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Synthesis process of cobalt acetate

A synthesis process and technology of cobalt acetate, applied in the directions of cobalt carbonate, carboxylate preparation, carboxylate preparation, etc., can solve the problems of large consumption of raw materials and energy, high production cost, low reaction efficiency, etc., and improve the reaction contact efficiency. , The effect of reducing the consumption of raw materials and reducing the reaction concentration

Pending Publication Date: 2022-03-25
MAANSHAN DEHONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Cobalt acetate is the most important catalyst for the preparation of terephthalic acid by liquid-phase oxidation of p-xylene. The process used in the early stage of the synthesis of cobalt acetate is generally produced by the nitric acid method to obtain cobalt acetate crystals. When used, it is dissolved. A lot of equipment is required, the process is long, the equipment is severely corroded, there is environmental pollution, the consumption of cobalt in the production is large, and the production cost is high
Then the nitric acid method was improved, that is, nitric acid acetic acid mixed acid was used to react with metal cobalt, and crystal cobalt acetate was produced through concentrated crystallization and impurity removal, but there were still many defects in this process, such as environmental pollution, low reaction efficiency, large consumption of raw materials and energy, In the later stage of the reaction, the cobalt activity decreases, and the impurity content in the product is high, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of cobalt powder:

[0021] Mix azobisisobutyronitrile, toluene, N-vinylpyrrolidone and lauryl methacrylate, stir and react for 24 hours at a temperature of 70°C under nitrogen protection, after the reaction is completed, add hydrochloric acid acidified methanol to stop the reaction , mixed the obtained reaction solution with n-hexane, filtered, vacuum-dried at 40°C to constant weight, and then mixed with ethylene glycol according to the dosage ratio of 1g:100mL to obtain a surfactant; among them, azobisisobutyronitrile, toluene, The dosage ratio of N-vinylpyrrolidone and lauryl methacrylate is 50mg: 20mL: 1g: 0.5g;

[0022] Add cobalt chloride aqueous solution and ammonium bicarbonate aqueous solution into the autoclave, then add the surfactant, stir for 30 minutes after the addition, then raise the temperature to 200°C, and the pressure is 3MPa; keep warm for 12 hours, reduce the pressure to normal pressure, and cool to room temperature , filtered, and the...

Embodiment 2

[0025] Preparation of cobalt powder:

[0026] Mix azobisisobutyronitrile, toluene, N-vinylpyrrolidone and lauryl methacrylate, stir and react for 24 hours at a temperature of 70°C under nitrogen protection, after the reaction is completed, add hydrochloric acid acidified methanol to stop the reaction , mixed the obtained reaction solution with n-hexane, filtered, vacuum-dried at 40°C to constant weight, and then mixed with ethylene glycol according to the dosage ratio of 1g:100mL to obtain a surfactant; among them, azobisisobutyronitrile, toluene, The dosage ratio of N-vinylpyrrolidone and lauryl methacrylate is 50mg: 20mL: 1g: 0.5g;

[0027] Add cobalt chloride aqueous solution and ammonium bicarbonate aqueous solution into the autoclave, then add the surfactant, stir for 30 minutes after the addition, then raise the temperature to 200°C, and the pressure is 3MPa; keep warm for 12 hours, reduce the pressure to normal pressure, and cool to room temperature , filtered, and the...

Embodiment 3

[0030] A kind of synthetic technique of cobalt acetate, comprises the steps:

[0031] Add acetic acid and 50% water in the reaction kettle, then add the cobalt powder obtained in Example 1 in three batches, after the addition, add hydrogen peroxide and the remaining water, control the reaction temperature to 60°C, and the pressure to 0.3MPa, Stay for 3 minutes, then filter, and add a small amount of hydrogen peroxide for impurity removal and activation to obtain an aqueous solution of cobalt acetate, which is then concentrated by evaporation, crystallized by cooling, and sieved to obtain cobalt acetate. Among them, the molar ratio of acetic acid, hydrogen peroxide and water is 1:1:20. The amount ratio of cobalt powder added in three batches is 1:2:3; the interval time is 1min; the molar ratio of the total amount of cobalt powder to acetic acid is 1:2. The cobalt acetate aqueous solution does not contain nickel, and the utilization rate of hydrogen peroxide is 100%.

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Abstract

The invention relates to a synthesis process of cobalt acetate, which belongs to the technical field of catalyst synthesis, and comprises the following steps: reducing cobalt carbonate powder in a hydrogen atmosphere at the reduction temperature of 480-500 DEG C for 2 hours to obtain cobalt powder; the method comprises the following steps: adding acetic acid and 50% water into a reaction kettle, then adding cobalt powder in three batches, then adding hydrogen peroxide and residual water, controlling the reaction temperature to be 60-90 DEG C and the pressure to be 0.3-0.4 MPa, staying for 3-6 minutes, filtering to obtain a cobalt acetate aqueous solution, and carrying out evaporation concentration, cooling crystallization and sieving to obtain cobalt acetate. Cobalt acetate is prepared by directly reacting metal cobalt with acetic acid and hydrogen peroxide; the metal cobalt contact reaction is slow, the mass transfer speed is slow, and the side reaction is aggravated, through the prepared cobalt powder, the reaction contact efficiency is improved, acetic acid is added firstly and then an oxidizing agent is added, the utilization rate of hydrogen peroxide is improved, and raw material consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of catalyst synthesis, and in particular relates to a synthesis process of cobalt acetate. Background technique [0002] Cobalt acetate is the most important catalyst for the preparation of terephthalic acid by liquid-phase oxidation of p-xylene. The process used in the early stage of the synthesis of cobalt acetate is generally produced by the nitric acid method to obtain cobalt acetate crystals. When used, it is dissolved. A lot of equipment is required, the process is long, the equipment is severely corroded, there is environmental pollution, the consumption of cobalt in the production is large, and the production cost is high. Then the nitric acid method was improved, that is, nitric acid acetic acid mixed acid was used to react with metal cobalt, and crystal cobalt acetate was produced through concentrated crystallization and impurity removal, but there were still many defects in this process, such as e...

Claims

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Application Information

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IPC IPC(8): C07C53/10C07C51/41C01G51/06
CPCC07C51/412C01G51/06C01P2006/80C07C53/10
Inventor 陈敏裴锡贵李志勇
Owner MAANSHAN DEHONG BIOTECH
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