CN112588008A - Brine denitration and ammonium removal integrated treatment system for full-brine alkali preparation - Google Patents
Brine denitration and ammonium removal integrated treatment system for full-brine alkali preparation Download PDFInfo
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- CN112588008A CN112588008A CN202011401577.5A CN202011401577A CN112588008A CN 112588008 A CN112588008 A CN 112588008A CN 202011401577 A CN202011401577 A CN 202011401577A CN 112588008 A CN112588008 A CN 112588008A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
- C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a brine denitration and ammonium removal integrated treatment system for total-brine alkali production, which sequentially comprises an activated carbon filter, a primary diversion tank, a secondary diversion tank, an ammonium removal tower, a 10 ℃ condensation chamber, a tertiary diversion tank, a quartic diversion tank, a high-pressure pump, a ceramic nanofiltration membrane, a 5 ℃ condensation chamber and a two-stage material pushing centrifuge, wherein brine is heated by a low-temperature heating plate and subjected to mass transfer and heat transfer by boiling water after being filtered by activated carbon; sodium hypochlorite is added through the primary baffling groove and the secondary baffling groove, then flows into the ammonium removing tower, and volatile aerial fog is collected by a 25 ℃ condensing chamber through an impact fan; cooling bittern in condensing chamber at 10 deg.C, adding hydrochloric acid and Na2SO3Removing free chlorine; filtering by a ceramic nanofiltration membrane to obtain trapped lean nitrate solution and discharged rich nitrate solution; the obtained film rich nitrate solution passes through a condensation chamber with the temperature of 5 ℃ and a two-stage pusher centrifuge to obtain Na2SO4·10H2And O, separating the lean nitrate solution, combining the separated lean nitrate solution and the trapped lean nitrate solution to obtain the finished product recovered water. The method has high denitration and ammonium removal efficiency and low cost, and the obtained reclaimed water product meets the alkali making requirement.
Description
Technical Field
The invention relates to the technical field of brine alkali preparation, in particular to a brine denitration and ammonium removal integrated treatment system for full-brine alkali preparation.
Background
The production of chlor-alkali has high energy consumption and certain pollution. The state requires that an ion membrane process alkali-making process is required to be used in a new project of the caustic soda industry, and an old diaphragm electrolysis process is eliminated in a limited period. However, the new ion membrane caustic soda production process has very strict requirements on various indexes of brine in an electrolytic cell, and enterprises which generally use an ion membrane method to produce caustic soda rarely use brine to prepare the caustic soda, and basically use solid salt to dissolve the solid salt into saturated brine for treatment. In order to meet the requirements of energy conservation and emission reduction of a new caustic soda industry, part of domestic manufacturers begin to research and partially or completely use brine for alkali preparation, wherein Shaanxi Jintai chemical company Limited is more prominent in the aspect of alkali preparation by doping brine, and total alkali preparation by brine is realized at present.
The industry already has a total-brine alkali-making process, but the quality requirement on brine is higher. The brine is subjected to ammonium removal and denitration treatment to control SS to be below 0.3ppm, calcium and magnesium ions are detected as 0 by titration, ICP is used for detection, the total content of ammonium is less than 2ppm, free chlorine is not contained, and sulfate ions are less than 3 g/L. After the full-brine alkali preparation is realized, on the premise that the quality of finished alkali is not influenced, solid salt is not needed in the original primary brine refining, and all brine is conveyed by an external pipeline, so that raw salt purchasing is reduced, the production water for dissolving salt is reduced, the consumption of refining agent and steam is greatly reduced, the energy conservation and consumption reduction are realized, and the sustainable development of enterprises is ensured.
Various substances in brine can affect the quality of brine, and the quality of brine directly affects the performances of an ion membrane and a cathode-anode net so as to affect the quality of finished alkali. Such as NH in brine4 +Higher content of NCl in the electrolytic bath3The concentrated chlorine liquid is enriched in liquid chlorine, and the accumulated chlorine liquid with a certain concentration can explode under the induction of the external environment to cause a large accident, which is also the main reason that many enterprises dare not to increase the consumption of brine. In addition, for example, brine contains a large amount of Na2SO4(about 10g/L in mass concentration), and Na, if not treated in time, is accumulated to a certain extent2SO4Will be separated out in the catholyte and cover the surface of the catholyte, increasing the escape pressure of hydrogen bubbles, thereby leading H to be2Reverse osmosis to the anode area causes the hydrogen content in the chlorine to rise and cause explosion, and the voltage of the cell rises, so that the power consumption is increased.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides an integrated treatment system for denitration and ammonium removal of brine for total-brine alkali preparation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a brine denitration and ammonium removal integrated treatment system for total-brine alkali production sequentially comprises an activated carbon filter, a primary diversion tank, a secondary diversion tank, an ammonium removal tower, a 10 ℃ condensation chamber, a tertiary diversion tank, a quartic diversion tank, a high-pressure pump, a ceramic nanofiltration membrane, a 5 ℃ condensation chamber and a two-stage material pushing centrifuge along brine feeding, brine enters from the top of the activated carbon filter and is filtered by activated carbon to remove most suspended matters and organic impurities, a low-temperature heating plate is arranged on the bottom wall of the activated carbon filter, and 100 ℃ boiling water is introduced into the bottom of the side wall of the activated carbon filter and used for rapid mass and heat transfer;
when the temperature of the brine is 50 +/-5 ℃, the brine sequentially enters a primary baffling tank and a secondary baffling tank, sodium hypochlorite reacts with the brine in two batches, and ammonium salts in the brine are converted into extremely volatile monochloramine and dichloramine;
bittern flows into and removes the ammonium tower, it is equipped with the impulse fan to remove ammonium tower middle part, bittern flows down to impulse fan one side top position, the compressed air is blown into to the position of impulse fan opposite side below, drive the high-speed rotation of impulse fan through compressed air, play the effect that the fog was made, was swept and the air current drives, volatile aerial fog flows into 25 ℃ condensation chamber through removing the ammonium top of the tower, obtain monochloramine and dichloramine liquid and collect after the condensation, reach and remove NH4 +The purpose is to;
cooling the ammonium-removed brine in a condensation chamber at 10 ℃ in advance, and then passing through a third baffling tank and a fourth baffling tank once, wherein hydrochloric acid is added into the third baffling tank to adjust the pH value to be 4-8, and Na is added into the fourth baffling tank2SO3Removing free chlorine;
then the mixture is sent into a ceramic nanofiltration membrane by a high-pressure pump for filter pressing, one side of the ceramic nanofiltration membrane obtains trapped lean nitrate liquid, and the other side of the ceramic nanofiltration membrane obtains membrane rich nitrate liquid;
cooling the film-out rich nitrate solution in a condensation chamber at 5 ℃ to ensure that Na2SO4Primary crystallization, and final two-stage pushMaterial centrifuge, on the one hand Na formation2SO4·10H2Discharging the O out of the system, obtaining separated lean nitrate solution on the other hand, and combining the separated lean nitrate solution and the retained lean nitrate solution to obtain finished product recovered water;
the recovered water is subjected to ammonium removal and denitration integrated treatment, is used as a production raw material of caustic soda, and can be mixed with production water and salt-containing condensate in proportion to realize appropriate concentration of alkali preparation solution, so that the process of preparing the total halogen or partially doped halogen is realized.
Preferably, the temperature of the low temperature heating plate ranges from 70 to 80 ℃.
Further, the specific gravity of the sodium hypochlorite divided into two batches is as follows: 10-20% of the first diversion trench and 80-90% of the second diversion trench.
Further, the recovered water is further subjected to primary salt hydration.
Further, the obtained sodium sulfate decahydrate was sent to the anhydrous sodium sulfate production step.
Further, the recovered water is sampled and monitored by an ICP (inductively coupled plasma) analyzer in the alkali preparation process, such as NH (hydrogen) in the alkali preparation liquid4 +If the content cannot be reduced, the consumption of the recovered water is reduced, and the salt-containing condensate or the production water is supplemented for replacement; when the content of sulfate radicals in the alkali liquor is increased, the flow of dechlorinated light brine for salt preparation is increased, and simultaneously, the salt-containing condensate or production water is supplemented to primary brine.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the method, ammonium salt components in brine are quickly removed through the processes of activated carbon filtration, heat transfer and mass transfer quick heating, batch sodium hypochlorite addition and ammonium impact removal; part of free chlorine can be introduced while ammonium is removed, so that the process of 10 ℃ pre-condensation, hydrochloric acid pH adjustment, sodium sulfite free chlorine removal, nanofiltration, 5 ℃ condensation, double-material extrusion and centrifugation is adopted to obtain recovered water subjected to denitration and ammonium removal integrated treatment, and the recovered water is mixed with production water and salt-containing condensate to realize proper concentration of alkali preparation solution, so that the alkali preparation process of full-halogen or partial-halogen mixing is realized;
2. according to the invention, the rich nitrate solution and the poor nitrate solution are separated or combined in sequence, mutual reinforcement is realized among all processes and devices, the denitration efficiency is high, the cost is low, and the obtained recovered water product meets the alkali making requirement.
Drawings
Fig. 1 is a schematic structural diagram (horizontally arranged) of an integrated treatment system for denitration and ammonium removal of brine for total-halogen alkali production according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, a brine denitration that full bittern system alkali was used removes ammonium integration processing system includes activated carbon filter, a diversion groove, secondary diversion groove, removes ammonium tower, 10 ℃ condensation chamber, cubic diversion groove, quartic diversion groove, high-pressure pump, ceramic nanofiltration membrane, 5 ℃ condensation chamber and doublestage along brine feeding in proper order and pushes away material centrifuge, and specific process is as follows: the brine enters from the top of the activated carbon filter, most suspended matters and organic impurities are filtered out by activated carbon filtration, the bottom wall of the activated carbon filter is provided with a low-temperature heating plate, and the bottom of the side wall of the activated carbon filter is also introduced with 100 ℃ boiling water for rapid mass and heat transfer; when the temperature of the brine is 50 +/-5 ℃, the brine sequentially enters a primary baffling tank and a secondary baffling tank, sodium hypochlorite reacts with the brine in two batches, and ammonium salts in the brine are converted into extremely volatile monochloramine and dichloramine; bittern flows into and removes the ammonium tower, it is equipped with the impulse fan to remove ammonium tower middle part, bittern flows down to impulse fan one side top position, the compressed air is blown into to the position of impulse fan opposite side below, drive the high-speed rotation of impulse fan through compressed air, play the effect that the fog was made, was swept and the air current drives, volatile aerial fog flows into 25 ℃ condensation chamber through removing the ammonium top of the tower, obtain monochloramine and dichloramine liquid and collect after the condensation, reach and remove NH4 +The purpose is to; cooling the ammonium-removed brine in a condensation chamber at 10 ℃ in advance, and then passing through a third baffling tank and a fourth baffling tank once, wherein hydrochloric acid is added into the third baffling tank to adjust the pH value to be 4-8, and Na is added into the fourth baffling tank2SO3Removing free chlorine; then is pumped into the ceramic by a high pressure pumpFilter pressing the ceramic nanofiltration membrane to obtain trapped lean nitrate solution on one side of the ceramic nanofiltration membrane and membrane rich nitrate solution on the other side; cooling the film-out rich nitrate solution in a condensation chamber at 5 ℃ to ensure that Na2SO4Primary crystallization, and finally entering a two-stage pusher centrifuge to form Na on the one hand2SO4·10H2Discharging the O out of the system, obtaining separated lean nitrate solution on the other hand, and combining the separated lean nitrate solution and the retained lean nitrate solution to obtain finished product recovered water; the recovered water is subjected to ammonium removal and denitration integrated treatment, is used as a production raw material of caustic soda, and can be mixed with production water and salt-containing condensate in proportion to realize appropriate concentration of alkali preparation solution, so that the alkali preparation process of full halogen or partial halogen doping is realized; the recovered water is sampled and monitored by an ICP analyzer in the alkali preparation process, such as NH in the alkali preparation liquid4 +If the content cannot be reduced, the consumption of the recovered water is reduced, and the salt-containing condensate or the production water is supplemented for replacement; when the content of sulfate radicals in the alkali liquor is increased, the flow of dechlorinated light brine for salt preparation is increased, and simultaneously, the salt-containing condensate or production water is supplemented to primary brine.
In the actual operation process, various substances in the brine can influence the quality of the brine, and the quality of the brine directly influences the performances of an ion membrane and a cathode-anode net so as to influence the quality of finished alkali. Therefore, the study on the influence of different halogen doping amounts on the quality of alkali needs to be carried out on the premise of a new electrolytic cell and an ion membrane. However, the current Asahi formation electrolytic cell has been operated for nearly 8 years, the cathode anode net and the ion membrane are in the end of life, and if the influence of different halogen doping amounts on the quality of the electrolytic cell, the ion membrane and the alkali is to be researched, the cathode anode net and the ion membrane must be replaced. The method is characterized in that an electrolytic cell cathode-anode net and an electrolytic cell ion membrane are planned to be replaced every month from 3 months in 2020, meanwhile, various technical indexes of the replaced electrolytic cell are continuously tracked and data are collected, on the premise that the finished product alkali is a high-grade product, the power consumption and the raw salt cost are considered, the brine mixing ratio is timely adjusted, the data are continuously tracked and collected, the best balance point of the two is found at most, and a result report is formed.
By 3 months in 2020, the company has achieved a preliminary effect according to the above invented equipment method, as follows:
1. all indexes of the finished product alkali reach the standard of a superior product.
2. The direct current power consumption of the Asahi formation electrolytic cell is below 2160 KWh/ton alkali.
3. The halogen doping ratio reaches more than 15 percent.
The following economic and social effects are expected to be achieved: first line of the Asahi chemical synthesis electrolyzer is about 16 ten thousand tons of caustic soda production capacity and 24.32 ten thousand tons of industrial salt are needed. The cost of industrial salt is about 300 yuan/ton, the cost of brine is about 41 yuan/ton, calculated by doping 15% of brine, the cost of salt can be saved by 944.8 ten thousand yuan throughout the year, and the economic benefit is better.
And further researching the results transformation difficulty analysis and popularization application prospect of the invention, the following conclusion can be obtained: the invention can be directly applied to a two-line electrolytic cell and a two-stage device, and can realize the operation of all doping brine by respectively adding a two-line three-line brine pipeline in the ammonium removal process. If the total amount is calculated according to 15% of doped brine, the cost of the original salt can be saved by 2834.4 ten thousand yuan all the year after the second-stage complete construction and the production, and the method has great popularization and application values in the industry.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A brine denitration and ammonium removal integrated treatment system for total-brine alkali production sequentially comprises an activated carbon filter, a primary diversion tank, a secondary diversion tank, an ammonium removal tower, a 10 ℃ condensation chamber, a tertiary diversion tank, a quartic diversion tank, a high-pressure pump, a ceramic nanofiltration membrane, a 5 ℃ condensation chamber and a two-stage material pushing centrifuge along brine feeding, and is characterized in that brine enters from the top of the activated carbon filter, most suspended matters and organic impurities are filtered and removed through activated carbon filtration, a low-temperature heating plate is arranged on the bottom wall of the activated carbon filter, and 100 ℃ boiling water is introduced into the bottom of the side wall of the activated carbon filter and used for rapid mass and heat transfer;
when the temperature of the brine is 50 +/-5 ℃, the brine sequentially enters a primary baffling tank and a secondary baffling tank, sodium hypochlorite reacts with the brine in two batches, and ammonium salts in the brine are converted into extremely volatile monochloramine and dichloramine;
bittern flows into and removes the ammonium tower, it is equipped with the impulse fan to remove ammonium tower middle part, bittern flows down to impulse fan one side top position, the compressed air is blown into to the position of impulse fan opposite side below, drive the high-speed rotation of impulse fan through compressed air, play the effect that the fog was made, was swept and the air current drives, volatile aerial fog flows into 25 ℃ condensation chamber through removing the ammonium top of the tower, obtain monochloramine and dichloramine liquid and collect after the condensation, reach and remove NH4 +The purpose is to;
cooling the ammonium-removed brine in a condensation chamber at 10 ℃ in advance, and then passing through a third baffling tank and a fourth baffling tank once, wherein hydrochloric acid is added into the third baffling tank to adjust the pH value to be 4-8, and Na is added into the fourth baffling tank2SO3Removing free chlorine;
then the mixture is sent into a ceramic nanofiltration membrane by a high-pressure pump for filter pressing, one side of the ceramic nanofiltration membrane obtains trapped lean nitrate liquid, and the other side of the ceramic nanofiltration membrane obtains membrane rich nitrate liquid;
cooling the film-out rich nitrate solution in a condensation chamber at 5 ℃ to ensure that Na2SO4Primary crystallization, and finally entering a two-stage pusher centrifuge to form Na on the one hand2SO4·10H2Discharging the O out of the system, obtaining separated lean nitrate solution on the other hand, and combining the separated lean nitrate solution and the retained lean nitrate solution to obtain finished product recovered water;
the recovered water is subjected to ammonium removal and denitration integrated treatment, is used as a production raw material of caustic soda, and can be mixed with production water and salt-containing condensate in proportion to realize appropriate concentration of alkali preparation solution, so that the process of preparing the total halogen or partially doped halogen is realized.
2. The integrated brine denitration and ammonium removal treatment system for total halogen alkali production according to claim 1, wherein the temperature range of the low temperature heating plate is 70-80 ℃.
3. The integrated brine denitration and ammonium removal treatment system for total halogen alkali production according to claim 1, wherein the proportion of sodium hypochlorite divided into two batches is as follows: 10-20% of the first diversion trench and 80-90% of the second diversion trench.
4. The integrated brine denitration and ammonium removal treatment system for total halogen alkali production according to claim 1, wherein the recovered water is further subjected to primary salt hydration.
5. The integrated brine denitration and ammonium removal treatment system for preparing alkali from total halogen as claimed in claim 1, wherein the obtained sodium sulfate decahydrate is sent to a anhydrous sodium sulphate process.
6. The integrated brine denitration and ammonium removal treatment system for total-halogen alkali preparation according to claim 1, wherein the recovered water is sampled and monitored by an ICP (inductively coupled plasma) analyzer in the alkali preparation process, such as NH (NH) in the alkali preparation liquid4 +If the content cannot be reduced, the consumption of the recovered water is reduced, and the salt-containing condensate or the production water is supplemented for replacement; when the content of sulfate radicals in the alkali liquor is increased, the flow of dechlorinated light brine for salt preparation is increased, and simultaneously, the salt-containing condensate or production water is supplemented to primary brine.
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| CN112588008B (en) | 2022-09-13 |
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