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Preparation method of difluoroboron-bridged ethyldiketone dioxime cobalt complex

A technology based on ethylenedionedioxime and difluoroboron, which is applied in the field of preparation of ethylenedionedioxime cobalt complex, can solve the problems of low yield and purity, unfriendly environment, difficult purification, etc., and achieve optimal reaction conditions , Improve product purity, improve the effect of safety performance

Active Publication Date: 2018-09-14
NIPPON PAINT GUANGZHOU +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention solves serious problems such as low yield and purity and difficult purification in the prior art, as well as other problems such as the use of a large amount of organic low-boiling-point and highly toxic solvents, unfriendly environment, time-consuming, high cost, etc.

Method used

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  • Preparation method of difluoroboron-bridged ethyldiketone dioxime cobalt complex
  • Preparation method of difluoroboron-bridged ethyldiketone dioxime cobalt complex
  • Preparation method of difluoroboron-bridged ethyldiketone dioxime cobalt complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0089] Embodiment 1~3: Synthesis of COBF

[0090] The general steps are as follows:

[0091] Under nitrogen atmosphere, add cobalt(II) acetate tetrahydrate (2.000 g), dimethylglyoxime (1.900 g), tetrahydrofuran (abbreviated as THF) in a 100-mL eggplant-type reaction flask at room temperature or under heating (40ml), after mixing and stirring for 15 to 30 minutes, slowly add boron trifluoride etherate complex (10ml) dropwise, and the addition was completed in about 15 to 30 minutes. Then continue stirring at room temperature or under heating conditions (20-65° C.) for 6-9 hours. The obtained dark brown precipitate was separated by suction filtration with filter paper or a sand core funnel, and then dried in vacuum or reduced pressure to obtain the crude difluoroboryl-bridged ethylenedionedioxime cobalt complex (hereinafter referred to as the crude product).

[0092] The purification steps are as follows: mix the crude product with methanol (6 times the mass of the crude produ...

Embodiment 4～6

[0095] Embodiment 4~6: the synthesis of COPhBF

[0096] Similarly, the general steps are as follows:

[0097] Under nitrogen atmosphere, at room temperature or under heating (20~65 ℃), add cobalt (II) acetate tetrahydrate (1.000 g), biphenyl dioxime (1.930 g) in a 100-ml eggplant type reaction flask, Tetrahydrofuran (20ml), after mixing and stirring for 15-30 minutes, slowly added boron trifluoride etherate (5ml) dropwise, and the addition was completed in about 15-30 minutes. Then continue to stir for 6-9 hours at room temperature or under heating (20-65° C.). The obtained dark brown precipitate was separated by suction filtration with filter paper or a sand core funnel, and then dried in vacuum or reduced pressure to obtain a crude product.

[0098]The purification steps are as follows: mix the crude product with a small amount of methanol (6 times the mass of the crude product), stir for about 30 minutes or sonicate for 3 to 10 minutes, then filter again, and dry the resu...

Embodiment 3

[0101] The products purified twice in Example 3 and Example 6 are respectively COBF and COPhBF, and the elemental analysis results of the two are consistent with the theoretical values ​​(see Table 4).

[0102] Table 3: Synthesis and purification of COBF and

[0103] Synthesis and purification of embodiment 4~6COPhBF

[0104]

[0105]

[0106] ^ In order to simplify the calculation, the calculation of the yield in the examples of the present invention is based on the dihydrate of cobalt difluoroboryldioxime: such as COBF dihydrate, molecular weight 420.78; CoPhBF dihydrate, molecular weight 669.06, that is, water molecules as axial body and cobalt coordination. Because methanol was used as the purification solvent, the obtained products contained methanol as the axial ligand, and the corresponding molecular weights were 449.08 and 697.12, respectively. Unless otherwise stated, the calculations of the yields in the examples of the present invention are based on the dih...

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Abstract

The invention discloses a preparation method of a difluoroboron-bridged ethyldiketone dioxime cobalt complex. A molecular formula is as shown in the description, wherein R1, R2, R3 and R4 are hydrogen(H) or substituent groups which can be identical or different or can be independent or belong to cyclic substituent groups; and L1 and L2 are axial ligands which are solvents or water molecules withweaker coordination ability. The preparation method comprises the following steps: under nitrogen gas or inert gas atmosphere, mixing and stirring divalent cobalt salt and ethyldiketone dioxime ligandwith a reaction solvent; adding a boron trifluoride ether complex, performing stirring reaction at room temperature or under the condition of heating or ice water bath, and then, filtering the obtained reaction mixture to obtain a precipitate, namely a crude product; and mixing and stirring the crude product with a purification solvent of which the polarity is not lower than isobutanol or water for 5-30min or performing ultrasonic treatment for 1-10min, then performing filtration, and performing drying in vacuum or drying under reduced pressure to obtain a purified difluoroboron-bridged ethyldiketone dioxime cobalt complex. The method disclosed by the invention simplifies the purification steps and increases the yield.

Description

technical field [0001] The invention belongs to the technical field of metal-organic complex materials, and in particular relates to a preparation method and application of ethylenedionedioxime cobalt complex. Background technique [0002] Bis[(difluoroboryl) ethylenedionedioxime subunit] cobalt acid complex (hereinafter referred to as difluoroboryldioxime cobalt complex), the molecular formula is [0003] Among them, R 1 , R 2 , R 3 , R 4 It is hydrogen (H) or a substituent group, which can be the same or different, and can be independent or belong to the same cyclic substituent group, L 1 and L 2 As an axial ligand, as a solvent or water molecule with weak coordination ability, it can be used as a very efficient catalyst for catalyzing chain transfer polymerization. Catalyzed chain transfer polymerization can be used to synthesize macromonomers, which can be further copolymerized with other monomers to form graft copolymers. Graft copolymers are widely used in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/06
CPCC07F15/065
Inventor 胡剑蒋隆恒
Owner NIPPON PAINT GUANGZHOU