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Nickel metal complex as well as preparation method and application thereof

A technology of metal complexes and reactions, which is applied in the direction of nickel organic compounds, etc., can solve the problems of poor solubility of alkali metal fluoride salts, difficulty in industrial scale-up, and inability to obtain the degree of polymerization, etc., so as to reduce the amount of solvent used, the conditions are not harsh, and the polymerization The effect of cost reduction

Inactive Publication Date: 2021-03-12
浙江诺亚氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the strong water absorption of CsF, the degree of polymerization is low and the yield is low.
[0007] The K-type perfluoropolyether obtained according to the polymerization method mentioned in the above-mentioned documents uses mostly alkali metal fluoride potassium fluoride and cesium fluoride as the main catalyst, and the used solvent is a polar aprotic solvent , the solubility of alkali metal fluoride salts in solvents is very poor, which results in the need to use a large amount of solvent to dissolve the catalyst, resulting in increased polymerization costs and difficulties in solvent recovery
In addition, the catalytic activity of potassium fluoride is low, and perfluoropolyether with a high degree of polymerization cannot be obtained. For cesium fluoride, although the catalytic activity is higher than potassium fluoride, it is expensive and hygroscopic. Difficulties in industrial scale-up

Method used

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  • Nickel metal complex as well as preparation method and application thereof
  • Nickel metal complex as well as preparation method and application thereof
  • Nickel metal complex as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Raw material A has a structure shown in formula (I);

[0035] Raw material B has a structure shown in formula (II-1);

[0036] Catalyst has the structure shown in formula (III-1);

[0037] Step 1: under nitrogen protection system, take by weighing raw material Ni (cod) 2 (21.3mmol), P( i Pr) 3 (37.9mmol) into the reaction system, add 65mL THF solvent, react at 40°C under nitrogen protection for 6h, then cool to room temperature, there is a precipitate, after the reaction is completed, the solid is obtained by suction filtration, washed with n-pentane, and finally placed in a vacuum After drying in a drying oven, raw material B (7.00 g, yield 47%) was obtained as a yellow powder.

[0038] Step 2: Weigh raw material A (13.3mmol), add raw material B (8.0mmol), then add THF 30mL to the system, under nitrogen protection, react at 25°C for 12h, drain the solvent, wash with n-pentane, and remove the remaining solid in Dry in a vacuum oven to obtain a yellow powdery solid ...

Embodiment 2

[0041] Raw material A has a structure shown in formula (I);

[0042] Raw material B has a structure shown in formula (II-1);

[0043] Catalyst has the structure shown in formula (III-1);

[0044] Step 1: under nitrogen protection system, take by weighing raw material Ni (cod) 2 (36.4mmol), P( i Pr) 3 (87.5mmol), then add THF 150mL to the system, react at 40°C for 6h under the protection of nitrogen, then cool to room temperature, there is a precipitate, after the reaction is completed, the solid is obtained by suction filtration, washed with n-pentane, and finally put into a vacuum oven Drying in medium temperature afforded raw material B (13.1 g, yield 63%) as a yellow powder.

[0045] Step 2: Weigh raw material A (22.3mmol), add raw material B (29.0mmol), then add THF 65mL to the system, under nitrogen protection, react at 25°C for 12h, drain the solvent, wash with n-pentane, and remove the remaining solid in Dry in a vacuum oven to obtain a yellow powdery solid (5.11 g...

Embodiment 3

[0048] Raw material A has a structure shown in formula (I);

[0049] Raw material B has a structure shown in formula (II-1);

[0050] Catalyst has the structure shown in formula (III-1);

[0051] Step 1: under nitrogen protection system, take by weighing raw material Ni (cod) 2 (29.5mmol), P( i Pr) 3 (104.5mmol), then added THF 150mL to the system, reacted at 60°C under nitrogen protection for 4h, then cooled to room temperature, and a precipitate was precipitated. After the reaction, the reaction solution was suction filtered, and the solid was washed with n-pentane, and then Put it into a vacuum drying oven and dry to obtain raw material B (10.79 g, yield 64%) as a yellow powder.

[0052] Step 2: Weigh raw material A (21.6mmol), add raw material B (75.6mmol), then add THF120mL to the system, under nitrogen protection, react at 35°C for 9h, drain the solvent, wash with n-pentane, and finally obtain The solid was dried in a vacuum drying oven to finally obtain a yellow po...

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Abstract

The invention discloses a nickel metal complex as well as a preparation method and an application thereof. The structural formula of the nickel metal complex is shown as a formula (III), wherein R isethyl, isopropyl or cyclohexyl in the formula (III). The nickel metal complex prepared by the preparation method disclosed by the invention is applied to the process of preparing the K-type perfluoropolyether oil as a catalyst and can effectively prepare the K-type perfluoropolyether oil with high polymerization degree, improves the product yield and reduces the amount of used solvents and the like, thereby effectively promoting the reduction of the production cost of the K-type perfluoropolyether.

Description

technical field [0001] The invention belongs to the technical field of perfluoropolyether oil polymerization, and in particular relates to a nickel metal complex and its preparation method and application. Background technique [0002] Perfluoropolyether is a high-molecular polymer containing only three elements of C, F, and O. It is a colorless, odorless, viscous oily liquid at room temperature. Compared with hydrocarbon compounds, F atoms in perfluoropolyether molecules replace all H atoms in hydrocarbon compounds, and all C-H bonds are replaced by C-F bonds with higher bond energy. The shielding effect of the C-F bond on the C-C and C-O bonds of the main chain makes perfluoropolyether have excellent chemical stability, oxidation resistance and corrosion resistance. Due to the strong electronegativity of the F atom, it has a small intermolecular attraction force, so the surface tension is small, showing good lubricity and permeability, and its stabilized product perfluoro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04C08G65/22
CPCC07F15/04C08G65/226
Inventor 刘兵陶杨
Owner 浙江诺亚氟化工有限公司
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