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Preparing method of bis (cyclopentadienyl) cobalt

A technology of dicyclopentadiene and sodium cyclopentadienide, which is applied in chemical instruments and methods, organic chemistry, metallocene, etc., can solve the problems of high market price of dicyclopentadiene cobalt, production, packaging, storage, etc. Problems such as transportation and other difficulties, difficulty in industrialized production, etc., achieve the effects of easy separation and purification, easy operation, and strong solubility

Inactive Publication Date: 2012-09-19
DONGYING SHIDA HONGYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing patent documents US4320066, US4556714, DE1223839, and CN101108366A, the process method adopted is all relatively primitive, mostly adopts more than two solvents to repeatedly dissolve, filter, concentrate, low vacuum recovery solvent, low vacuum drying, complicated process, high cost, resulting in The market price of dicyclopentadiene cobalt remains high, which restricts the development of related fields of my country's chemical industry
In addition, dicyclopentadiene cobalt has high activity, and cobalt is easy to oxidize and change in value. Its production, packaging, storage and transportation are difficult, and it is not easy for industrial production. It can only be produced on a laboratory scale
So far, only the School of Chemistry and Chemical Engineering of Nanjing University has this product in China, and the price is expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Heat 18 kg of 95 wt% dicyclopentadiene to 170° C. in a heating kettle to decompose 15 kg of cyclopentadiene, condense it at 0° C. for later use. 3 kg of heavy components as by-product heavy oil fuel.

[0022] Add 100 kg of benzene and 5 kg of granular metallic sodium into a sodium-cene kettle, stir at a constant temperature of 0°C, and gradually add 15 kg of cyclopentadiene to generate sodium cyclopentadienide and hydrogen. After 60 minutes no hydrogen gas was evolved and the sodium metal was completely reacted.

[0023] Add 100 kilograms of benzene, 15 kilograms of liquid ammonia and 15 kilograms of cobalt dichloride into the cobalt-forming kettle, and stir and react at 10° C. for 60 minutes to form a complex of cobalt dichloride and ammonia.

[0024] Keep the temperature of the cobalt-forming kettle at 20° C., gradually add 19 kg of the prepared sodium cyclopentadienide solution, and stir for 2 hours to obtain a dicyclopentadienyl-cobalt mixed solution.

[0025] Rem...

Embodiment 2

[0028] The preparation of cyclopentadiene and sodium cyclopentadienide is the same as example 1.

[0029] Add 100 kilograms of acetonitrile, 30 kilograms of 30 wt % ammonia water and 30 kilograms of cobalt dichloride into the cobalt-forming kettle, and stir and react at 20° C. for 20 minutes to form a complex of cobalt dichloride and ammonia water.

[0030] Keep the temperature of the cobalt-forming kettle at a constant temperature of 30° C., gradually add 40 kg of sodium cyclopentadienylate solution, stir and react for 1 hour, and obtain a dicyclopentadienyl-cobalt mixed solution.

[0031] Heat the cobaltocene kettle to 120°C, distill ammonia water and acetonitrile for recycling. Inside the kettle is a solid mixture of sodium chloride and dicyclopentadienyl cobalt.

[0032] Add 50 kg of acetonitrile and stir at room temperature. After dicyclopentadienyl cobalt is completely dissolved, remove sodium chloride by filtration. The obtained filtrate is the target product dicyclop...

Embodiment 3

[0034] The preparation of cyclopentadiene and sodium cyclopentadienide is the same as example 1.

[0035] Add 100 kg of acetonitrile, 40 kg of 25wt% ammonia water and 40 kg of cobalt dichloride into the cobalt-based still, and stir and react at 20° C. for 20 minutes to form a complex of cobalt dichloride and ammonia water.

[0036] Keep the temperature of the cobaltocene kettle at a constant temperature of 30° C., gradually add 50 kg of sodium cyclopentadienide solution, stir and react for 1 hour, and obtain a dicyclopentadienyl cobalt mixed solution.

[0037] Remove the sodium chloride generated by the reaction by filtration, heat the filtrate to 110°C, distill off the ammonia water and benzene, and recycle them separately. Obtain target product dicyclopentadienyl cobalt in still.

[0038] Dissolve dicyclopentadienyl cobalt in 40 kg of acetonitrile, avoiding exposure to air.

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Abstract

The invention discloses a preparing method of bis (cyclopentadienyl) cobalt. The preparing method includes the following steps that Lewis base and cobalt dichloride are reacted to produce coordination compounds, and the coordination compounds and sodium cyclopentadienide are reacted to produce bis (cyclopentadienyl) cobalt. The preparing method has the advantages that the bis (cyclopentadienyl) cobalt is prepared through a method which is simple in process and safe and feasible, and production cost can be greatly reduced.

Description

technical field [0001] The invention relates to a preparation method of dicyclopentadienyl cobalt. Background technique [0002] Dicyclopentadiene cobalt is referred to as dicyclopentadienyl cobalt, mainly used as catalyst, vulcanization accelerator, olefin polymerization inhibitor, paint drier, oxygen desorbent, etc. The traditional preparation method is prepared by reacting cobalt dichloride and sodium cyclopentadienate in tetrahydrofuran or ethylene glycol dimethyl ether. Existing patent documents US4320066, US4556714, DE1223839, and CN101108366A, the process method adopted is all relatively primitive, mostly adopts more than twice solvent to dissolve repeatedly, filter, concentrate, low vacuum reclaims solvent, low vacuum is dried, and process is complicated, and cost is high, causes The market price of dicyclopentadiene cobalt remains high, which restricts the development of related fields of my country's chemical industry. In addition, dicyclopentadiene cobalt has hig...

Claims

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Application Information

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IPC IPC(8): C07F17/02
Inventor 于景东刘强孙景辉杜寿考鲍林
Owner DONGYING SHIDA HONGYI CHEM
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