CN101660173B - Method for preparing silver nitrate solution for silver electrolysis and device thereof - Google Patents

Method for preparing silver nitrate solution for silver electrolysis and device thereof Download PDF

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CN101660173B
CN101660173B CN 200910177820 CN200910177820A CN101660173B CN 101660173 B CN101660173 B CN 101660173B CN 200910177820 CN200910177820 CN 200910177820 CN 200910177820 A CN200910177820 A CN 200910177820A CN 101660173 B CN101660173 B CN 101660173B
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reactor
nitrate solution
silver nitrate
hydrogen peroxide
silver
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CN101660173A (en
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周松林
赵继武
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Yanggu Xiangguang Copper Co Ltd
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Yanggu Xiangguang Copper Co Ltd
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Abstract

The invention relates to the field of silver electrolysis, in particular to a method for preparing silver nitrate solution for silver electrolysis. The method can be used for preparing the silver nitrate solution by adding raw materials with the mixture ratio into a reactor for reaction, wherein the mixture ratio among the raw materials of silver powder, nitric acid, hydrogen peroxide and water is 100kg: 30-40L: 20-40L: 60L; and the concentration of the nitric acid NHO3 is 50%, and the concentration of the hydrogen peroxide H2O2 is 30-50%. The invention also provides a device for preparing the silver nitrate solution. In the reaction process of adding the nitric acid to dissolve silver, the hydrogen peroxide is continuously added into the reaction solution, and the main response equation is 2Ag+2HNO3+H2O2=2AgNO3+2H2O, so that a great deal of oxynitrides (NO and NO2) can be prevented from being produced in the reaction process, and the pollution of the oxynitrides for the environment can be eliminated; and meanwhile, the consumption of the nitric acid is recued, and the liquid manufacturing efficiency is improved.

Description

Silver nitrate solution preparation method and device that a kind of silver-colored electrolysis is used
Technical field
The present invention relates to silver-colored electrolysis field, particularly relate to silver nitrate solution preparation method and device that a kind of silver-colored electrolysis is used.
Background technology
Silver nitrate solution is the main raw material in the silver-colored electrolytic process, generally still adopts traditional liquid making method both at home and abroad at present, i.e. reaction by silver powder and concentrated nitric acid obtains, and reaction formula is Ag+HNO 3=AgNO 3+ NOx (NO, NO 2)+H 2O, as seen, traditional liquid making method can make HNO in the liquid making process 3In 1/3 N form oxynitrides NOx (NO, NO 2) gas, these gases are harmful to the health of human body.The enterprise that has directly discharges this NOx gas, severe contamination working space and atmospheric environment; The enterprise that has dissolves this gas absorption with absorption agent, but can produce the problem that absorption liquid is handled again, can pollute environment equally.And traditional liquid making mode production efficiency is low, and nitric acid consumption is big.
Summary of the invention
The problem that technical problem to be solved by this invention is a solution preparation silver nitrate solution contaminate environment, production efficiency is low, nitric acid consumption is big.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention provides the silver nitrate solution preparation method that a kind of silver-colored electrolysis is used, silver powder is added in the normal pressure reactor, in the reaction process that adds nitric acid dissolve silver, continuously add hydrogen peroxide, obtain silver nitrate solution with this, principal reaction is 2Ag+2HNO 3+ H 2O 2=2AgNO 3+ 2H 2O.
Aforesaid method is specially in reactor and adds following proportion raw material reaction and obtain silver nitrate solution, and described raw material and proportioning thereof are silver powder: nitric acid: hydrogen peroxide: water=100kg: 30～40L: 20～40L: 60L; Nitric acid HNO wherein 3Concentration be 50%, oxydol H 2O 2Concentration be 30～50%.
Based on the above method, described reaction is divided into two stages, and the concrete steps in each stage are as follows:
Fs:
The silver powder that adds 200kg in step 1, the reactor;
Add the deionized water of 120L and 50% concentrated nitric acid solution 28L in step 2, the nitration mixture groove, stir and obtain the fs after 2～3 minutes and use salpeter solution;
Step 3, to be 30～50% hydrogen peroxide with concentration constantly join in the reactor with the flow of 200～300ml/min, and after 3～4 minutes, the fs that step 2 is obtained joins in the reactor with salpeter solution again; Above-mentioned hydrogen peroxide and salpeter solution all add from the bottom of reactor;
Step 4, after reaction in 1～1.5 hour the silver nitrate solution that obtains to dashpot, this moment, the temperature of silver nitrate solution was 40～45 ℃ from reactor overflow, concentration is 120g/L;
Subordinate phase:
Step 5, when the silver nitrate solution temperature that obtains when step 4 drops to 25 ℃, add the 49L concentrated nitric acid and stir after 2～3 minutes and obtain the subordinate phase silver nitrate solution;
Step 6, to be 30～50% hydrogen peroxide with concentration constantly join in the reactor with the flow of 200～300ml/min, and after 3～4 minutes, the subordinate phase that step 5 is obtained joins in the reactor with silver nitrate solution again; Above-mentioned hydrogen peroxide and salpeter solution all add from the bottom of reactor;
Step 7, after reaction in 2～3 hours the silver nitrate solution that obtains from reactor overflow to dashpot and obtain the finished product silver nitrate solution after filtration, this moment, the concentration of silver nitrate solution was 450g/L.
Further, first or subordinate phase in, the temperature on reactor top is 65 ℃, the temperature of bottom is 85 ℃; If temperature of lower＞93 ℃ stop hydrogen peroxide volume pump and mixed acid liquid volume pump simultaneously.
The silver nitrate solution preparation facilities that the present invention also provides a kind of silver-colored electrolysis to use, comprise reactor, dashpot, concentrated nitric acid storage tank, hydrogen peroxide storage, nitration mixture groove and Controlling System, described reactor is provided with the bottom that inlet and spillway and inlet are positioned at reactor, and spillway is positioned at the top of reactor; Described dashpot has an inlet and first, second two outlets, and inlet is communicated with the spillway on reactor top; Described concentrated nitric acid storage tank is used to store dense pin acid and carries concentrated nitric acid to the nitration mixture groove by the concentrated nitric acid volume pump; Described hydrogen peroxide storage tank is used to store hydrogen peroxide and carries the inlet of hydrogen peroxide to the reactor by the hydrogen peroxide volume pump; Described nitration mixture groove has clear water inlet, concentrated nitric acid inlet and elementary silver nitrate solution inlet, and quantitatively at the uniform velocity export inlet on the reactor to by the acid solution that the mixed acid liquid volume pump is finished being mixed in the nitration mixture groove, the clear water inlet is communicated with the clear water water-supply line, the concentrated nitric acid inlet is communicated to the concentrated nitric acid storage tank, elementary silver nitrate solution inlet is communicated to first outlet of dashpot, and second outlet of dashpot is communicated to finished product silver nitrate solution output channel; Described Controlling System comprises control unit and timing unit, and timing unit begins and start the mixed acid liquid volume pump by control unit when Preset Time arrives in timing under the triggering of hydrogen peroxide volume pump initiating signal.
Also comprise the temperature sensor that is arranged on reactor lower part in the said apparatus, control unit receives temperature signal that this temperature sensor sends and closes hydrogen peroxide volume pump and mixed acid liquid volume pump during in temperature＞93 ℃ simultaneously.
The present invention in the reaction process that adds nitric acid dissolve silver, continuously adds hydrogen peroxide, and the principal reaction formula is 2Ag+2HNO 3+ H 2O 2=2AgNO 3+ 2H 2O stops a large amount of oxynitrides of output (NO and NO in the reaction process with this 2), eliminate the pollution of oxynitrides to environment, reduce nitric acid consumption simultaneously, improve liquid making efficient.
Description of drawings
The silver nitrate solution preparation facilities structural representation that Fig. 1 uses for a kind of silver-colored electrolysis of the present invention.
Embodiment
Make detailed explanation below in conjunction with the silver nitrate solution preparation facilities that accompanying drawing is used a kind of silver-colored electrolysis of the present invention.
As shown in Figure 1, this device comprises reactor 4, dashpot 5, concentrated nitric acid storage tank 2, hydrogen peroxide storage tank 1, nitration mixture groove 3 and Controlling System.
Reactor 4 is provided with the bottom that inlet and spillway and inlet are positioned at reactor, and spillway is positioned at the top of reactor, and the below of reactor is provided with mixer for liquid 41, is used to mix acid solution and the hydrogen peroxide that input comes in and is delivered to inlet on the reactor 4.
Dashpot 5 has an inlet and first, second two outlets, and its inlet is communicated with the spillway on reactor 4 tops.
Concentrated nitric acid storage tank 2 is used to store dense pin acid, carries concentrated nitric acid to nitration mixture groove 3 by concentrated nitric acid volume pump 21;
Hydrogen peroxide storage tank 1 is used to store hydrogen peroxide, carries hydrogen peroxide and through the inlet of mixer for liquid 41 to the reactor 4 by hydrogen peroxide volume pump 11;
Nitration mixture groove 3 has clear water inlet 31, concentrated nitric acid inlet 32 and elementary silver nitrate solution inlet 33, and quantitatively at the uniform velocity output and of the acid solution of finishing being mixed in the nitration mixture groove by mixed acid liquid volume pump 34 through the inlet of mixer for liquid 41 to the reactor 4, clear water inlet 31 is communicated with the clear water water-supply line, concentrated nitric acid inlet 32 is communicated to concentrated nitric acid storage tank 2, and elementary silver nitrate solution inlet 33 is communicated to first outlet 52 of dashpot 5; Second outlet 53 of dashpot 5 is communicated to finished product silver nitrate solution output channel, and elementary silver nitrate solution is delivered to nitration mixture groove 3 or finished product silver nitrate solution output channel by the adjusting of manual valve 54,55.
Controlling System comprises control unit and timing unit, and timing unit begins and start mixed acid liquid volume pump 34 by control unit when Preset Time arrives in timing under the triggering of hydrogen peroxide volume pump 11 initiating signals.
The temperature sensor 42 that the bottom of reactor 4 is provided with, control unit receive temperature signal that temperature sensor 42 sends and close hydrogen peroxide volume pump 11 and mixed acid liquid volume pump 31 during in this temperature＞93 ℃ simultaneously.Above-mentioned control all can be implemented by known technology.
The silver nitrate solution preparation method that silver-colored electrolysis provided by the invention is used adds silver powder in the normal pressure reactor, in the reaction process that adds nitric acid dissolve silver, continuously adds hydrogen peroxide, obtains silver nitrate solution with this, and principal reaction is 2Ag+2HNO 3+ H 2O 2=2AgNO 3+ 2H 2O.Tool is local to be said, adds following proportion raw material reaction and obtain silver nitrate solution in reactor, and wherein raw material and proportioning thereof are silver powder: nitric acid: hydrogen peroxide: water=100kg: 30～40L: 20～40L: 60L; Wherein the content of silver powder is 99.99%, nitric acid HNO 3Concentration be 50%, oxydol H 2O 2Concentration be 30～50%.Above-mentioned raw materials and mass percent can adopt the prominent example of executing of following several concrete enforcement:
Embodiment 1, silver powder: nitric acid: hydrogen peroxide: water=100kg: 30L: 20L: 60L;
Embodiment 2, silver powder: nitric acid: hydrogen peroxide: water=100kg: 35L: 30L: 60L;
Embodiment 3, silver powder: nitric acid: hydrogen peroxide: water=100kg: 40L: 40L: 60L;
Aforesaid method is divided into two stages to carry out, and in conjunction with the accompanying drawings 1, the concrete steps in each stage are as follows:
Fs:
Step 1, open screw feeder 7, in reactor 4, add the silver powder of 200kg;
Step 2, the valve of opening the technology ventilator trunk and blower fan, and beat priming valve door on the clear water water supply line adds 120L in nitration mixture groove 3 deionized water, open concentrated nitric acid volume pump 21 simultaneously and in nitration mixture groove 3, add 50% concentrated nitric acid solution 28L, start nitration mixture groove agitator, move after 2～3 minutes, stop to stir the salpeter solution that the solution in this moment nitration mixture groove was used as the fs;
Step 3, startup hydrogen peroxide volume pump 11, being 30～50% hydrogen peroxide with concentration constantly joins in the reactor 4 with the flow of 200～300ml/min, after 3～4 minutes, restart mixed acid liquid volume pump 34, the fs that step 2 is obtained joins in the reactor 4 simultaneously with salpeter solution; Above-mentioned hydrogen peroxide and salpeter solution all add from the bottom of reactor 4, and in reaction process, hydrogen peroxide adds always;
Step 4, along with the continuous adding of hydrogen peroxide and salpeter solution, they in reactor with silver powder reaction after, form silver nitrate solution and overflow to the dashpot 5, in reaction process, can emit heat from the top of reactor, the temperature of solution can constantly raise, the temperature on general reactor top is about 65 ℃, and the temperature of bottom is 85 ℃, if temperature of lower＞93 ℃, reaction can be interlocked and be stopped, and promptly hydrogen peroxide volume pump 11 and mixed acid liquid volume pump 34 stop simultaneously.When solution had all overflowed in the dashpot 5, the reaction of fs finished, and the used time is approximately 1h～1.25h, and this moment, the temperature of silver nitrate solution was approximately 40～45 ℃, and concentration is about 120g/L.
Subordinate phase:
Step 5, start dashpot transferpump 51, the silver nitrate solution that step 4 is obtained is transported in the nitration mixture groove 3 through two core strainers 6, this moment, the temperature of silver nitrate solution was 40～45 ℃, the entrance of cooling water valve of the coiled pipe cooler 35 in the nitration mixture groove 3 can start (design temperature is 30 ℃) automatically, when solution temperature drops to 25 ℃, the entrance of cooling water valve of coiled pipe cooler is closed automatically, start concentrated nitric acid volume pump 21 this moment, the 49L concentrated nitric acid is joined in the nitration mixture groove 3, start the agitator of nitration mixture groove, stir after 2～3 minutes, stop to stir, obtain the subordinate phase silver-colored solution of pin acid;
Step 6, start hydrogen peroxide volume pump 11, being 30～50% hydrogen peroxide with concentration constantly joins in the reactor with the flow of 200～300ml/min, and after 3～4 minutes, the subordinate phase that step 5 is obtained joins in the reactor with silver nitrate solution again; The same with step 3, above-mentioned hydrogen peroxide and silver nitrate solution all add from the bottom of reactor, and in reaction process, hydrogen peroxide adds always;
Step 7, similar to step 4, continuous adding along with hydrogen peroxide and silver nitrate solution, they continue reaction with silver powder and form silver nitrate solution and overflow to the dashpot 5 from the top of reactor 3 in reactor, in reaction process, can emit heat, the temperature of solution can constantly raise, the temperature on general reactor top is about 65 ℃, and the temperature of bottom is 85 ℃, if temperature of lower＞93 ℃, reaction can be interlocked and be stopped, be that hydrogen peroxide volume pump 11 and mixed acid liquid volume pump 34 stop simultaneously, when solution had all overflowed in the dashpot, the reaction of subordinate phase finished, the used time is approximately 2～3 hours, and this moment, the concentration of silver nitrate solution was 450g/L.
The present invention is not limited to above-mentioned preferred forms, and anyone should learn the structural changes of making under enlightenment of the present invention, and every have identical or close technical scheme with the present invention, all falls within protection scope of the present invention.

Claims (4)

1. the silver nitrate solution preparation method that silver-colored electrolysis is used is characterized in that being divided into two stages, and the concrete steps in each stage are as follows:
Fs:
The silver powder that adds 200kg in step 1, the reactor;
Add the water of 120L and 50% concentrated nitric acid solution 28L in step 2, the nitration mixture groove, stir and obtain the fs after 2～3 minutes and use salpeter solution;
Step 3, to be 30～50% hydrogen peroxide with concentration constantly join in the reactor with the flow of 200～300mL/min, and after 3～4 minutes, the fs that step 2 is obtained joins in the reactor with salpeter solution again; Above-mentioned hydrogen peroxide and salpeter solution all add from the bottom of reactor;
Step 4, after reaction in 1～1.5 hour the silver nitrate solution that obtains to dashpot, this moment, the temperature of silver nitrate solution was 40～45 ℃ from reactor overflow, concentration is 120g/L;
Subordinate phase:
Step 5, when the silver nitrate solution temperature that obtains when step 4 drops to 25 ℃, add the 49L concentrated nitric acid and stir after 2～3 minutes and obtain the subordinate phase silver nitrate solution;
Step 6, to be 30～50% hydrogen peroxide with concentration constantly join in the reactor with the flow of 200～300mL/min, and after 3～4 minutes, the subordinate phase that step 5 is obtained joins in the reactor with silver nitrate solution again; Above-mentioned hydrogen peroxide and silver nitrate solution all add from the bottom of reactor;
Step 7, after reaction in 2～3 hours the silver nitrate solution that obtains from reactor overflow to dashpot and obtain the finished product silver nitrate solution after filtration, this moment, the concentration of silver nitrate solution was 450g/L.
2. the silver nitrate solution preparation method that a kind of silver-colored electrolysis as claimed in claim 1 is used, it is characterized in that first or subordinate phase in, the temperature on reactor top is 65 ℃, the temperature of bottom is 85 ℃; If temperature of lower＞93 ℃ stop hydrogen peroxide volume pump and acid solution volume pump simultaneously.
3. the silver nitrate solution preparation facilities that silver-colored electrolysis is used is characterized in that comprising:
Reactor is provided with the bottom that inlet and spillway and inlet are positioned at reactor, and spillway is positioned at the top of reactor;
Dashpot, it has an inlet and first, second two outlets, and described inlet is communicated with the spillway on reactor top;
The concentrated nitric acid storage tank is used to store concentrated nitric acid and carries concentrated nitric acid to the nitration mixture groove by the concentrated nitric acid volume pump;
The hydrogen peroxide storage tank is used to store hydrogen peroxide and carries the inlet of hydrogen peroxide to the reactor by the hydrogen peroxide volume pump;
The nitration mixture groove, have clear water inlet, concentrated nitric acid inlet and elementary silver nitrate solution inlet, and quantitatively at the uniform velocity export inlet on the reactor to by the acid solution that the mixed acid liquid volume pump is finished being mixed in the nitration mixture groove, the clear water inlet is communicated with the clear water water-supply line, the concentrated nitric acid inlet is communicated to the concentrated nitric acid storage tank, elementary silver nitrate solution inlet is communicated to first outlet of dashpot, and second outlet of dashpot is communicated to finished product silver nitrate solution output channel;
Controlling System comprises control unit and timing unit, and timing unit begins and start the mixed acid liquid volume pump by control unit when Preset Time arrives in timing under the triggering of hydrogen peroxide volume pump initiating signal.
4. the silver nitrate solution preparation facilities that silver-colored electrolysis as claimed in claim 3 is used, it is characterized in that also comprising the temperature sensor that is arranged on reactor lower part, control unit receives temperature signal that this temperature sensor sends and closes hydrogen peroxide volume pump and mixed acid liquid volume pump during in temperature＞93 ℃ simultaneously.
CN 200910177820 2009-09-25 2009-09-25 Method for preparing silver nitrate solution for silver electrolysis and device thereof Active CN101660173B (en)

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CN104118897A (en) * 2014-08-09 2014-10-29 江西龙天勇有色金属有限公司 Pollution-free method for controlling electric potential and oxidizing and dissolving silver
CN106048660B (en) * 2016-08-18 2018-01-16 紫金矿业集团股份有限公司 Prepare the method and its device of silver-colored electrolysis silver nitrate solution
CN113308609A (en) * 2021-05-26 2021-08-27 江苏北矿金属循环利用科技有限公司 Method for clean recovery and resource utilization of spent silver-containing waste catalyst

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