 31 is fixedly provided on the shaking frame 3, and the lifting block 31 is slidably provided in the guide groove 52. When the rotating block 51 rotates, the lifting block 31 cooperates with the guide groove 52 and makes the lifting block 31 slide back and forth with the shaking frame 3 to prevent the solid from precipitating during the filtration process and affecting the filtration effect, and at the same time drive the solid to shake to avoid excessive liquid adhering to the solid, which affects the filtration effect.

[0069] Furthermore, a sliding rod 6 is slidably provided on the straight tube 5, and a polygonal rod 61 is rotatably provided on the sliding rod 6. The polygonal rod 61 is slidably connected to the rotating block 51. A driving motor 63 is fixedly provided on the sliding rod 6, and an output shaft of the driving motor 63 is fixedly connected to the polygonal rod 61. The polygonal rod 61 is driven to rotate by the driving motor 63, and the rotation of the polygonal rod 61 drives the rotating block 51 to rotate, thereby realizing the up and down reciprocating sliding of the shaking frame 3.

[0070] Furthermore, the clamping assembly includes a clamping rod 53 rotatably set on the straight tube 5, a round tube 7 is slidably set on the straight tube 5, a protrusion 71 is fixedly set on the round tube 7, a limiting groove 54 is set on the clamping rod 53, and the protrusion 71 is slidably set in the limiting groove 54. When the round tube 7 slides up and down, the clamping rod 53 is rotated to cooperate with the baffle on the straight tube 5 through the action of the protrusion 71 and the limiting groove 54 to clamp the filter paper 2, thereby improving the portability of replacing the filter paper 2.

[0071] In an embodiment further provided by the present invention, a lifting rod 64 is fixedly provided on the polygonal rod 61, and the lifting rod 64 is rotatably connected to the circular tube 7. When the polygonal rod 61 slides along with the straight tube 5, the lifting rod 64 is driven to slide, so as to drive the circular tube 7 to make the protrusion 71 slide.

[0072] In the embodiment provided by the present invention, a spring 62 is arranged between the straight tube 5 and the sliding rod 6, and the two ends of the spring 62 are fixedly connected to the straight tube 5 and the sliding rod 6 respectively. When the sliding rod 6 is pressed, the polygonal rod 61 and the lifting rod 64 move downward at the same time, the spring 62 is stretched, and the clamping rod 53 releases the clamping of the filter paper 2. After replacing the filter paper 2, the sliding rod 6 is released, and under the resetting action of the spring 62, the clamping rod 53 clamps the filter paper 2.

[0073] Working principle: when fixing the filter paper 2, press the sliding rod 6 to compress the spring 62, so that the sliding rod 6 drives the polygonal rod and the lifting rod 64 to move downward, and the round tube 7 moves downward at the same time. When moving downward, the clamping rod 53 is rotated to cooperate with the baffle on the straight tube 5 through the cooperation of the protrusion 71 and the limit groove 54 to clamp the filter paper 2, and then the locking block 41 is aligned with the locking groove 55 and inserted, and the straight tube 5 is rotated to engage with the locking groove 55 to complete the installation of the filter paper 2. Then, during the filtering process, the polygonal rod 61 is driven to rotate by the driving motor 63, and the rotating block 51 is driven to rotate. Through the cooperation of the guide groove 52 on the rotating block 51 and the lifting block 31, the shaking frame 3 slides back and forth.

[0074] The above description is only by way of illustration of certain exemplary embodiments of the present invention. It is undoubted that those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A method for synthesizing a high-purity cobalt complex precursor, characterized in that: The synthesis method of the high-purity cobalt complex precursor comprises the following steps: S1: Add urea (125 g, 2.08 mol)-(375 g, 6.24 mol) and choline chloride (387.2 g, 2.77 mol)-(193.6 g, 1.39 mol) into the reaction bottle, and heat to 80°C. The system slowly turns into a colorless transparent solution and then slowly returns to room temperature; S2: Cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6 g, 0.23 mol) and triethylamine (15.6 g, 0.15 mol) were added to the reaction system in sequence, and the temperature was raised to 60-90°C; S3: add 10% hydrogen peroxide (6.8 g, 0.02 mol)-(34 g, 0.1 mol) dropwise, and react for 12 hours; S4: Filter, set aside the filtrate, wash the solid with 20 ml of n-hexane three times, dry, and sublime the crude product (120° / 0.5 mm) to obtain tris(2,2,6,6-tetramethyl-3,5-heptanedione)cobalt; S5: Add cobalt chloride (10 g, 0.08 mol), 2,2,6,6-tetramethyl-3,5-heptanedione (42.6 g, 0.23 mol) and triethylamine (15.6 g, 0.15 mol) to the filtrate filtered during treatment, and heat to 60-90°C; S6: dropwise add 10% hydrogen peroxide (6.8 g, 0.02 mol)-(34 g, 0.1 mol), react at room temperature for 12 hours, filter through a funnel, recycle the filtrate, wash the solid with n-hexane, dry, and sublime to obtain tris(2,2,6,6-tetramethyl-3,5-heptanedione)cobalt; The funnel includes a shaking component, which is used to shake the filtered solids to improve the filtering efficiency.

2. The method for synthesizing a high-purity cobalt complex precursor according to claim 1, characterized in that: In step S2 and step S5, the temperature is raised to 80°C.

3. The method for synthesizing a high-purity cobalt complex precursor according to claim 1, characterized in that: In the steps S3 and S6, hydrogen peroxide (20.4 g, 0.06 mol) with a mass fraction of 10% is added dropwise.

4. The method for synthesizing a high-purity cobalt complex precursor according to claim 1, characterized in that: It comprises a funnel body (1) and a straight tube (5), wherein the straight tube (5) is detachably provided with filter paper (2), and the shaking assembly comprises a shaking frame (3) slidably provided on the straight tube (5); The straight tube (5) is provided with a locking groove (55), a supporting block (4) is fixedly provided on the funnel body (1), a locking block (41) is fixedly provided on the supporting block (4), and the locking block (41) is engaged and connected with the locking groove (55); It also comprises a clamping assembly, which is used to clamp the filter paper (2).

5. The method for synthesizing a high-purity cobalt complex precursor according to claim 4, characterized in that: A rotating block (51) is rotatably arranged on the straight tube (5), and a guide groove (52) is arranged on the rotating block (51). A lifting block (31) is fixedly arranged on the shaking frame (3), and the lifting block (31) is slidably arranged in the guide groove (52).

6. The method for synthesizing a high-purity cobalt complex precursor according to claim 5, characterized in that: A sliding rod (6) is slidably arranged on the straight tube (5), a polygonal rod (61) is rotatably arranged on the sliding rod (6), and the polygonal rod (61) is slidably connected to the rotating block (51).

7. The method for synthesizing a high-purity cobalt complex precursor according to claim 6, characterized in that: The clamping assembly comprises a clamping rod (53) rotatably arranged on a straight tube (5), a round tube (7) is slidably arranged on the straight tube (5), a protrusion (71) is fixedly arranged on the round tube (7), a limiting groove (54) is arranged on the clamping rod (53), and the protrusion (71) is slidably arranged in the limiting groove (54).

8. The method for synthesizing a high-purity cobalt complex precursor according to claim 7, characterized in that: A lifting rod (64) is fixedly arranged on the polygonal rod (61), and the lifting rod (64) is rotatably connected to the circular tube (7).

9. The method for synthesizing a high-purity cobalt complex precursor according to claim 6, characterized in that: A spring (62) is provided between the straight tube (5) and the sliding rod (6), and two ends of the spring (62) are fixedly connected to the straight tube (5) and the sliding rod (6) respectively.

10. The method for synthesizing a high-purity cobalt complex precursor according to claim 6, characterized in that: A driving motor (63) is fixedly arranged on the sliding rod (6), and an output shaft of the driving motor (63) is fixedly connected to the polygonal rod (61).

Citation Information

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