Process for preparing cobalt boracylate by hybrid reaction of cobaltous carbonate and organic carboxyl acid

A preparation process, organic carboxylic acid technology, applied in cobalt organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problem of reducing the adhesion stability of rubber and steel wire, unfavorable rubber and steel wire adhesion, and high total acidity of free fatty acids. problems, to achieve the effect of maintaining stability, preventing metal rust, and improving heat-resistant oxygen

Inactive Publication Date: 2009-01-21
逯大成
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

They have high reactivity during rubber vulcanization and play a major role in strengthening the adhesion between rubber and steel wire. However, the total acidity of free fatty acids generated by

Method used

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  • Process for preparing cobalt boracylate by hybrid reaction of cobaltous carbonate and organic carboxyl acid
  • Process for preparing cobalt boracylate by hybrid reaction of cobaltous carbonate and organic carboxyl acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 60g of glacial acetic acid, 70g of neodecanoic acid, 34g of isooctanoic acid, and 100g of cobalt carbonate to a 1000ml four-necked flask equipped with a reflux condenser, a temperature-regulating electric heating mantle, and a vacuum pump, and control the reaction temperature at 105°C. Drain to remove the water formed by the reaction. Add 60g of dibutyl borate at a temperature of 170°C, the reaction time is 2 hours, heat up and drain, vacuum depressurize and drain, discharge butyl acetate, add 16g of active calcium carbonate and 20g of resin acid at a temperature of 180°C, and evenly After stirring for 1 hour, the materials were discharged to obtain the cobalt boroacylate product. The prepared cobalt boroacylate has a cobalt content of 22.7% and a blue-purple appearance.

Embodiment 2

[0044] Add 64g of glacial acetic acid, 74g of neodecanoic acid, 36g of isooctanoic acid, and 98g of cobalt carbonate to a 1000ml four-neck flask equipped with a reflux condenser, a temperature-regulating electric heating mantle, and a vacuum pump in sequence, and control the reaction temperature at 100°C. The reaction time is 4 hours, and the temperature is raised. Drain, remove the water generated by the reaction, add 64g of tributyl borate at a temperature of 160°C, react for 2.5 hours, heat up and drain, vacuum and reduce pressure, drain butyl acetate, add active calcium carbonate at 175°C 18g, 24g of resin acid, stirred evenly for 1 hour, and discharged to obtain a cobalt boroacylate product with a cobalt content of 22.5% and a blue-purple appearance.

Embodiment 3

[0046] Add 62g of glacial acetic acid, 73g of neodecanoic acid, 38g of isooctanoic acid, and 96g of cobalt carbonate into a 1000ml four-neck flask with a reflux condenser, a temperature-regulating electric heating mantle, and a vacuum pump in sequence, and control the reaction temperature at 110°C. Drain, remove the water generated by the reaction, add 62g of tributyl borate at a temperature of 180°C, react for 3 hours, heat up and drain, vacuum and reduce pressure, drain butyl acetate, add active calcium carbonate at 185°C 20g and 22g of resin acid were stirred evenly for 1 hour and discharged to obtain a cobalt boroacylate product with a cobalt content of 22.1% and a blue-purple appearance.

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Abstract

The invention provides a process for preparing a carboxyl cobalt-boron complex by the mixing reaction of cobalt carbonate and an organic carboxylic acid, belonging to the organic synthesis technical field. Cobalt carbonate is taken as a material, and the invention is characterized in that the preparation process comprises the following steps that: (1) cobalt carbonate, glacial acetic acid, neodecanoic acid and isooctanoic acid are taken as materials and put in a normal pressure sealing reactor, the reaction temperature is controlled to be between 100 and 110 DEG C, and the reaction time is no less than 3h; (2) tributyl borate is added in the reaction system, the reaction temperature is controlled to be between 160 and 180 DEG C, the reaction time is no less than 2h, and the carboxyl cobalt-boron complex and the side product of butyl acetate are generated; (3) the temperature is controlled to be between 175 and 185 DEG C, and active carbon and resin acid are added to obtain the refined product. In the invention, cobalt carbonate is used to replace cobaltous hydroxide, the carboxyl cobalt-boron complex is added with adhesion agent and activated calcium carbonate with amphoteric compound, thereby effective balancing ph in the system, making the product effectively prevent corrosion of metal, enhancing adhesion level and improving thermal oxygen resistant, heat resistant and steam ageing resistant performances.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a process technology for preparing cobalt carboxyl boroacylate. Background technique [0002] Cobalt boroacylate, whose theoretical molecular formula is B(O-C 0 -O-R n ) 3 . Cobalt boroacylate is a highly active adhesion promoter, mainly used for bonding of natural rubber, synthetic rubber or brass, zinc bare copper and brass, zinc plated steel cord, cable, metal plate Promote. It is made of cobalt hydroxide, propionic acid and related organic acids as raw materials, first undergoes acid-base salt formation reaction, and then undergoes acid displacement reaction. The cobalt boroacylate prepared by the method contains relatively high cobalt content. They have high reactivity when rubber is vulcanized, and play a major role in strengthening the adhesion between rubber and steel wire. However, the total acidity of free fatty acids produced by the reaction...

Claims

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Application Information

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IPC IPC(8): C07F15/06C07F5/02
Inventor 逯大成梅明
Owner 逯大成
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