Method of synthesizing solid cobaltic naphthenate

A technology of cobalt naphthenate and synthesis method, which is applied in the separation/purification of carboxylic acid compounds, preparation of carboxylate, etc., can solve the problems of low cobalt and cobalt naphthenate content, affecting the bonding strength of rubber and steel wire, etc., and achieve cobalt The effects of increased content, reduced impurity components, and improved equipment efficiency and production capacity

Inactive Publication Date: 2007-08-15
谭昌诚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent No.: 200310105264.5 Due to the use of domestic naphthenic acid in the disclosed technology, the content of cobalt and cobalt in the prepared naphthenic acid is low, which affects the bonding strength of rubber and steel wire

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: Purification and preparation of naphthenic acid

[0019] 1) Extraction - the raw material naphthenic acid is extracted with chloroform or isoamyl butyrate in an extraction kettle, the extraction solvent and naphthenic acid are mixed at a weight ratio of 60:35, and then the mixer is started, stirred for 10-15 minutes, and then allowed to stand for stratification , release the insoluble matter in the lower layer, and recover the solvent by distillation at a temperature of 130-150 °C.

[0020] 2) Distillation - transfer the extraction phase to a distillation pot for distillation, the reflux ratio is less than 3, the number of trays is 8-10 layers, and the solvent is recovered at 130-150 °C, and the distillation head accounts for about 5% of the total weight of the feed. Not used as raw material.

[0021] 3) Distillation and purification - start the vacuum pump to carry out vacuum distillation, keep the system at -0.09Mpa for 20-30min, then collect the middle...

Embodiment 2

[0022] Embodiment 2: cobalt naphthenate synthesis

[0023] Get cobalt sulfate and sodium carbonate (industrial base) to react in aqueous solution with 1: 1 molar ratio and generate basic cobalt carbonate precipitation, reaction pH value 10~11, reactant concentration 17~54% (weight), reaction temperature 40~95 ℃, the resulting basic cobalt carbonate was washed to neutral, and when the pH value was less than or equal to 8, it was press-filtered for later use; 4 moles of purified naphthenic acid and 1 mole of basic cobalt carbonate wet filter cake were used for synthesis reaction, and the solvent oil was selected from two toluene. The addition amount of xylene: the theoretical formation amount of cobalt naphthenate=1:1 (weight ratio).

[0024] When the temperature rises to 40°C, add 40% of the total weight of naphthenic acid; the reaction temperature is 60-80°C, and the reaction time is 2 hours, and the remaining amount of naphthenic acid is added; when the reaction temperature ...

Embodiment 3

[0026] Preparation of basic cobalt carbonate intermediate and purification of naphthenic acid are the same as in Examples 1 and 2. Get naphthenic acid: basic cobalt carbonate=4: 1 (molar ratio) and 170# solvent gasoline, gasoline addition: theoretical generation amount of naphthenic acid cobalt=1: 1 (weight ratio). When the temperature rises to 40°C, add 20% of the total weight of naphthenic acid; react for 2 hours, and when the temperature reaches 70±2°C, add 20% of the total weight of naphthenic acid; Hours later, add the remaining amount of naphthenic acid, the reaction temperature is 90±2°C, and the time is 3-4 hours; react at the bubble point of the system while dehydrating and reflux, and the reflux time is kept for 7-8 hours; when the temperature rises to 160°C Start to remove the solvent while reacting above, and the reflux time for the solvent removal is 4 to 6 hours. When the system temperature reaches 210±5°C, the solvent is removed completely.

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PUM

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Abstract

The invention discloses a synthesizing method of solid cobaltic naphthenate, which comprises the following steps: dissolving naphthenic acid into polar organic solvent; separating insolubles under lower layer; setting the weight rate of extractant and naphthenic acid at 60: 30-35; transmitting extracting phase into distilling autoclave to distill with reflux rate less than 3; setting the tower floor layer number at 8-10; recycling solvent at 130-150 deg.c; decompressing and rectifying under -0.07-0.09Mpa for 20min; purifying; collecting middle fraction and naphthenic acid at 140-150 deg.c for 16-22h; adding naphthenic acid within 2-4 times.

Description

technical field [0001] The invention relates to a method for preparing cobalt naphthenate, in particular to a method for synthesizing cobalt naphthenate by refining and purifying naphthenic acid raw materials. Background technique [0002] Solid cobalt naphthenate can be used as an adhesion promoter for steel radial tires to improve the bonding strength between steel wire and rubber. At present, the cobalt content in the domestic cobalt naphthenate in the domestic market is low, and this is because the acid value in the synthetic raw material naphthenic acid is low, contains unsaponifiable substances such as high-boiling hydrocarbons and colloids, (the acid value is about 180KOH / mg Neutralization value, the content of non-saponifiable matter is more than 5%.) These non-saponifiable matters not only reduce the cobalt content of cobalt naphthenate, but also increase the impurity components, and also reduce the bonding strength between steel wire and rubber. Therefore, wholly-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C51/42
Inventor 谭昌诚于立珍王心满颜秉舟
Owner 谭昌诚
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