CN213802942U - Recycling treatment device for ferric trichloride etching solution - Google Patents
Recycling treatment device for ferric trichloride etching solution Download PDFInfo
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Abstract
The utility model provides a recycling treatment device of ferric trichloride etching solution, which comprises an oxidation reaction tank, an evaporation cooling crystallization device, a dissolving tank, a first pH adjusting device, a second filter, a second pH adjusting device, a third filter, a neutralization reaction device, a third pH adjusting device, a stripping deamination device, a fourth filter, a raw material storage tank, a water storage tank, a concentrated hydrochloric acid storage tank, an oxidant storage tank, a regeneration etching solution storage tank, an ammonia water storage tank and a liquid caustic soda storage tank; the utility model adopts the method of evaporative cooling crystallization and pH regulation precipitation to control the quality of the recovered ferric salt, and controls the evaporation capacity so as to control the contents of chromium chloride and nickel chloride in the 6-water ferric chloride, thereby ensuring the quality of the 6-water ferric chloride, and the ferric chloride after the solution can be used as etching solution or water purifying agent; the utility model discloses effectual molysite, the nickel salt of having retrieved promptly utilizes evaporative cooling crystallization and ammoniation precipitation to combine again, has reduced the liquid caustic soda use amount, has reduced the manufacturing cost of technology.
Description
Technical Field
The utility model relates to an environmental protection field technique, concretely relates to processing apparatus is resourceful again of ferric trichloride etching solution.
Background
The etching of metals such as steel and iron is widely applied in various fields of national life, and the FeCl3 etching solution is adopted to carry out mature etching technology of various grades of steel, iron, copper and the like, can be used for manufacturing metal word plates, embossing rollers and the like for printing, and can be used for etching sheet parts which are difficult to machine, such as metal screen plates, small holes, gratings and the like, and can be used for engraving and printing patterns on metal surfaces of plaque boards, instruments and equipment. In the etching process, Fe3+ in FeCl3 etching solution is gradually changed into Fe2+ to lose etching capacity, meanwhile, the total iron content is increased, the yield of ferric trichloride etching waste solution is high, heavy metals such as Cr, Ni and Cu carried in metal materials enter the waste solution besides a large amount of Fe, the discharge is not up to standard, and a large amount of iron and the like are used as waste to cause waste of resources.
At present, the domestic method for recycling FeCl3 etching waste liquid is more, and the method can be classified into a precipitation method, a chemical oxidation regeneration method, an extraction method, an electrolysis method and the like.
The precipitation method regeneration (patent CN1540036 and patent CN1566401) mainly uses concentrated or roasted waste liquid to obtain FeCl3 crystal for recovery, and redissolves to realize the recovery and regeneration of ferric trichloride, and the energy consumption in the concentration or roasting process is high, and the recovery rate is limited.
The chemical oxidation regeneration method (China patent applications CN1309194, CN107162276A, CN101462803, CN106348509A, CN206872949U and the like) mainly adopts chlorine, oxidants such as H2O2, NaClO3 and auxiliary reagents such as HCl to regenerate the ferric trichloride, has the problems that the oxidants are toxic, the oxidation effect is limited or extra impurity ions are added to the oxidants, and the like, increases the waste liquid increment in the regeneration process, has limited regeneration cycle times, increases the discharge amount of the waste liquid, and has limited practical production application.
The extraction method (patent CN1470674 and patent CN101497484) mainly uses organic solvent extraction to separate iron and nickel, and then performs back extraction to obtain FeCl3 for recycling, which has the problems of complex process, high cost, further treatment of extractant, and the like, and is not suitable for large-scale industrial application.
In recent years, electrochemical methods (patents CN106958021A, CN107059011A, CN206872948U, CN206033893U, CN104131285A, CN104451688A, and CN103710706A) are frequently applied to the regeneration technology of ferric trichloride waste liquid, at present, diaphragms are mostly used to separate the cathode and the anode of an electrolytic cell, Fe2+ in the waste liquid in the anode region is oxidized into Fe3+ during electrolysis, so that part of the waste liquid is regenerated and recycled, and the waste liquid in the cathode region is subjected to oxidation reverse process of reducing Fe3+ into Fe2+, so that the waste liquid in the cathode chamber must be subjected to secondary oxidation treatment of the anode for reuse, or is discarded after subsequent treatment (such as replacement or extraction of precipitated iron powder), thereby increasing the regeneration cost and the discharge of solid waste, and the overall recycling rate of the waste liquid is low, and the requirements of production and application are difficult to achieve.
Accordingly, there is a need for improvements in the art.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to provide a resourceful treatment device again of efficient ferric trichloride etching solution.
In order to solve the technical problem, the utility model provides a recycling treatment device of ferric trichloride etching solution, including oxidation reaction tank, evaporation cooling crystallization device, dissolving tank, first pH adjusting device, second filter, second pH adjusting device, third filter, neutralization reaction device, third pH adjusting device, strip deamination device, fourth filter, raw materials storage tank, water storage tank, concentrated hydrochloric acid storage tank, oxidant storage tank, regeneration etching solution storage tank, aqueous ammonia storage tank and liquid caustic soda storage tank;
outlets of the raw material storage tank, the oxidant storage tank and the concentrated hydrochloric acid storage tank are all connected with an inlet of the oxidation reaction tank;
the outlet of the oxidation reaction tank is connected with the inlet of the evaporative cooling crystallization device;
the solid outlet of the evaporative cooling crystallization device is connected with the inlet of the dissolving tank; the outlet of the water storage tank is connected with the inlet of the dissolving tank;
the outlet of the dissolving tank is connected with the inlet of the regenerated etching solution storage tank;
the liquid outlet of the evaporative cooling crystallization device is connected with the inlet of the first pH adjusting device;
the outlet of the first pH adjusting device is connected with the inlet of the second filter;
the solid outlet of the second filter is connected with the inlet of the neutralization reaction device;
outlets of the water storage tank and the concentrated hydrochloric acid storage tank are both connected with an inlet of the neutralization reaction device;
the outlet of the neutralization reaction device is connected with the inlet of the regenerated etching solution storage tank;
the liquid outlet of the second filter is connected with the inlet of the second pH adjusting device;
the outlet of the second pH adjusting device is connected with the inlet of a third filter;
the liquid outlet of the third filter is connected with the inlet of a third pH adjusting device; the outlet of the liquid caustic soda storage tank is connected with the inlet of the third pH adjusting device;
the outlet of the third pH adjusting device is connected with the inlet of the stripping deamination device;
the tower bottom liquid outlet of the stripping deamination device is connected with the inlet of a fourth filter;
an ammonia water outlet of the stripping deamination device is connected with an inlet of an ammonia water storage tank;
and the outlet of the ammonia water storage tank is respectively connected with the inlet of the first pH adjusting device and the inlet of the second pH adjusting device.
As right the utility model discloses the improvement of the resourceful treatment device again of ferric trichloride etching solution:
the first pH adjusting device, the second pH adjusting device and the third pH adjusting device are used for adjusting the pH value;
the second filter, the third filter and the fourth filter are used for filtering the solution;
the oxidation reaction tank is used for oxidizing ferrous chloride in the etching solution, and the ferrous chloride is converted into ferric chloride after oxidation;
the evaporation cooling crystallization device is used for evaporation concentration under normal pressure or reduced pressure, and then is cooled and crystallized to obtain ferric trichloride hexahydrate crystals;
the dissolving tank is used for dissolving crystals;
the stripping deamination device is used for carrying out stripping deamination treatment on the solution and recovering 20% ammonia water;
the raw material storage tank stores waste ferric trichloride etching solution;
the oxidant storage tank is used for storing an oxidant, and the oxidant is hydrogen peroxide or a hypochlorous acid solution;
the water storage tank is used for storing water;
the concentrated hydrochloric acid storage tank is used for storing a hydrochloric acid solution, and the mass concentration of the concentrated hydrochloric acid storage tank is 20-31%;
the ammonia water storage tank is used for storing ammonia water with the mass concentration of 20%;
the liquid caustic soda storage tank is used for storing a sodium hydroxide solution with the mass concentration of 30%;
the neutralization reaction device is used for neutralizing and reacting ferric hydroxide and hydrochloric acid;
and the regenerated etching solution storage tank is used for storing a regenerated ferric chloride solution.
As right the utility model discloses the further improvement of the resourceful treatment device again of ferric trichloride etching solution:
the oxidant adopts one of the following three components:
firstly, hydrogen peroxide solution;
secondly, sodium hypochlorite solution;
and thirdly, oxygen or ozone.
The utility model provides a recycling treatment process of ferric trichloride etching solution, comprising the following steps:
oxidizing ferrous chloride in the etching solution into ferric trichloride; obtaining oxidized etching solution;
step two, evaporating and concentrating the oxidized etching solution obtained in the step one, evaporating and concentrating most ferric trichloride, and cooling and crystallizing to obtain ferric chloride hexahydrate crystals; obtaining crystallization mother liquor;
step three, adding ammonia water or liquid ammonia into the crystallization mother liquor obtained in the step two, controlling the pH value to be 3-5, and converting most ferric iron in the precipitation solution into ferric hydroxide precipitate; obtaining filtrate obtained in the third step;
step four, continuously adding ammonia water or liquid ammonia into the filtrate obtained in the step three, controlling the pH value to be between 9 and 12, precipitating the residual iron ions and chromium ions in the solution to form a mixture of ferric hydroxide and chromium hydroxide, and complexing nickel and ammonia in the solution to dissolve the nickel and the chromium ions in the solution; obtaining filtrate obtained in the step four;
and fifthly, adding liquid alkali or calcium hydroxide into the filtrate obtained in the fourth step, controlling the pH value to be 12-13, then carrying out stripping deamination and recycling to obtain ammonia water or liquid ammonia, and carrying out decomplexation on nickel ions and ammonia to form nickel hydroxide precipitate for recycling.
As to the utility model discloses the improvement of the resourceful treatment process again of ferric trichloride etching solution:
in the first step:
adding an oxidant solution and concentrated hydrochloric acid into the waste ferric trichloride etching solution in the raw material storage tank to react, and oxidizing ferrous chloride in the waste ferric trichloride etching solution into ferric trichloride to obtain oxidized etching solution.
As to the utility model discloses the further improvement of the resourceful treatment process again of ferric trichloride etching solution:
in the second step:
evaporating and concentrating the oxidized etching solution at normal pressure or reduced pressure, and cooling and crystallizing to obtain ferric chloride hexahydrate crystal and crystallization mother liquor;
the ferric chloride hexahydrate crystal can be sold directly or dissolved with water in a dissolving tank to form ferric chloride dissolved solution which is temporarily stored in a regenerated etching solution storage tank and used as regenerated etching solution or water purifying agent meeting the national standard for sale.
As to the utility model discloses the further improvement of the resourceful treatment process again of ferric trichloride etching solution:
in step three:
adding ammonia water or liquid ammonia with the mass concentration of 20% into the crystallized mother liquor in a first pH adjusting device to adjust the pH to 4-4.5, converting most of ferric iron into ferric hydroxide precipitate, and then filtering in a second filter to obtain a second filter cake and a second filtrate; taking the second filtrate as filtrate obtained in the third step;
the second filter cake can be directly sold for treatment, or hydrochloric acid and water are added into a neutralization reaction device for reaction to obtain ferric trichloride solution; the ferric trichloride solution is temporarily stored in a regenerated etching solution storage tank for sale.
As to the utility model discloses the further improvement of the resourceful treatment process again of ferric trichloride etching solution:
in step four:
continuously adding ammonia water or liquid ammonia with the mass concentration of 20% into the second filtrate in a second pH adjusting device, controlling the pH to be 11, controlling the ammonia content in the solution to be about 3-10%, respectively forming ferric hydroxide and chromium hydroxide precipitates and separating out the residual iron and chromium salt, and reacting all nickel and ammonia to obtain a nickel-ammonia complex; filtering in a third filter to obtain a third filter cake and a third filtrate; and taking the third filtrate as the filtrate obtained in the fourth step.
As to the utility model discloses the further improvement of the resourceful treatment process again of ferric trichloride etching solution:
in the fifth step:
adding 30 mass percent sodium hydroxide solution or calcium hydroxide solution into the third pH adjusting device to adjust the pH to be more than 12, and converting ammonium chloride into free ammonia; then ammonia water or liquid ammonia with the mass concentration of 20 percent is recovered by stripping deamination in a stripping deamination device; obtaining tower bottom liquid and ammonia water or liquid ammonia with the mass concentration of 20%;
and in the stripping process, the nickel-ammonia complex is decomplexed to form nickel hydroxide and ammonia, the ammonia is stripped and condensed to obtain 20% ammonia water or liquid ammonia, the nickel hydroxide is precipitated to form a precipitate, the precipitate is filtered, and the filter cake is sold or pyrolyzed to form nickel oxide. And (4) discharging or evaporating and crystallizing the tower bottom liquid after adjusting the pH value to obtain sodium chloride crystals for sale.
As to the utility model discloses the further improvement of the resourceful treatment process again of ferric trichloride etching solution:
in the first step, the mass ratio of the oxidant solution to the ferric trichloride etching solution is 0.1: 2, the mass ratio of the concentrated hydrochloric acid solution to the etching solution is 0.1: 5.
as to the utility model discloses the further improvement of the resourceful treatment process again of ferric trichloride etching solution:
in the second step, the temperature of evaporation concentration is 90-120 ℃, the moisture with the mass fraction of 40-80% is evaporated, the temperature of cooling crystallization is 0-40 ℃, and the pH value of the crystallization mother liquor is 0-1.5.
As to the utility model discloses the further improvement of the resourceful treatment process again of ferric trichloride etching solution:
in the third step, the mass concentration of the hydrochloric acid participating in the reaction is 10-31%, the pH is controlled to be 1-3, and the added water amount is controlled, so that the mass content of the ferric chloride is more than 38%.
The utility model adopts a three-stage treatment method: (1) evaporating and concentrating, cooling and crystallizing, converting 40-90% ferric chloride in the etching solution into ferric chloride hexahydrate crystals, and controlling the concentration rate to control the content of chromium chloride/nickel chloride in the crystals; (2) adjusting the pH value of the crystallization mother liquor by using ammonia water, and respectively controlling the precipitation of iron under the condition of 4-4.5 and the precipitation of chromium under the condition of 11-12; since ammonia and nickel have a complexing action, ammonia and nickel form a complex dissolved substance (Ni (NH3) in the chromium-precipitated state2Cl2、Ni(NH3)4Cl2、 Ni(NH3)6Cl2) Dissolving in a solution; (3) recovering ammonia by stripping deamination, ammonia in the stripping process, nickel decomplexation and nickel hydroxide precipitation recovery.
The utility model discloses iron trichloride etching solution's resourceful processing apparatus's technical advantage does:
1. the method of evaporative cooling crystallization and pH regulation precipitation is adopted to control the quality of the recovered ferric salt, and the evaporation amount is controlled to control the contents of chromium chloride and nickel chloride in the 6-water ferric trichloride so as to ensure the quality of the 6-water ferric chloride, and the ferric chloride after the solution can be used as an etching solution or a water purifying agent;
2. the pH is adjusted by adopting 20% ammonia water or liquid ammonia, and because the ammonia water is alkalescent, the pH is easy to accurately control, so that the chromium hydroxide is not precipitated, the quality of the ferric hydroxide is controlled, and the ferric hydroxide can be used as etching solution or water purifying agent for sale after being acidified;
3. the ammonia and the nickel form a soluble complexing agent, so that the separation of the nickel from the chromium and the iron is realized, the ammonia is removed, the nickel hydroxide is separated out after the ammonia is recovered, and a nickel hydroxide product with high purity is obtained for sale or is pyrolyzed into nickel oxide for sale.
4. The utility model discloses effectual molysite, the nickel salt of having retrieved promptly utilizes evaporative cooling crystallization and ammoniation precipitation to combine again, has reduced the liquid caustic soda use amount, has reduced the manufacturing cost of technology.
Drawings
The following describes the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic view of a recycling apparatus for an etching solution of ferric trichloride.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
Embodiment 1, iron trichloride etching solution's resourceful treatment device, as shown in fig. 1, includes oxidation reaction tank 3, evaporation cooling crystallization device 4, dissolving tank 5, first pH adjusting device 9, second filter 10, second pH adjusting device 12, third filter 13, neutralization reaction device 11, third pH adjusting device 15, strip deamination device 16, fourth filter 17, raw materials storage tank 1, water storage tank 6, concentrated hydrochloric acid storage tank 7, oxidant storage tank 2, regeneration etching solution storage tank 18, aqueous ammonia storage tank 8 and liquid caustic soda storage tank 14.
The first pH adjusting device 9, the second pH adjusting device 12 and the third pH adjusting device 15 are used for adjusting the pH value;
the second filter 10, the third filter 13 and the fourth filter 17 are used for filtering the solution;
the oxidation reaction tank 3 is used for oxidizing ferrous chloride in the etching solution into ferric trichloride;
the evaporation cooling crystallization device 4 is used for evaporation concentration under normal pressure or reduced pressure, and then is cooled and crystallized to obtain ferric trichloride hexahydrate crystals;
the dissolution tank 5 is used for dissolving crystals.
The stripping deamination device 16 is used for carrying out stripping deamination treatment on the solution to recover 20% ammonia water;
the raw material storage tank 1 stores waste ferric trichloride etching solution;
the oxidant storage tank 2 is used for storing an oxidant, and the oxidant is hydrogen peroxide or a hypochlorous acid solution;
the water storage tank 6 is used for storing water;
the concentrated hydrochloric acid storage tank 7 is used for storing hydrochloric acid solution, and the mass concentration is 20-31%;
the ammonia water storage tank 8 is used for storing ammonia water with the mass concentration of 20%;
the caustic soda liquid storage tank 14 is used for storing a sodium hydroxide solution with the mass concentration of 30%;
the neutralization reaction device 11 is used for neutralizing and reacting ferric hydroxide and hydrochloric acid;
the regenerated etching solution storage tank 18 is used for storing a regenerated ferric trichloride solution.
The utility model discloses iron trichloride etching solution's resourceful processing apparatus's relation of connection is:
outlets of the raw material storage tank 1, the oxidant storage tank 2 and the concentrated hydrochloric acid storage tank 7 are all connected with an inlet of the oxidation reaction tank 3;
the outlet of the oxidation reaction tank 3 is connected with the inlet of the evaporative cooling crystallization device 4;
the solid outlet of the evaporation cooling crystallization device 4 is connected with the inlet of the dissolving tank 5; the outlet of the water storage tank 6 is connected with the inlet of the dissolving tank 5;
an outlet of the dissolving tank 5 is connected with an inlet of a regenerated etching solution storage tank 18;
the liquid outlet of the evaporative cooling crystallization device 4 is connected with the inlet of a first pH adjusting device 9;
the outlet of the first pH adjusting device 9 is connected with the inlet of a second filter 10;
the solid outlet of the second filter 10 is connected with the inlet of the neutralization reaction device 11;
outlets of the water storage tank 6 and the concentrated hydrochloric acid storage tank 7 are both connected with an inlet of the neutralization reaction device 11;
an outlet of the neutralization reaction device 11 is connected with an inlet of a regenerated etching solution storage tank 18;
the liquid outlet of the second filter 10 is connected with the inlet of a second pH adjusting device 12;
the outlet of the second pH adjusting device 12 is connected with the inlet of a third filter 13;
the liquid outlet of the third filter 13 is connected with the inlet of a third pH adjusting device 15; an outlet of the liquid caustic soda storage tank 14 is connected with an inlet of a third pH adjusting device 15;
the outlet of the third pH adjusting device 15 is connected with the inlet of a stripping deamination device 16;
an outlet of a tower bottom liquid of the stripping deamination device 16 is connected with an inlet of a fourth filter 17;
an ammonia water outlet of the stripping deamination device 16 is connected with an inlet of the ammonia water storage tank 8;
the outlet of the ammonia water storage tank 8 is respectively connected with the inlet of the first pH adjusting device 9 and the inlet of the second pH adjusting device 12.
The recycling treatment process of the ferric trichloride etching solution by using the recycling treatment device of the ferric trichloride etching solution comprises the following steps:
1) adding an oxidant solution and concentrated hydrochloric acid into the waste ferric trichloride etching solution in the raw material storage tank 1 in an oxidation reaction tank 3 for reaction, and oxidizing ferrous chloride in the waste ferric trichloride etching solution into ferric chloride to obtain oxidized etching solution;
the oxidant solution in the oxidant storage tank adopts one of the following three components:
firstly, hydrogen peroxide solution;
secondly, sodium hypochlorite solution;
and thirdly, oxygen or ozone.
The concentration of hydrogen peroxide is 10-40% and the mass concentration of sodium hypochlorite is 5-20%. The oxidant can also be oxygen with a concentration of 30-99%, or ozone.
The mass ratio of the oxidant solution to the ferric trichloride etching solution is 0.1: 2, the mass ratio of the concentrated hydrochloric acid solution to the etching solution is 0.1: 5.
2) Evaporating and concentrating the oxidized etching solution at 90-120 ℃ under normal pressure or reduced pressure, evaporating moisture with the mass fraction of 40-80%, and cooling and crystallizing (0-40 ℃) to obtain ferric chloride hexahydrate crystal and crystallization mother liquor;
the pH value of the crystallization mother liquor is about 0.1-1.5;
3) dissolving the ferric chloride hexahydrate crystal with water in a dissolving tank 5 to form ferric chloride dissolved solution, adding the ferric chloride dissolved solution into a regenerated etching solution storage tank 18, and selling the ferric chloride dissolved solution as regenerated etching solution or a water purifying agent meeting the national standard;
4) adding ammonia water with the mass concentration of 20% into the crystallization mother liquor in a first pH adjusting device 9 to adjust the pH to 4-4.5, converting most ferric chloride into ferric hydroxide precipitate, and then filtering in a second filter 10 to obtain a second filter cake and a second filtrate;
5) adding hydrochloric acid and water into the second filter cake in a neutralization reaction device 11, and reacting to obtain an iron chloride solution; adding the ferric chloride solution into a regenerated etching solution storage tank 18 for sale;
the mass concentration of the added hydrochloric acid is 10-31%, the pH is controlled to be 1-3, and the added water amount is controlled to ensure that the mass content of the ferric chloride is more than 38%;
6) continuously adding ammonia water with the mass concentration of 20% into the second filtrate in a second pH adjusting device 12, controlling the pH to be between 11 and 12, controlling the ammonia content in the solution to be about 3 to 10 percent, respectively forming ferric hydroxide and chromium hydroxide by the residual iron and chromium for precipitation, and dissolving all nickel into a nickel-ammonia complex; filtering in a third filter 13 to obtain a third filter cake and a third filtrate;
7) adding 30 mass percent sodium hydroxide solution into the third pH adjusting device 15 to adjust the pH to be more than 12, and converting ammonium chloride into free ammonia; then ammonia water with the mass concentration of 20 percent is recovered by stripping deamination in a stripping deamination device 16; obtaining tower bottom liquid and ammonia water with the mass concentration of 20%;
in the stripping process, the nickel-ammonia complex is decomplexed to form nickel hydroxide and ammonia, the ammonia is stripped and condensed to recover 20% ammonia water, and the nickel hydroxide is separated out to form a precipitate;
8) filtering the tower bottom liquid in a fourth filter 17 to obtain a fourth filter cake and a fourth filtrate;
the fourth filter cake is used as nickel hydroxide to be recycled for sale, or the nickel oxide is obtained after high-temperature pyrolysis for sale;
and adjusting the pH of the fourth filtrate to be neutral, and then performing outward feeding or evaporative crystallization to obtain sodium chloride crystals.
9) And ammonia water of 20% mass concentration are added to the first pH adjusting device 9 and the second pH adjusting device 12, respectively.
Finally, it is also noted that the above-mentioned list is only a few specific embodiments of the present invention. Obviously, the present invention is not limited to the above embodiments, and many modifications are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the invention should be considered as within the scope of the invention.
Claims (3)
1. The recycling treatment device of the ferric trichloride etching solution is characterized in that: the device comprises an oxidation reaction tank (3), an evaporation cooling crystallization device (4), a dissolving tank (5), a first pH adjusting device (9), a second filter (10), a second pH adjusting device (12), a third filter (13), a neutralization reaction device (11), a third pH adjusting device (15), a stripping deamination device (16), a fourth filter (17), a raw material storage tank (1), a water storage tank (6), a concentrated hydrochloric acid storage tank (7), an oxidant storage tank (2), a regenerated etching solution storage tank (18), an ammonia water storage tank (8) and a liquid caustic soda storage tank (14);
outlets of the raw material storage tank (1), the oxidant storage tank (2) and the concentrated hydrochloric acid storage tank (7) are all connected with an inlet of the oxidation reaction tank (3);
the outlet of the oxidation reaction tank (3) is connected with the inlet of the evaporative cooling crystallization device (4);
the solid outlet of the evaporation cooling crystallization device (4) is connected with the inlet of the dissolving tank (5); the outlet of the water storage tank (6) is connected with the inlet of the dissolving tank (5);
the outlet of the dissolving tank (5) is connected with the inlet of a regenerated etching solution storage tank (18);
the liquid outlet of the evaporative cooling crystallization device (4) is connected with the inlet of a first pH adjusting device (9);
the outlet of the first pH adjusting device (9) is connected with the inlet of a second filter (10);
the solid outlet of the second filter (10) is connected with the inlet of the neutralization reaction device (11);
outlets of the water storage tank (6) and the concentrated hydrochloric acid storage tank (7) are connected with an inlet of the neutralization reaction device (11);
the outlet of the neutralization reaction device (11) is connected with the inlet of a regenerated etching solution storage tank (18);
the liquid outlet of the second filter (10) is connected with the inlet of a second pH adjusting device (12);
the outlet of the second pH adjusting device (12) is connected with the inlet of a third filter (13);
the liquid outlet of the third filter (13) is connected with the inlet of a third pH adjusting device (15); an outlet of the liquid caustic soda storage tank (14) is connected with an inlet of a third pH adjusting device (15);
the outlet of the third pH adjusting device (15) is connected with the inlet of a stripping deamination device (16);
the tower bottom liquid outlet of the stripping deamination device (16) is connected with the inlet of a fourth filter (17);
an ammonia water outlet of the stripping deamination device (16) is connected with an inlet of an ammonia water storage tank (8);
and the outlet of the ammonia water storage tank (8) is respectively connected with the inlet of the first pH adjusting device (9) and the inlet of the second pH adjusting device (12).
2. The apparatus according to claim 1, wherein:
the first pH adjusting device (9), the second pH adjusting device (12) and the third pH adjusting device (15) are used for adjusting the pH value;
the second filter (10), the third filter (13) and the fourth filter (17) are used for filtering the solution;
the oxidation reaction tank (3) is used for oxidizing ferrous chloride in the etching solution and converting the ferrous chloride into ferric chloride after oxidation;
the evaporation cooling crystallization device (4) is used for evaporation concentration under normal pressure or reduced pressure, and then is cooled and crystallized to obtain ferric trichloride hexahydrate crystals;
the dissolving tank (5) is used for dissolving crystals;
the stripping deamination device (16) is used for carrying out stripping deamination treatment on the solution and recovering 20% of ammonia water;
the raw material storage tank (1) stores waste ferric trichloride etching solution;
the oxidant storage tank (2) is used for storing an oxidant, and the oxidant is hydrogen peroxide or a hypochlorous acid solution;
the water storage tank (6) is used for storing water;
the concentrated hydrochloric acid storage tank (7) is used for storing a hydrochloric acid solution, and the mass concentration is 20-31%;
the ammonia water storage tank (8) is used for storing ammonia water with the mass concentration of 20%;
the liquid caustic soda storage tank (14) is used for storing a sodium hydroxide solution with the mass concentration of 30%;
the neutralization reaction device (11) is used for neutralizing and reacting ferric hydroxide and hydrochloric acid;
and the regenerated etching solution storage tank (18) is used for storing a regenerated ferric chloride solution.
3. The apparatus according to claim 2, wherein:
the oxidant adopts one of the following three components:
firstly, hydrogen peroxide solution;
secondly, sodium hypochlorite solution;
and thirdly, oxygen or ozone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021719022.0U CN213802942U (en) | 2020-08-18 | 2020-08-18 | Recycling treatment device for ferric trichloride etching solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021719022.0U CN213802942U (en) | 2020-08-18 | 2020-08-18 | Recycling treatment device for ferric trichloride etching solution |
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| CN213802942U true CN213802942U (en) | 2021-07-27 |
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