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A kind of regeneration and circulation method of ferric chloride etching solution

A ferric chloride etching and etching solution technology, applied in the field of regeneration and recycling of etching waste solution, can solve the problems of complex process, increased regeneration cost and solid waste discharge, unsuitable for large-scale industrial application, etc., and achieve simplified operation The effect of the process

Active Publication Date: 2022-02-08
SHENYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction method (patents CN1470674 and CN101497484) mainly obtains the separation of iron, nickel, etc. through organic solvent extraction, and then back-extracts to obtain FeCl 3 Reuse, there are problems such as complicated process, high cost, and the extraction agent needs to be further processed, so it is not suitable for large-scale industrial applications
In recent years, electrochemical methods (patents CN106958021A, CN107059011A, CN206872948U, CN206033893U, CN104131285A, CN104451688A, CN103710706A) have been applied to ferric chloride waste liquid regeneration technology. Fe in area waste 2+ Oxidized to Fe 3+ , to realize the regeneration and recycling of part of the waste liquid, while the waste liquid in the cathode area is due to the occurrence of Fe 3+ reduced to Fe 2+ In the reverse oxidation process, the waste liquid in the cathode chamber must be re-used after anodic secondary oxidation treatment, or discarded after subsequent treatment (such as precipitation iron powder replacement or extraction), which increases the regeneration cost and solid waste discharge. The overall recycling rate of liquid is low, and it is difficult to meet the requirements of production and application

Method used

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  • A kind of regeneration and circulation method of ferric chloride etching solution

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Experimental program
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Effect test

Embodiment 1

[0024]Batch operation: Take a certain volume of ferric chloride etching waste solution, and use ICP-MS to detect that it contains 205g / L of total iron, 104mg / L of Cr, 1069mg / L of Mn, and 741mg / L of Cu. Adjust the pH of the waste liquid to 2-3, add a chemical precipitant to the reaction tank, and after filtering through the sedimentation tank, take the supernatant and introduce it into the anode chamber, using titanium plates as cathode and anode respectively, with a current density of 18A / dm 2 Add the pre-prepared electrolyte to the cathode chamber, monitor the concentration of the electrolyte in the cathode chamber according to the concentration detector, replenish the electrolyte consumed in the electrolysis process in time, and keep the temperature between 50-60°C; the Fe in the waste liquid of the anode chamber 2+ Oxidized to Fe 3+ , the etching ability gradually recovers, the waste etching solution is regenerated, and the Fe 2+ The concentration is 0.3g / L, and the conver...

Embodiment 2

[0026] On-line operation: random monitoring of ferric chloride etching waste liquid, with ICP-MS detection of total iron 178g / L, Cr 243mg / L, Mn 1927mg / L, Ni 5964mg / L in the waste liquid; regular precipitation removal Miscellaneous treatment, adjust the pH2-3 during treatment, add chemical precipitant to the reaction tank, filter through the sedimentation tank for use, and do not need precipitation treatment during online operation; the etching waste liquid is directly and continuously introduced into the lower inlet of the anode chamber, and flows out from the upper outlet anode chamber. The titanium plate is used as cathode and anode respectively, and the current density is 16A / dm 2 . The cathode chamber is filled with pre-prepared electrolyte, and the electrolyte consumed in the electrolysis process is replenished in time, and the temperature is kept between 50-60°C. Fe in anode chamber waste 2+ Oxidized to Fe 3+ , the etching ability gradually recovers, the waste etchin...

Embodiment 3

[0028] Take a certain volume of ferric chloride etching waste solution, and use ICP-MS to detect that the waste solution contains 193g / L of total iron, 89mg / L of Cr, 44mg / L of Ni, 1033mg / L of Mn, and 569mg / L of Cu. Adjust the pH of the waste liquid to 2-3, add a chemical precipitant to the reaction tank, and after filtering through the sedimentation tank, take the supernatant and introduce it into the anode chamber, and use the graphite plate as the cathode and anode respectively. Current density 20A / dm 2 . The cathode chamber is filled with pre-prepared electrolyte, and the electrolyte consumed in the electrolysis process is replenished in time, and the temperature is kept between 50-60°C. Fe in anode chamber waste 2+ Oxidized to Fe 3+ , the etching ability gradually recovers, the waste etching solution is regenerated, and the Fe 2+ The concentration is 0.5g / L, and the conversion rate reaches 95%. The regenerated anolyte enters the adjustment pool, and according to the m...

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Abstract

A method for regenerating and recycling ferric chloride etching solution. The invention proposes a "diaphragm-one-pass process" technology. The diaphragm of the electrolyzer is divided into a cathode chamber and an anode chamber, and all the waste liquid is separated from Fe in the anode chamber. 2+ Oxidized to Fe 3+ , all the waste liquid is regenerated and recycled. The cathodic chamber solution uses a conductive electrolyte and uses a diaphragm. The anions in the electrolyte can be exchanged with the anode solution to achieve charge balance and material balance, and no Fe 3+ reduced to Fe 2+ The oxidation reverse process, so the catholyte does not need secondary electrolysis and subsequent treatment, clean and low consumption, greatly improving the regeneration efficiency, combined with chemical impurity removal methods, further reducing production costs, can be regenerated on-line or off-line, the process adopts Automatic control meets the practical application requirements for the recycling of ferric chloride etching solution.

Description

technical field [0001] The invention relates to a regeneration method and recycling use of a recyclable ferric chloride etching solution, and is especially suitable for regeneration and recycling of iron, steel, copper and other etching waste solutions. Background technique [0002] Metal etching such as iron and steel is widely used in various fields of national life, and FeCl 3 The etchant has a mature etching technology for various grades of steel, iron, copper, etc., and can be used to manufacture printing metal plates, flower rolls, etc., and etch thin parts that are difficult to machine, such as metal screens, small holes, Gratings, etc., used for plaques, graphic engraving on metal surfaces of instruments and equipment, etc. FeCl during etching 3 Fe in etchant 3+ Gradually become Fe 2+ However, the etching ability is lost, and the total iron content increases at the same time, and the output of ferric chloride etching waste liquid is large. In addition to being ri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23F1/46C23F1/28
CPCC23F1/46C23F1/28
Inventor 康艳红
Owner SHENYANG NORMAL UNIV
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