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Method and device for directly recovering oxalate precipitate of waste acid

A technology of oxalate and waste acid, which is applied in the direction of carboxylate preparation, carboxylate preparation, nitric acid, etc., can solve the problems of many equipments and long treatment process, and achieve short process, low operating cost and low consumption Effect

Inactive Publication Date: 2011-07-06
GANZHOU RECYCLE NEW TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention has a long treatment process and a lot of equipment, requires the use of flammable, explosive and toxic substances such as organic amines, and produces a large amount of sediment by-products formed by organic amines, acids and precipitants that need to be treated.

Method used

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  • Method and device for directly recovering oxalate precipitate of waste acid
  • Method and device for directly recovering oxalate precipitate of waste acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment one: carry out oxalic acid precipitation by dysprosium chloride solution to obtain dysprosium oxalate and reclaim hydrochloric acid

[0031] see figure 1 , the precipitation distillation pot, which is composed of a polytetrafluoroethylene-lined kettle body, a stirrer loaded from the top of the kettle body, and a far-infrared heater installed at the bottom of the kettle body, and the condenser, collector, and vacuum pump are sequentially used to compact pipe fittings Connect to form precipitation distillation equipment.

[0032] Among them, the internal parts of the precipitation distillation pot, the surface of the pipe fittings between the precipitation distillation pot and the condenser and the material contact surface are all lined with polytetrafluoroethylene; the condenser adopts graphite modified PP cold heat exchanger; the collector and the pipe fittings between the collector and the vacuum pump adopt Lined with polytetrafluoroethylene material.

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Embodiment 2

[0035] Embodiment two: cobalt acetate solution carries out oxalic acid precipitation to obtain cobalt oxalate and reclaim acetic acid

[0036] see figure 1 , Precipitation distillation equipment is the same as embodiment one.

[0037] Will C Co 2+ =70g / L, C H + = 1500L cobalt acetate solution of 1mol / L, added to 2m 3In the settling distillation pot, open the far-infrared heater to make the temperature of the material in the pot rise to 60°C, and add 228KG oxalic acid solids several times while stirring. Close the feeding port of the precipitation distillation pot. Continue stirring and heating, carry out normal pressure distillation, keep the material in the pot at 107°C, stop the distillation when the content in the pot is distilled to a residual liquid≤10%, and end the distillation operation. Obtain 1475 liters of pure acetic acid of 3.20mol / L, and the recovery rate of acetic acid is 93.30%. Add 1500L of hot water obtained by heat exchange in the condenser into the p...

Embodiment 3

[0039] Embodiment three: neodymium nitrate solution carries out oxalic acid precipitation to obtain neodymium oxalate and reclaim nitric acid

[0040] see figure 1 , Precipitation distillation equipment is the same as embodiment one.

[0041] Will C H + =0.360mol / L, C REO =1.462mol / L (REO=245.91g / L), 1500L of neodymium nitrate solution was added to 2m 3 In the precipitation distillation pot, add 419KG solid oxalic acid several times under normal temperature and stirring conditions. Close the feeding port of the precipitation distillation pot. Continue to stir and turn on the far-infrared heater to raise the temperature of the material in the pot to 80°C, turn on and adjust the water ring vacuum system, carry out vacuum distillation, keep the material in the pot between 90 and 100°C, and distill until the remaining in the precipitation distillation pot Stop distillation when liquid≤10%, obtain the nitric acid of 1465 liters 4.46mol / L. The recovery rate of nitric acid is ...

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Abstract

The invention relates to a method and a device for directly recovering the oxalate precipitate of waste acid. The method is characterized in that a soluble metal salt solution and oxalic acid are added in a precipitation-distillation kettle and sufficiently mixed to generate an oxalate precipitate and waste acid, and then the waste acid in the precipitation-distillation kettle is distilled and recovered; and water is added in the precipitation-distillation kettle, the oxalate precipitate is stirred into slurry, and then the slurry is discharged, filtered, washed and dried to obtain an oxalate product. The method can not only greatly reduce the evaporation capacity of waste acid as well as the energy loss and material damage in the prior precipitation process, but also greatly save the consumption of oxalic acid. In addition, the adopted device has the advantages of long service life, low maintenance cost, energy conservation and the like. The method and the device have the characteristics of simple process, less consumption of chemical raw materials, high efficiency, energy conservation, environmental protection and low running cost, and not only solve the problems of waste acid recovery and environmental pollution in the oxalate precipitation process, but also realize better economic benefit.

Description

technical field [0001] The invention belongs to the technical field of industrial wastewater treatment and hydrometallurgy, and in particular relates to a hydrometallurgical plant precipitation method and recycling of waste acid. Background technique [0002] Oxalate and many metal ions easily form crystalline oxalate precipitates. Oxalate precipitates not only have good crystal shape and particle size distribution, but also have fast precipitation speed, easy filtration, easy washing and easy drying in the process, and the obtained products have low impurity content and good quality; in addition, they can be decomposed and transformed into metal Oxide, so in the field of hydrometallurgy and powder metallurgy, oxalic acid precipitation process has a wide range of applications. [0003] Generally speaking, the existing oxalate precipitation and its wastewater treatment are carried out in different equipment in different processes. The existing oxalate precipitation process ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/08C07C51/02C01B7/03C01B21/42C07C55/07C07C51/41
Inventor 刘明彪龚斌袁军
Owner GANZHOU RECYCLE NEW TECH
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