CN210974281U - High-concentration waste sulfuric acid treatment system - Google Patents
High-concentration waste sulfuric acid treatment system Download PDFInfo
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- CN210974281U CN210974281U CN201921647498.5U CN201921647498U CN210974281U CN 210974281 U CN210974281 U CN 210974281U CN 201921647498 U CN201921647498 U CN 201921647498U CN 210974281 U CN210974281 U CN 210974281U
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Abstract
The utility model discloses a high-concentration waste sulfuric acid treatment system, which comprises a sulfuric acid diluting device, a primary heat exchange system, a secondary heat exchange system, a membrane concentration system and an evaporation concentration device, wherein the sulfuric acid diluting device comprises a concentration adjusting tank and a diluting water inlet arranged on the concentration adjusting tank; the primary heat exchange system comprises a circulating pipeline connected with the concentration regulating tank, a circulating pump arranged on the circulating pipeline and a first heat exchanger arranged on the circulating pipeline; the secondary heat exchange system comprises a second heat exchanger communicated with the circulating pipeline; the membrane concentration system comprises a pretreatment filter connected with the second heat exchanger, a first-stage nanofiltration membrane filtering device connected with the pretreatment filter, a second-stage nanofiltration membrane filtering device, a sulfuric acid caching device, a reverse osmosis membrane filtering device and a washing water caching device. The utility model discloses the heat of release when the system fully retrieves and utilizes concentrated sulfuric acid to dilute has reduced energy consumption and manufacturing cost.
Description
Technical Field
The utility model relates to the technical field of wet metallurgy, in particular to a high-concentration waste sulfuric acid treatment method and system.
Background
In hydrometallurgy, a large amount of high-concentration waste sulfuric acid is generated in the metallurgical production processes of leaching, electrolytic refining and the like, the high-concentration waste sulfuric acid contains inorganic acid, organic matters and valuable metals with different concentrations, and if the high-concentration waste sulfuric acid is directly discharged, not only can the environmental pollution be caused, but also the valuable metals and the sulfuric acid in the high-concentration waste sulfuric acid cannot be reasonably recovered. At present, the neutralization method is generally adopted for treating high-concentration sulfuric acid in the prior art, and the neutralization method has the defects that the neutralization method cannot effectively recover the sulfuric acid and valuable metals, and a large amount of waste residues are accumulated. In addition, when the neutralization method is used for treatment, high-concentration waste sulfuric acid needs to be diluted, when concentrated sulfuric acid is diluted to be too low in concentration, the whole process equipment is increased, the investment is overlarge, a large amount of heat release of the concentrated sulfuric acid in the dilution process cannot be utilized, heating is needed in evaporation concentration of the sulfuric acid, and the treatment energy consumption is increased.
SUMMERY OF THE UTILITY MODEL
The utility model mainly aims to provide a high-concentration waste sulfuric acid treatment method and a system, which solve the problem of low recovery rate when treating high-concentration waste sulfuric acid in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for treating high-concentration waste sulfuric acid, comprising the steps of:
(1) diluting high-concentration waste sulfuric acid, and carrying out primary heat exchange on the diluted waste sulfuric acid solution through a primary heat exchange system;
(2) carrying out secondary heat exchange on the waste sulfuric acid solution obtained by primary heat exchange by a secondary heat exchange system to further reduce the temperature;
(3) pretreating and filtering the waste sulfuric acid liquid subjected to heat exchange again to remove particle impurities to obtain primary filtrate; removing soluble impurity salt and high-valence metal ions from the primary filtrate through primary nanofiltration, storing primary clear liquid obtained by filtering, washing and filtering the filtered primary concentrated liquid through a secondary nanofiltration membrane, and summarizing the secondary clear liquid obtained by washing and filtering the secondary nanofiltration membrane and the primary clear liquid into sulfuric acid clear liquid for storage; filtering the sulfuric acid clear solution through a reverse osmosis membrane to obtain concentrated sulfuric acid, and filtering to obtain pure water;
(4) and (4) evaporating and concentrating the obtained concentrated sulfuric acid.
Further, in the step (4), the obtained pure water is returned to be used as the water for washing and filtering the secondary nanofiltration membrane, the concentrated sulfuric acid passes through the primary heat exchange system and is preheated by using the heat generated by the primary heat exchange, and then the preheated concentrated sulfuric acid is evaporated and concentrated.
Further, deionized water is adopted to dilute high-concentration waste sulfuric acid, the concentration of sulfuric acid in the high-concentration waste sulfuric acid is more than 30%, the content of impurities is less than 20%, the concentration of sulfuric acid in the diluted waste sulfuric acid solution is 20%, heat exchange is performed again to cool the waste sulfuric acid solution, and the temperature is adjusted to be less than or equal to 45 ℃.
Furthermore, steam condensate water generated by evaporation and concentration is recycled as dilution water of the high-concentration waste sulfuric acid.
The utility model discloses high concentration sulfuric acid waste treatment system compares in prior art's advantage lies in: the high-concentration impurity-containing waste sulfuric acid is filtered and concentrated by adopting a membrane concentration system, so that the early-stage sulfuric acid dilution amount is reduced, the later-stage evaporation amount is reduced, and the production energy consumption is reduced; the utility model adopts a physical separation method, does not add chemicals such as auxiliary agents and the like, reduces the cost and simultaneously reduces the difficulty of rear-end wastewater treatment; the utility model discloses the heat of release when the system fully retrieves and utilizes concentrated sulfuric acid to dilute has reduced energy consumption and manufacturing cost.
The utility model disclosesIn the process, water in the waste sulfuric acid is recycled to the maximum extent, the pH value of the discharged wastewater is close to neutral, and the wastewater treatment and recycling difficulty is low. The concentration of the sulfuric acid solution is realized by utilizing the separation effect of the reverse osmosis membrane on the solute and the solvent. The secondary nanofiltration membrane converts high valence ions, such as Fe3+、Fe2+、Ca2+、Mg2+Equal interception on the concentrate side, H+And the plasma penetrates through the membrane and enters the clear liquid side, so that the impurity ions in the sulfuric acid solution are removed.
The utility model also discloses a high concentration sulphuric acid waste treatment system, including sulphuric acid diluting device, first heat exchange system, the concentrated system of membrane, evaporation concentration device once more, wherein: the sulfuric acid diluting device comprises a concentration adjusting tank and a diluting water inlet arranged on the concentration adjusting tank;
the primary heat exchange system comprises a circulating pipeline connected with the concentration adjusting tank, a circulating pump arranged on the circulating pipeline and a first heat exchanger arranged on the circulating pipeline;
the secondary heat exchange system comprises a second heat exchanger communicated with the circulating pipeline;
the membrane concentration system comprises a pretreatment filter connected with the second heat exchanger, a first-stage nanofiltration membrane filtering device, a second-stage nanofiltration membrane filtering device, a sulfuric acid cache device, a reverse osmosis membrane filtering device and a washing water cache device which are connected with the pretreatment filter, the first level clear liquid outlet of the first level nanofiltration membrane filtering device is connected with the liquid inlet of the sulfuric acid caching device, the first-stage concentrated solution outlet of the first-stage nanofiltration membrane filtering device is connected with the liquid inlet of the second-stage nanofiltration membrane filtering device, the water outlet of the washing water buffer device is connected with the liquid inlet of the second-level nanofiltration membrane filtering device, the second-level clear liquid outlet of the second-level nanofiltration membrane filtering device is connected with the liquid inlet of the sulfuric acid buffer device, the liquid outlet of the sulfuric acid buffer device is connected with the liquid inlet of the reverse osmosis membrane filtering device, and the reverse osmosis concentrated liquid outlet of the reverse osmosis membrane filtering device is connected with the evaporation concentration device.
Can release when concentrated sulfuric acid dilutes and remove a large amount of heats, can produce if the heat does not take away and lead to the fact serious corrosion to equipment in a large number, it is more dangerous moreover, the utility model discloses utilize first heat exchanger on circulating line and the circulating line to carry out the heat exchange with the concentrated sulfuric acid liquid of back end purification, not only reduced the temperature of sulfuric acid solution in the adjusting tank, still preheat the concentrated sulfuric acid that follow-up needs the evaporation, reduce the energy consumption of evaporimeter. The utility model adopts a physical separation method, does not add chemicals such as auxiliary agents and the like, reduces the cost and simultaneously reduces the difficulty of rear-end wastewater treatment; the utility model discloses the heat of release when the system fully retrieves and utilizes concentrated sulfuric acid to dilute has reduced energy consumption and manufacturing cost.
Furthermore, a flow regulating valve is further arranged on the circulating pipeline. The flow regulating valve can effectively regulate the flow of the waste sulfuric acid liquid entering the membrane concentration system.
Furthermore, a reverse osmosis concentrated solution outlet of the reverse osmosis membrane filtering device is connected with a second heat exchanger, and the second heat exchanger is connected with the evaporation and concentration device. Concentrated sulfuric acid after reverse osmosis membrane filters is through evaporating preheating with the first heat exchanger of concentration control jar in the anterior segment technology, further reduces the evaporation energy consumption in later stage.
Furthermore, a reverse osmosis clear liquid outlet of the reverse osmosis membrane filtering device is connected with a water inlet of the washing and filtering water caching device. Therefore, the pure water obtained through reverse osmosis filtration can be used as the washing and filtering water of the secondary nanofiltration membrane in the washing and filtering water of the former process, and the recovery rate of the waste sulfuric acid solution is further improved.
Further, an evaporation condensate outlet of the evaporation and concentration device is communicated with a dilution water inlet. The evaporation condensate generated by evaporation and condensation is recycled to the former process to be used as water for diluting concentrated sulfuric acid.
Further, the air conditioner is provided with a fan,
the first-stage nanofiltration membrane filtering device intercepts organic matters with the molecular weight of 200-1000 and dissolved 2-valent metal ions.
The secondary nanofiltration membrane filtering device intercepts 200-1000 molecular weight and dissolved 2-valent metal ions.
The reverse osmosis membrane filtering device intercepts organic matters with molecular weight more than 100 and dissolved salts.
The pretreatment filter adopts an intermetallic compound inorganic membrane filter element
Therefore, the utility model reduces the early stage sulfuric acid dilution amount, reduces the later stage evaporation amount, and reduces the production energy consumption; the utility model adopts a physical separation method, does not add chemicals such as auxiliary agents and the like, reduces the cost and simultaneously reduces the difficulty of rear-end wastewater treatment; the utility model discloses the heat of release when the system fully retrieves and utilizes concentrated sulfuric acid to dilute has reduced energy consumption and manufacturing cost.
The present invention will be further described with reference to the accompanying drawings and the detailed description. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which form a part of the disclosure, are included to assist in understanding the disclosure, and the description provided herein and the accompanying drawings, which are related thereto, are intended to explain the disclosure, but do not constitute an undue limitation on the disclosure.
In the drawings:
FIG. 1 is a schematic view of the equipment flow of the high-concentration waste sulfuric acid treatment system of the present invention.
The relevant references in the above figures are:
1: a concentration adjusting tank;
2: a first heat exchanger;
3: a second heat exchanger;
4: a pretreatment filter;
5: a first-stage nanofiltration membrane filtering device;
6: a secondary nanofiltration membrane filtering device;
7: a sulfuric acid buffer device;
8: a reverse osmosis membrane filtration device;
9: a washing water caching device;
10: an evaporation concentration device;
11: a first high pressure pump;
12: a flow regulating valve;
13: a second high pressure pump;
14: a third high pressure pump;
15: a fourth high pressure pump.
Detailed Description
The present invention will be described more fully with reference to the accompanying drawings. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. Before the present invention is described with reference to the accompanying drawings, it is to be noted that:
the technical solutions and features provided in the present invention in each part including the following description may be combined with each other without conflict.
Moreover, the embodiments of the invention described in the following description are generally only examples of a subset of the invention, and not all examples. Therefore, all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention shall fall within the protection scope of the present invention.
With respect to the terms and units of the present invention. The terms "comprising," "having," and any variations thereof in the description and claims of this invention and the related sections are intended to cover non-exclusive inclusions.
The high-concentration waste sulfuric acid treatment method comprises the following steps:
diluting high-concentration waste sulfuric acid, and carrying out primary heat exchange on the diluted waste sulfuric acid solution through a primary heat exchange system;
carrying out secondary heat exchange on the waste sulfuric acid solution obtained by primary heat exchange by a secondary heat exchange system to further reduce the temperature;
pretreating and filtering the waste sulfuric acid liquid subjected to heat exchange again to remove particle impurities to obtain primary filtrate;
removing soluble impurity salt and high-valence metal ions from the primary filtrate through primary nanofiltration, storing primary clear liquid obtained by filtering, washing and filtering the filtered primary concentrated liquid through a secondary nanofiltration membrane, and summarizing the secondary clear liquid obtained by washing and filtering the secondary nanofiltration membrane and the primary clear liquid into sulfuric acid clear liquid for storage;
filtering the sulfuric acid clear solution through a reverse osmosis membrane to obtain concentrated sulfuric acid, and filtering to obtain pure water;
(4) and (4) evaporating and concentrating the obtained concentrated sulfuric acid.
And (4) returning the obtained pure water to be used as water for washing and filtering the secondary nanofiltration membrane, preheating the concentrated sulfuric acid by the heat generated by the primary heat exchange through a primary heat exchange system, and then evaporating and concentrating the preheated concentrated sulfuric acid.
Diluting high-concentration waste sulfuric acid by using deionized water, wherein the concentration of sulfuric acid in the high-concentration waste sulfuric acid is more than 30%, the content of impurities is less than 20%, the concentration of sulfuric acid in the diluted waste sulfuric acid solution is 20%, cooling the waste sulfuric acid solution by heat exchange again, and adjusting the temperature to be less than or equal to 45 ℃.
High concentration spent sulfuric acid processing system, including sulphuric acid diluting device, first heat exchange system, membrane concentration system, evaporation concentration device 10 once more, wherein:
the sulfuric acid diluting device comprises a concentration adjusting tank 1 and a diluting water inlet arranged on the concentration adjusting tank 1;
the primary heat exchange system comprises a circulating pipeline connected with the concentration adjusting tank 1, a circulating pump arranged on the circulating pipeline and a first heat exchanger 2 arranged on the circulating pipeline;
the secondary heat exchange system comprises a second heat exchanger 3 communicating with the circulation circuit;
the membrane concentration system comprises a pretreatment filter 4 connected with the second heat exchanger 3, a first-stage nanofiltration membrane filtering device 5 connected with the pretreatment filter 4, a second-stage nanofiltration membrane filtering device 6, a sulfuric acid cache device 7, a reverse osmosis membrane filtering device 8 and a washing and filtering water cache device 9, the first-level clear liquid outlet of the first-level nanofiltration membrane filtering device 5 is connected with the liquid inlet of the sulfuric acid buffer device 7, the first-stage concentrated solution outlet of the first-stage nanofiltration membrane filtering device 5 is connected with the solution inlet of the second-stage nanofiltration membrane filtering device 6, the water outlet of the washing and filtering water buffer device 9 is connected with the liquid inlet of the second-level nanofiltration membrane filtering device 6, a second-level clear liquid outlet of the second-level nanofiltration membrane filtering device 6 is connected with a liquid inlet of the sulfuric acid buffer device 7, the liquid outlet of the sulfuric acid buffer device 7 is connected with the liquid inlet of the reverse osmosis membrane filtering device 8, and the reverse osmosis concentrated liquid outlet of the reverse osmosis membrane filtering device 8 is connected with the evaporation concentration device 10.
And the circulating pipeline is also provided with a flow regulating valve.
And a reverse osmosis concentrated solution outlet of the reverse osmosis membrane filtering device 8 is connected with the second heat exchanger 3, and the second heat exchanger 3 is connected with the evaporation and concentration device 10.
And a reverse osmosis clear liquid outlet of the reverse osmosis membrane filtering device 8 is connected with a water inlet of the washing and filtering water caching device 9.
And an evaporation condensate outlet of the evaporation and concentration device 10 is communicated with a dilution water inlet.
The first-stage nanofiltration membrane filtering device 5 intercepts organic matters with the molecular weight of 200-1000 and dissolved 2-valent metal ions.
The secondary nanofiltration membrane filtering device 6 intercepts the metal ions with the molecular weight of 200-1000 and the dissolved valence-2.
The reverse osmosis membrane filtering device 8 intercepts organic matters with molecular weight more than 100 and dissolved salts.
As shown in figure 1, in the high concentration waste sulfuric acid treatment system of the utility model, a dilution water inlet is arranged on a concentration adjusting tank 1, a circulating pipeline connected with the concentration adjusting tank 1 is arranged on the concentration adjusting tank 1, a first high pressure pump 1, a flow regulating valve 12 and a first heat exchanger 2 are arranged on the circulating pipeline, the circulating pipeline is connected with a second heat exchanger 3, the second heat exchanger 3 is connected with a pretreatment filter 4, the pretreatment filter 4 is connected with a first-stage nanofiltration membrane filtering device 5, a second high pressure pump 13 is arranged between the pretreatment filter 4 and the first nanofiltration membrane filtering device 5, a first-stage clear liquid outlet of the first-stage nanofiltration membrane filtering device 5 is connected with a liquid inlet of a sulfuric acid caching device 7, a first-stage concentrated liquid outlet of the first-stage nanofiltration membrane filtering device 5 is connected with a liquid inlet of a second-stage nanofiltration membrane filtering device 6, a water outlet of a washing and filtering device 9 is connected with a liquid inlet of the second-, a third high-pressure pump 14 is arranged between the washing and filtering water caching device 9 and the second-stage nanofiltration membrane filtering device 6, a second-stage clear liquid outlet of the second-stage nanofiltration membrane filtering device 6 is connected with a liquid inlet of a sulfuric acid caching device 7, a liquid outlet of the sulfuric acid caching device 7 is connected with a liquid inlet of a reverse osmosis membrane filtering device 8, a fourth high-pressure pump 15 is further arranged on a connecting pipeline of the sulfuric acid caching device 7 and the reverse osmosis membrane filtering device 8, a reverse osmosis concentrated liquid outlet of the reverse osmosis membrane filtering device 8 is connected with an evaporation concentration device 10, a reverse osmosis concentrated liquid outlet of the reverse osmosis membrane filtering device 8 is connected with a second heat exchanger 3, and the second heat exchanger 3 is connected with the evaporation concentration device 10. And a reverse osmosis clear liquid outlet of the reverse osmosis membrane filtering device 8 is connected with a water inlet of the washing and filtering water caching device 9. And an evaporation condensate outlet of the evaporation and concentration device 10 is communicated with a dilution water inlet.
The first-stage nanofiltration membrane filtering device (5) intercepts organic matters with the molecular weight of 200-1000 and dissolved 2-valent metal ions.
The secondary nanofiltration membrane filtering device (6) intercepts the metal ions with the molecular weight of 200-1000 and the dissolved valence-2.
The reverse osmosis membrane filtering device (8) intercepts organic matters with molecular weight more than 100 and dissolved salts.
A high-concentration waste sulfuric acid treatment method is shown in figure 1, diluting waste sulfuric acid solution with sulfuric acid concentration of more than 30% and impurity content of less than 20% by dilution water injected from a concentration adjusting tank 1 and a dilution water inlet, collecting heat generated in the waste sulfuric acid dilution process by a first heat exchanger 2, feeding the diluted waste sulfuric acid solution into a second heat exchanger 3 under the pump pressure of a first high-pressure pump 11, performing heat exchange and temperature adjustment on the waste sulfuric acid solution in the second heat exchanger 3, controlling the temperature of the waste sulfuric acid solution at 45 ℃, feeding the waste sulfuric acid solution after temperature adjustment into a membrane concentration system, adjusting the flow of the waste sulfuric acid entering the membrane concentration system by a flow adjusting valve 12, feeding the waste sulfuric acid solution into a pretreatment filtering device 4 to remove impurities such as suspended particles in the waste sulfuric acid solution, and then feeding the waste sulfuric acid solution into a primary nanofiltration membrane filtering device 5 under the pump pressure of a second high-pressure pump 13 to remove soluble impurity salts and high-valence metal ions, the first-stage nanofiltration membrane filtering device 5 stores the obtained first-stage clear liquid, namely sulfuric acid, through a sulfuric acid caching device 7, the first-stage concentrated liquid obtained by the first-stage nanofiltration membrane filtering device 5, namely concentrated liquid containing high-valence metal ions, is washed and filtered by a second-stage nanofiltration membrane filtering device 6 under the action of a washing and filtering water caching device 9 and a third high-pressure pump 14, the second-stage clear liquid obtained by the second-stage nanofiltration membrane filtering device 6, namely sulfuric acid, enters the sulfuric acid caching device 7 and is converged into sulfuric acid clear liquid, the sulfuric acid clear liquid is pumped into a reverse osmosis membrane filtering device 8 through a fourth high-pressure pump 15 to be concentrated to obtain concentrated sulfuric acid and pure water, the pure water is returned to the washing and filtering water caching tank 9 to be used as washing and filtering water for washing and filtering of the second-stage nanofiltration membrane filtering device 6, the concentrated sulfuric acid is firstly evaporated and preheated by heat generated by diluting with, the evaporative condensate produced by the evaporative concentration device 10 is used as concentrated sulfuric acid diluent to be circulated into the concentration adjusting tank 1. The concentrated solution of the second-stage nanofiltration is metal miscellaneous salt separated from the concentrated sulfuric acid solution, is weakly acidic, and can enter a common wastewater treatment system or other recovery processes for treatment. The method comprises the following steps of diluting high-concentration waste sulfuric acid by using deionized water, wherein the concentration of sulfuric acid in the high-concentration waste sulfuric acid is more than 30%, the content of impurities is less than 20%, and the concentration of sulfuric acid in the diluted waste sulfuric acid solution is 20%. And carrying out heat exchange again to cool the waste sulfuric acid solution and regulating the temperature to be less than or equal to 45 ℃.
Example 1:
and (3) feeding the waste sulfuric acid solution with the sulfuric acid concentration of 40% and the impurity content of less than 15% into a concentration adjusting tank 1, and adding deionized water according to the concentrated sulfuric acid concentration and the adjusted concentration to enable the adjusted sulfuric acid concentration to be 20%. When concentrated sulfuric acid is diluted, a large amount of heat can be released, if the heat is not taken away, a large amount of acid-containing steam can be generated to cause serious corrosion to equipment, and the equipment is dangerous. The utility model discloses utilize 1 outside first high-pressure pump 11 of concentration control jar and first heat exchanger 2 to collect the heat that produces in the spent sulfuric acid dilution process and carry out the heat exchange with the concentrated sulfuric acid liquid of back end purification, not only reduced the temperature of sulfuric acid solution in the concentration control jar 1, still can be used to preheat the concentrated sulfuric acid that follow-up needs are evaporated, reduce the energy consumption of evaporative concentration device 10.
A flow regulating valve 12 is arranged on the circulating pipeline to regulate the flow of the waste sulfuric acid entering the membrane concentration system, and the waste sulfuric acid after concentration regulation and heat exchange of the first heat exchanger 2 enters the second heat exchanger 3 to regulate the temperature to 45 ℃.
The waste sulfuric acid liquid which reaches the membrane entering condition after being cooled firstly enters a pretreatment filtering device (the pretreatment filtering device adopts an intermetallic compound inorganic membrane) to remove suspended particle impurities.
The concentrated sulfuric acid solution without suspended particle impurities is fed into a first-stage nanofiltration membrane filtering device 5 through a second high-pressure pump 13 to separate soluble impurity salts and high-valence metal ions, separated first-stage clear liquid, namely sulfuric acid, enters a filtrate side and is collected in a sulfuric acid cache device 7, the first-stage concentrated solution containing the soluble impurity salts and the high-valence metal ions enters a concentrated solution side, the first-stage concentrated solution is still high-pressure and directly enters a second-stage nanofiltration membrane filtering device 6 through a series pipeline, the energy of the second high-pressure pump 13 at the front end is effectively utilized, and the operation power consumption is reduced. Wherein, the first-stage nanofiltration membrane filtering device 5 intercepts organic matters with the molecular weight of 200 and dissolved 2-valent metal ions. The secondary nanofiltration membrane filtering device 6 intercepts metal ions with the molecular weight of 200 and the dissolved valence 2. The reverse osmosis membrane filtration device 8 retains organic matter having a molecular weight of 150 and dissolved salts.
The process comprises the steps that part of sulfuric acid is still contained in the primary concentrated solution of the primary nanofiltration membrane filtering device 5, the sulfuric acid is further recycled, the subsequent treatment process of salt-containing wastewater is simplified, the primary concentrated solution of the nanofiltration membrane filtering device 5 continuously enters the secondary nanofiltration membrane filtering device 6, a washing and filtering water caching device 9 is additionally arranged at a water inlet of the secondary nanofiltration membrane filtering device 6, the primary concentrated solution is washed and filtered, the secondary nanofiltration membrane filtering device 6 also intercepts soluble impurity salts and high-valence metal ions and enters the concentrated solution side, secondary clear solution enters the sulfuric acid caching device 7 to be collected, deionized water can be added according to the washing and filtering concentration requirement in the process section, and the water produced by the subsequent reverse osmosis membrane filtration enters the secondary nanofiltration membrane filtering device 6 to wash and filter the primary concentrated solution.
The purified sulfuric acid is easily concentrated by using the reverse osmosis membrane filtering device 8, the sulfuric acid is intercepted at the concentrated solution side, water permeates through the membrane and enters the filtrate side so as to reduce the evaporation capacity of the subsequent evaporation concentration device 10, and the produced water at the filtrate side of the reverse osmosis membrane filtering device 8 returns to the front end to be used as the washing water of the second-stage nanofiltration membrane system for cyclic utilization.
The concentrated sulfuric acid solution of the reverse osmosis membrane filtering device 8 is evaporated and preheated by the first heat exchanger 2 in the former stage process, so that the evaporation energy consumption is further reduced, and the final sulfuric acid concentration can reach 98%.
The evaporator condensate water finally enters the concentration adjusting tank 1 as concentrated sulfuric acid diluent in a circulating mode, and finally the water is recycled, so that water resources are saved, and waste water discharge is reduced.
Example 2
And (3) feeding the waste sulfuric acid solution with the sulfuric acid concentration of 50% and the impurity content of less than 10% into a concentration adjusting tank 1, and adding deionized water according to the concentrated sulfuric acid concentration and the adjusted concentration to enable the adjusted sulfuric acid concentration to be 20%. When concentrated sulfuric acid is diluted, a large amount of heat can be released, if the heat is not taken away, a large amount of acid-containing steam can be generated to cause serious corrosion to equipment, and the equipment is dangerous. The utility model discloses utilize 1 outside first high-pressure pump 11 of concentration control jar and first heat exchanger 2 to collect the heat that produces in the spent sulfuric acid dilution process and carry out the heat exchange with the concentrated sulfuric acid liquid of back end purification, not only reduced the temperature of sulfuric acid solution in the concentration control jar 1, still can be used to preheat the concentrated sulfuric acid that follow-up needs are evaporated, reduce the energy consumption of evaporative concentration device 10.
A flow regulating valve 12 is arranged on the circulating pipeline to regulate the flow of the waste sulfuric acid entering the membrane concentration system, and the waste sulfuric acid after concentration regulation and heat exchange of the first heat exchanger 2 enters the second heat exchanger 3 to regulate the temperature to be 40 ℃.
The waste sulfuric acid liquid which reaches the membrane entering condition after being cooled firstly enters a pretreatment filtering device (the pretreatment filtering device adopts an intermetallic compound inorganic membrane) to remove suspended particle impurities.
The concentrated sulfuric acid solution without suspended particle impurities is fed into a first-stage nanofiltration membrane filtering device 5 through a second high-pressure pump 13 to separate soluble impurity salts and high-valence metal ions, separated first-stage clear liquid, namely sulfuric acid, enters a filtrate side and is collected in a sulfuric acid cache device 7, the first-stage concentrated solution containing the soluble impurity salts and the high-valence metal ions enters a concentrated solution side, the first-stage concentrated solution is still high-pressure and directly enters a second-stage nanofiltration membrane filtering device 6 through a series pipeline, the energy of the second high-pressure pump 13 at the front end is effectively utilized, and the operation power consumption is reduced. Wherein, the first-stage nanofiltration membrane filtering device 5 intercepts organic matters with the molecular weight of 500 and dissolved 2-valent metal ions. The secondary nanofiltration membrane filtering device 6 intercepts 500 molecular weight and dissolved 2-valent metal ions. The reverse osmosis membrane filtration device 8 retains organic matter having a molecular weight of 250 and dissolved salts.
The process comprises the steps that part of sulfuric acid is still contained in the primary concentrated solution of the primary nanofiltration membrane filtering device 5, the sulfuric acid is further recycled, the subsequent treatment process of salt-containing wastewater is simplified, the primary concentrated solution of the nanofiltration membrane filtering device 5 continuously enters the secondary nanofiltration membrane filtering device 6, a washing and filtering water caching device 9 is additionally arranged at a water inlet of the secondary nanofiltration membrane filtering device 6, the primary concentrated solution is washed and filtered, the secondary nanofiltration membrane filtering device 6 also intercepts soluble impurity salts and high-valence metal ions and enters the concentrated solution side, secondary clear solution enters the sulfuric acid caching device 7 to be collected, deionized water can be added according to the washing and filtering concentration requirement in the process section, and the water produced by the subsequent reverse osmosis membrane filtration enters the secondary nanofiltration membrane filtering device 6 to wash and filter the primary concentrated solution.
The purified sulfuric acid is easily concentrated by using the reverse osmosis membrane filtering device 8, the sulfuric acid is intercepted at the concentrated solution side, water permeates through the membrane and enters the filtrate side so as to reduce the evaporation capacity of the subsequent evaporation concentration device 10, and the produced water at the filtrate side of the reverse osmosis membrane filtering device 8 returns to the front end to be used as the washing water of the second-stage nanofiltration membrane system for cyclic utilization.
The concentrated sulfuric acid solution of the reverse osmosis membrane filtering device 8 is evaporated and preheated by the first heat exchanger 2 in the former stage process, so that the evaporation energy consumption is further reduced, and the final sulfuric acid concentration can reach 98%.
The evaporator condensate water finally enters the concentration adjusting tank 1 as concentrated sulfuric acid diluent in a circulating mode, and finally the water is recycled, so that water resources are saved, and waste water discharge is reduced.
Example 3
And (3) feeding the waste sulfuric acid solution with the sulfuric acid concentration of 55% and the impurity content of less than 5% into a concentration adjusting tank 1, and adding deionized water according to the concentrated sulfuric acid concentration and the adjusted concentration to enable the adjusted sulfuric acid concentration to be 20%. When concentrated sulfuric acid is diluted, a large amount of heat can be released, if the heat is not taken away, a large amount of acid-containing steam can be generated to cause serious corrosion to equipment, and the equipment is dangerous. The utility model discloses utilize 1 outside first high-pressure pump 11 of concentration control jar and first heat exchanger 2 to collect the heat that produces in the spent sulfuric acid dilution process and carry out the heat exchange with the concentrated sulfuric acid liquid of back end purification, not only reduced the temperature of sulfuric acid solution in the concentration control jar 1, still can be used to preheat the concentrated sulfuric acid that follow-up needs are evaporated, reduce the energy consumption of evaporative concentration device 10.
A flow regulating valve 12 is arranged on the circulating pipeline to regulate the flow of the waste sulfuric acid entering the membrane concentration system, and the waste sulfuric acid after concentration regulation and heat exchange of the first heat exchanger 2 enters the second heat exchanger 3 to regulate the temperature to 35 ℃.
The waste sulfuric acid liquid which reaches the membrane entering condition after being cooled firstly enters a pretreatment filtering device (the pretreatment filtering device adopts an intermetallic compound inorganic membrane) to remove suspended particle impurities.
The concentrated sulfuric acid solution without suspended particle impurities is fed into a first-stage nanofiltration membrane filtering device 5 through a second high-pressure pump 13 to separate soluble impurity salts and high-valence metal ions, separated first-stage clear liquid, namely sulfuric acid, enters a filtrate side and is collected in a sulfuric acid cache device 7, the first-stage concentrated solution containing the soluble impurity salts and the high-valence metal ions enters a concentrated solution side, the first-stage concentrated solution is still high-pressure and directly enters a second-stage nanofiltration membrane filtering device 6 through a series pipeline, the energy of the second high-pressure pump 13 at the front end is effectively utilized, and the operation power consumption is reduced. Wherein, the first-stage nanofiltration membrane filtering device 5 intercepts the organic matters with the molecular weight of 1000 and the dissolved 2-valent metal ions. The secondary nanofiltration membrane filtering device 6 intercepts 1000 molecular weight and dissolved 2-valent metal ions. The reverse osmosis membrane filtration device 8 retains organic matter having a molecular weight of 350 and dissolved salts.
The process comprises the steps that part of sulfuric acid is still contained in the primary concentrated solution of the primary nanofiltration membrane filtering device 5, the sulfuric acid is further recycled, the subsequent treatment process of salt-containing wastewater is simplified, the primary concentrated solution of the nanofiltration membrane filtering device 5 continuously enters the secondary nanofiltration membrane filtering device 6, a washing and filtering water caching device 9 is additionally arranged at a water inlet of the secondary nanofiltration membrane filtering device 6, the primary concentrated solution is washed and filtered, the secondary nanofiltration membrane filtering device 6 also intercepts soluble impurity salts and high-valence metal ions and enters the concentrated solution side, secondary clear solution enters the sulfuric acid caching device 7 to be collected, deionized water can be added according to the washing and filtering concentration requirement in the process section, and the water produced by the subsequent reverse osmosis membrane filtration enters the secondary nanofiltration membrane filtering device 6 to wash and filter the primary concentrated solution.
The purified sulfuric acid is easily concentrated by using the reverse osmosis membrane filtering device 8, the sulfuric acid is intercepted at the concentrated solution side, water permeates through the membrane and enters the filtrate side so as to reduce the evaporation capacity of the subsequent evaporation concentration device 10, and the produced water at the filtrate side of the reverse osmosis membrane filtering device 8 returns to the front end to be used as the washing water of the second-stage nanofiltration membrane system for cyclic utilization.
The concentrated sulfuric acid solution of the reverse osmosis membrane filtering device 8 is evaporated and preheated by the first heat exchanger 2 in the former stage process, so that the evaporation energy consumption is further reduced, and the final sulfuric acid concentration can reach 98%.
The evaporator condensate water finally enters the concentration adjusting tank 1 as concentrated sulfuric acid diluent in a circulating mode, and finally the water is recycled, so that water resources are saved, and waste water discharge is reduced.
The contents of the present invention have been explained above. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. Based on the above-mentioned contents of the present invention, all other embodiments obtained by those skilled in the art without creative efforts shall fall within the protection scope of the present invention.
Claims (7)
1. High concentration spent sulfuric acid processing system, its characterized in that includes sulphuric acid diluting device, first heat exchange system, membrane concentration system, evaporation concentration device (10) once more, wherein:
the sulfuric acid diluting device comprises a concentration adjusting tank (1) and a diluting water inlet arranged on the concentration adjusting tank (1);
the primary heat exchange system comprises a circulating pipeline connected with the concentration adjusting tank (1), a circulating pump arranged on the circulating pipeline and a first heat exchanger (2) arranged on the circulating pipeline;
the system comprises a second heat exchanger (3) communicating with the circulation circuit;
the membrane concentration system comprises a pretreatment filter (4) connected with a second heat exchanger (3), a first-stage nanofiltration membrane filtering device (5) connected with the pretreatment filter (4), a second-stage nanofiltration membrane filtering device (6), a sulfuric acid caching device (7), a reverse osmosis membrane filtering device (8) and a washing water caching device (9), wherein a first-stage clear liquid outlet of the first-stage nanofiltration membrane filtering device (5) is connected with a liquid inlet of the sulfuric acid caching device (7), a first-stage concentrated liquid outlet of the first-stage nanofiltration membrane filtering device (5) is connected with a liquid inlet of the second-stage nanofiltration membrane filtering device (6), a water outlet of the washing water caching device (9) is connected with a liquid inlet of the second-stage nanofiltration membrane filtering device (6), a second-stage clear liquid outlet of the second-stage nanofiltration membrane filtering device (6) is connected with a liquid inlet of the sulfuric acid caching device (7), and a liquid outlet of the sulfuric acid caching device (7) is connected with a liquid inlet of the reverse, and a reverse osmosis concentrated solution outlet of the reverse osmosis membrane filtering device (8) is connected with the evaporation and concentration device (10).
2. The high concentration waste sulfuric acid treatment system as claimed in claim 1, wherein a flow regulating valve is further provided on the circulation line.
3. The high concentration waste sulfuric acid treatment system according to claim 1, wherein the reverse osmosis concentrate outlet of the reverse osmosis membrane filtration unit (8) is connected to a second heat exchanger (3), and the second heat exchanger (3) is connected to an evaporative concentration unit (10).
4. The high concentration waste sulfuric acid treatment system according to claim 1, wherein the reverse osmosis clear liquid outlet of the reverse osmosis membrane filtration device (8) is connected to the water inlet of the washing water buffer device (9).
5. The high concentration spent sulfuric acid treatment system according to claim 1, wherein the evaporative condensate outlet of the evaporative concentration device (10) is communicated with the dilution water inlet.
6. The high concentration spent sulfuric acid treatment system according to claim 1,
the first-stage nanofiltration membrane filtering device (5) intercepts organic matters with the molecular weight of 200-1000 and dissolved 2-valent metal ions;
the secondary nanofiltration membrane filtering device (6) intercepts the metal ions with the molecular weight of 200-1000 and the dissolved valence 2;
the reverse osmosis membrane filtering device (8) intercepts organic matters with molecular weight more than 100 and dissolved salts.
7. The high-concentration waste sulfuric acid treatment system according to claim 1, wherein the pretreatment filter (4) employs an intermetallic inorganic membrane filter element.
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