CN116873867A - Harmless treatment method and system for high-purity bromine - Google Patents
Harmless treatment method and system for high-purity bromine Download PDFInfo
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- CN116873867A CN116873867A CN202311153531.XA CN202311153531A CN116873867A CN 116873867 A CN116873867 A CN 116873867A CN 202311153531 A CN202311153531 A CN 202311153531A CN 116873867 A CN116873867 A CN 116873867A
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- Prior art keywords
- circulating
- hydroxide solution
- sodium hydroxide
- absorption tower
- metal box
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- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 title claims abstract description 98
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910052794 bromium Inorganic materials 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 314
- 238000010521 absorption reaction Methods 0.000 claims abstract description 152
- 229910052751 metal Inorganic materials 0.000 claims abstract description 99
- 239000002184 metal Substances 0.000 claims abstract description 99
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 44
- 239000002912 waste gas Substances 0.000 claims abstract description 31
- 239000000919 ceramic Substances 0.000 claims abstract description 24
- 238000005507 spraying Methods 0.000 claims abstract description 23
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 63
- 238000012856 packing Methods 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 238000004891 communication Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 230000001502 supplementing effect Effects 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 238000004065 wastewater treatment Methods 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 4
- 230000006378 damage Effects 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 103
- 238000006243 chemical reaction Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000000126 substance Substances 0.000 description 9
- 230000009286 beneficial effect Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 229910000435 bromine oxide Inorganic materials 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 101100298222 Caenorhabditis elegans pot-1 gene Proteins 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/09—Bromine; Hydrogen bromide
- C01B7/096—Bromine
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention belongs to the technical field of high-purity bromine treatment, and in particular relates to a harmless treatment method and a harmless treatment system of high-purity bromine, wherein the method comprises the following steps of: s110, placing a ceramic tank filled with Gao Chunxiu element with bromine content more than or equal to 98.5wt% into a metal box, and placing sodium hydroxide solution in the metal box; s120, starting the circulating absorption tower and the waste gas induced draft fan at the same time; s130, when the pH value of the solution in the metal box is monitored to be 13-14, starting a crushing device, and spraying sodium hydroxide solution from top to bottom through a nozzle during crushing; s140, after crushing, if the pH value of the solution in the metal box is monitored to be lower than 10, adding sodium hydroxide into the metal box; if the colorimeter test value in the closed chamber is monitored to exceed 10 degrees, the tetramethylammonium hydroxide solution is additionally introduced into the circulating absorption tower. The invention realizes harmless and full treatment of high-purity bromine and avoids damage caused by bromine escaping into the environment.
Description
Technical Field
The invention belongs to the technical field of high-purity bromine treatment, and particularly relates to a harmless treatment method and a harmless treatment system for high-purity bromine.
Background
At present, for emergency disposal of bromine leakage, sandy soil, dry lime or soda ash are mixed and collected and then buried, and a large amount of water is used for flushing, so that diluted wastewater is sent to a wastewater system for disposal. However, no reasonable solution is proposed for the high purity of the waste bromine, and escape of bromine from the container can be harmful to the environment and organisms.
The mode that bromine is mixed and collected by sand, dry lime or soda ash and then buried still cannot ensure that bromine cannot escape into the environment to cause harm; because of poor water solubility, simple dilution with water causes waste of water resources, and because of extremely low solubility of bromine simple substance in simple water, the treatment effect is poor.
Thus, there is a need in the art for an effective treatment for high purity bromine.
Disclosure of Invention
The invention aims to overcome the defect that high-purity bromine cannot be effectively treated in the prior art, and provides a harmless treatment method and a harmless treatment system for the high-purity bromine.
In order to achieve the above object, in a first aspect, the present invention provides a method for innocuous treatment of high-purity bromine, comprising the steps of:
s110, placing a ceramic tank filled with Gao Chunxiu element with bromine content more than or equal to 98.5wt% into a metal box with an opening at the upper end, placing sodium hydroxide solution in the metal box, and placing the metal box in a closed chamber; the colorimeter and the crushing device are arranged in the closed chamber, the crushing device comprises a hydraulic plate and a plurality of nozzles which are arranged in the hydraulic plate and are used for spraying sodium hydroxide solution, and the nozzles are arranged at intervals along the circumferential direction of the edge of the hydraulic plate and spray downwards;
s120, introducing tail gas in the closed chamber into a circulating absorption tower, introducing sodium hydroxide solution into the circulating absorption tower, and circulating bottom absorption liquid of the circulating absorption tower to the top of the circulating absorption tower for circulating absorption; the waste gas of the circulating absorption tower is led out through a waste gas induced draft fan; simultaneously starting a circulating absorption tower and an exhaust gas induced draft fan, controlling the air quantity of the exhaust gas induced draft fan to be 1950-2850 m/h, and controlling the flow quantity of circulating absorption liquid in the circulating absorption tower to be 1.5-2.5 m/h;
s130, when the pH value of the solution in the metal box is monitored to be 13-14, starting a crushing device, moving the hydraulic plate to the crushing ceramic tank towards the direction of the metal box, spraying sodium hydroxide solution from top to bottom through a nozzle during crushing, and carrying out full absorption reaction on the volatilized bromine after crushing together by matching with the sodium hydroxide solution arranged at the bottom of the metal box;
s140, after crushing, if the pH value of the solution in the metal box is monitored to be lower than 10, adding sodium hydroxide solution or sodium hydroxide solid into the metal box; if the colorimeter test value in the closed chamber is monitored to be more than 10 degrees, additionally introducing tetramethylammonium hydroxide solution into the circulating absorption tower;
and S150, when the pH value of the absorption liquid in the metal box is not lower than 13 and is maintained for 4-6min, reducing the frequency of the waste gas induced draft fan, removing residues in the closed chamber, and transferring the absorption liquid in the metal box.
In some preferred embodiments of the invention, the sodium hydroxide solution has a concentration of 45-55wt% and the tetramethylammonium hydroxide solution has a concentration of 45-55wt%.
In some preferred embodiments of the invention, in S110, the amount of sodium hydroxide solution is placed in the metal tank such that the liquid level is above and a distance of 30-50cm beyond the top surface of the ceramic tank.
In some preferred embodiments of the invention, in S120, sodium hydroxide solution is introduced into the circulating absorption column such that the liquid level is 50-80cm.
In some preferred embodiments of the present invention, in S130, the spraying flow rate of the sodium hydroxide solution sprayed from top to bottom through the nozzle is 1-2 m/h.
In some preferred embodiments of the present invention, in S140, the additional flow rate when the sodium hydroxide solution is additionally added in the metal tank is 15-20 m/h, and the additional flow rate when the tetramethylammonium hydroxide solution is additionally introduced in the circulating absorption tower is 15-20 m/h.
More preferably, in S140, the additional replenishment sodium hydroxide solution in the metal tank is replenished by spraying through the nozzle of the hydraulic plate.
In some preferred embodiments of the present invention, the innocuous treatment method further comprises: in S140, after crushing, if the pH value of the absorption liquid in the circulating absorption tower is monitored to be lower than 8.5, the sodium hydroxide solution is additionally supplemented in the circulating absorption tower, and the supplementing flow is controlled to be 15-20 m/h.
More preferably, the innocent treatment method further includes: if the pH value of the absorption liquid in the circulating absorption tower is monitored to be higher than 10, the introduction of the sodium hydroxide solution into the circulating absorption tower is stopped.
In a second aspect, the present invention provides a harmless treatment system for high-purity bromine, for performing the method for the harmless treatment of Gao Chunxiu elements according to the first aspect, wherein the harmless treatment system comprises:
a ceramic pot in which high-purity bromine is contained;
a metal box with an opening at the upper end and a sodium hydroxide solution placed therein, wherein a first pH meter is arranged in the metal box and is contacted with the sodium hydroxide solution; the ceramic pot is arranged in the metal box;
the metal box is positioned in the closed chamber;
a colorimeter disposed in the closed chamber;
the crushing device is positioned in the closed chamber and above the metal box, and comprises a hydraulic plate and a plurality of nozzles which are arranged in the hydraulic plate and are used for spraying sodium hydroxide solution, wherein the nozzles are arranged at intervals along the circumferential direction of the edge of the hydraulic plate and spray downwards;
the circulating absorption tower is provided with an air inlet and a liquid inlet at the middle part, a circulating outlet at the bottom, a circulating inlet and an exhaust outlet at the top, wherein the air inlet is communicated with the exhaust outlet of the closed chamber, and the circulating outlet is communicated with the circulating inlet through a circulating pump;
the alkali liquor supply unit comprises a sodium hydroxide solution supply source, a tetramethylammonium hydroxide solution supply source, a supply main pipe, branch pipes and control valves arranged on the pipelines, wherein the two supply sources are communicated with the supply main pipe, and the supply main pipe is respectively communicated with a nozzle of the crushing device, an inner cavity of the metal box and a liquid inlet of the circulating absorption tower through the branch pipes;
and an inlet of the waste gas induced draft fan is communicated with a waste gas outlet of the circulating absorption tower, and a first flowmeter is arranged on a pipeline used for the communication.
In some preferred embodiments of the invention, the innocent treatment system further comprises an interlocking control system which is respectively in interlocking connection with the pH meter, the colorimeter, the crushing device, the circulating absorption tower, the control valve on each pipeline of the alkali liquor supply unit, the waste gas induced draft fan and the flowmeter.
In some preferred embodiments of the invention, the innocent treatment system further comprises a salt-containing wastewater treatment system in communication with the liquid outlet of the metal tank.
In some preferred embodiments of the present invention, the circulating absorption tower is internally provided with an upper packing layer and a lower packing layer, the air inlet is positioned below the two packing layers, the liquid inlet is positioned in the two packing layers, and the circulating inlet is positioned above the two packing layers; and a liquid level meter is arranged on the circulating absorption tower.
In some preferred embodiments of the present invention, the structure that the circulation outlet is communicated with the circulation inlet through the circulation pump includes a first circulation pump and a second circulation pump which are connected in parallel, and a connecting pipeline thereof, a second flowmeter is arranged on a downstream connecting pipeline of the first circulation pump and the second circulation pump, and a sewage draining pipe is also arranged on a downstream connecting pipeline of the second flowmeter.
In some preferred embodiments of the invention, a second pH meter is disposed within the recycle absorber and contacts the bottom absorption liquid.
The beneficial effects are that:
according to the technical scheme, high-purity bromine is fully treated, sodium hydroxide solution sprayed from the upper part and at the bottom is fully absorbed in an omnibearing manner at the first time of volatilizing the bromine, unabsorbed bromine is continuously absorbed through a rear-end circulating absorption tower, the bromine reaction condition and escape condition are accurately monitored through the pH value and the chromaticity value, and the sodium hydroxide solution and the tetramethylammonium hydroxide solution are timely supplemented according to the conditions to accelerate the bromine reaction; thereby realizing harmless and full treatment of the high-purity bromine and avoiding harm caused by bromine escaping into the environment. The method neutralizes and reacts the high-purity bromine simple substance in a controllable environment, performs multistage absorption reaction and capture on the escaped bromine simple substance, avoids environmental pollution and biological injury caused by escape of the bromine simple substance, and can perform high-purity bromine treatment operation more safely and efficiently. In addition, the harmless treatment system does not need the participation of staff, and the staff does not directly contact with bromine simple substance, so that personal injury is avoided.
Specifically, sodium hydroxide solution is respectively injected into the absorption tower of the circulating tower and the metal box, when the exhaust draught fan is started, so that the closed chamber is under negative pressure, especially under the condition that the flow rate of circulating absorption liquid, the waste extraction air quantity and the pH value of the solution in the metal box are all in the condition that the bromine can be maximally absorbed, the crushing device is adopted to crush the ceramic tank in time, and then the crushed and volatilized bromine is fully absorbed together with the sodium hydroxide solution in the metal box through spraying holes in time, so that the bromine simple substance reacts with sodium hydroxide in the metal box to generate brine, and if the bromine simple substance which escapes due to the unobtainable reaction enters the rear-end circulating absorption tower to fully react with the sodium hydroxide; and according to the pH value of the solution in the metal box being lower than 10, timely supplementing sodium hydroxide into the metal box to ensure that the reaction speed of bromine and sodium hydroxide is at a faster level, reducing the escaped bromine amount and enabling a small amount of escaped bromine to be sufficiently and quickly captured by the circulating absorption tower; and when the escape concentration of bromine is low and can not be identified by naked eyes, a colorimeter is matched to monitor the reaction condition of bromine and sodium hydroxide solution and the escape condition of bromine, and when the chromaticity value in a closed chamber exceeds 10 degrees, the volatile bromine is relatively more at the moment, and the bromine can not be completely treated by the sodium hydroxide solution through the circulating absorption tower. Under the same conditions, if the pH value is lower than 10, sodium hydroxide is not added, the reaction of bromine and sodium hydroxide is slowed down, the sufficient absorption of bromine is not facilitated, the escaped bromine amount is increased, and the capturing of a rear-end absorption tower is not facilitated; if the chromaticity value exceeds 10 degrees, the tetramethyl ammonium hydroxide solution is not introduced, at the moment, more bromine is volatilized, the bromine cannot be completely treated by the circulating absorption tower through the sodium hydroxide solution, and the bromine escapes into the environment to cause harm.
In addition, because the solubility of bromine simple substance in pure water is extremely low, the sodium hydroxide solution and the tetramethylammonium hydroxide solution are adopted in the treatment method, bromine can be captured in real time through the absorption reaction of bromine and sodium hydroxide, the potential harm to the environment and the like caused by the fact that bromine is dissolved in a water solvent but does not participate in the absorption reaction is avoided, moreover, after the salt water generated by the absorption reaction is desalted, distilled water can be recycled to process water in a harmless treatment method of bromine, water participating in operation can be recycled, water resource loss is extremely low, and water resource can be remarkably saved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a harmless treatment system of the present invention;
FIG. 2 is a front view of a hydraulic plate portion of the present invention;
fig. 3 is a top view of fig. 2.
Description of the reference numerals
1. Ceramic tank, 2, metal box, 3, closed chamber, 4, colorimeter, 5a, first pH meter, 5b, second pH meter, 6, waste gas induced draft fan, 601, first flowmeter, 7, crushing device, 701, hydraulic plate, 702, spout, 8, circulating absorption tower, 801, air inlet, 802, liquid inlet, 803, circulating outlet, 804, circulating inlet, 805, waste gas outlet, 9, lye supply unit, 901, supply header, 10a, first circulating pump, 10b, second circulating pump, 10c, second flowmeter, 11, liquid level gauge.
Detailed Description
In the present invention, unless otherwise indicated, terms of orientation such as "upper, lower, left, right" and the like are used generally to refer to the orientation understanding shown in the drawings and in practice, and "inner, outer" refer to the inner, outer of the outline of the components.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. Wherein the terms "optional" and "optionally" mean either comprising or not comprising (or may not be present).
In a first aspect, the invention provides a harmless treatment method of high-purity bromine, comprising the following steps: s110, placing a ceramic tank filled with Gao Chunxiu element with bromine content more than or equal to 98.5wt% into a metal box with an opening at the upper end, placing sodium hydroxide solution in the metal box, and placing the metal box in a closed chamber; the colorimeter and the crushing device are arranged in the closed chamber, the crushing device comprises a hydraulic plate and a plurality of nozzles which are arranged in the hydraulic plate and are used for spraying sodium hydroxide solution, and the nozzles are arranged at intervals along the circumferential direction of the edge of the hydraulic plate and spray downwards.
The high-purity bromine of the invention can be any high-concentration bromine to be treated, such as waste gas high-purity bromine.
The innocent treatment method of the invention further comprises the following steps: s120, introducing tail gas in the closed chamber into a circulating absorption tower, introducing sodium hydroxide solution into the circulating absorption tower, and circulating bottom absorption liquid of the circulating absorption tower to the top of the circulating absorption tower for circulating absorption; the waste gas of the circulating absorption tower is led out through a waste gas induced draft fan; simultaneously starting a circulating absorption tower and an exhaust gas induced draft fan, controlling the air quantity of the exhaust gas induced draft fan to be 1950-2850 m/h, and controlling the flow quantity of circulating absorption liquid in the circulating absorption tower to be 1.5-2.5 m/h; and the air quantity and the flow of the circulating absorption liquid are controlled, so that escaped bromine can be fully contacted and reacted with sodium hydroxide solution.
The waste gas of the circulating absorption tower is led out by the waste gas induced draft fan and can be used for a waste gas treatment system.
The innocent treatment method of the invention further comprises the following steps: and S130, when the pH value of the solution in the metal box is monitored to be 13-14, starting the crushing device, moving the hydraulic plate to the crushing ceramic tank towards the direction of the metal box, spraying sodium hydroxide solution from top to bottom through a nozzle during crushing, and carrying out full absorption reaction on the volatilized bromine after crushing together by matching with the sodium hydroxide solution arranged at the bottom of the metal box. The pH value of the solution in the metal box is 13-14, which is more beneficial to the maximized rapid absorption of bromine.
In the present invention S130, the pH value of the solution in the metal box is monitored to be 13-14, wherein the initial value of the pH value of the solution in the metal box (i.e. before crushing) means that the pH value of the sodium hydroxide solution in the metal box is 13-14, and the pH value of the solution in the metal box is changed after the crushing.
The innocent treatment method of the invention further comprises the following steps: s140, after crushing, if the pH value of the solution in the metal box is monitored to be lower than 10, adding sodium hydroxide solution or sodium hydroxide solid into the metal box; if the colorimeter test value in the closed chamber is monitored to exceed 10 degrees, the tetramethylammonium hydroxide solution is additionally introduced into the circulating absorption tower. The pH value of the solution in the metal box is lower than 10, and the reaction speed of sodium hydroxide and bromine is slowed down, which is unfavorable for absorbing bromine. And the colorimeter test value exceeds 10 degrees, the bromine content in the air in the closed chamber is low, the bromine is not easy to be fully absorbed by the sodium hydroxide solution, the tetramethyl ammonium hydroxide solution is additionally introduced into the circulating absorption tower, and the full progress of accelerating the bromine reaction is realized by the mutual cooperation of the tetramethyl ammonium hydroxide and the sodium hydroxide, so that the method is favorable for fully absorbing escaped bromine.
It will be appreciated that after the metal can is placed in the enclosure, it is necessary to seal the enclosure.
In the present invention, after the sodium hydroxide solution or sodium hydroxide solid is additionally supplemented into the metal tank, the pH value of the solution in the metal tank is raised. The innocent treatment method of the invention further comprises the following steps: and S150, when the pH value of the absorption liquid in the metal box is not lower than 13 and is maintained for 4-6min, reducing the frequency of the waste gas induced draft fan, removing residues in the closed chamber, and transferring the absorption liquid in the metal box. The pH value of the absorption liquid in the metal box is not lower than 13 and is maintained for a certain time, so that bromine is basically not contained in the air in the closed chamber, the harm to staff can be avoided, and at the moment, after the frequency of the waste gas induced draft fan is reduced and the negative pressure in the closed chamber is reduced, the staff can enter the closed chamber to remove residues and the like.
In some preferred embodiments of the invention, the sodium hydroxide solution has a concentration of 45-55wt% and the tetramethylammonium hydroxide solution has a concentration of 45-55wt%. The preferred scheme is more beneficial to rapid absorption reaction of bromine.
In some preferred embodiments of the invention, in S110, the amount of sodium hydroxide solution is placed in the metal tank such that the liquid level is above and a distance of 30-50cm beyond the top surface of the ceramic tank.
In some preferred embodiments of the invention, in S120, sodium hydroxide solution is introduced into the circulating absorption column such that the liquid level is 50-80cm.
In some preferred embodiments of the present invention, in S130, the spraying flow rate of the sodium hydroxide solution sprayed from top to bottom through the nozzle is 1-2 m/h. The preferred scheme is more beneficial to rapid absorption reaction of bromine.
In some preferred embodiments of the invention, in S140, the additional flow rate when the sodium hydroxide solution is additionally supplemented in the metal tank is 15-20 m/h. The supplementary mode can be sprayed through the nozzle of the hydraulic plate, can also be directly introduced into the metal box, or can be combined with the metal box.
The supplementing amount is only favorable for improving the pH value to be in a required range of 13-14 when the sodium hydroxide solid is additionally supplemented in the metal box.
More preferably, in S140, the additional replenishment sodium hydroxide solution in the metal tank is replenished by spraying through the nozzle of the hydraulic plate. The preferred scheme is more beneficial to the full contact and rapid absorption reaction of bromine.
Preferably, in S140, the flow rate of the additional introduction of the tetramethylammonium hydroxide solution into the circulating absorption tower is 15-20 m/h.
In some preferred embodiments of the present invention, the innocuous treatment method further comprises: in S140, after crushing, if the pH value of the absorption liquid in the circulating absorption tower is monitored to be lower than 8.5, the sodium hydroxide solution is additionally supplemented in the circulating absorption tower, and the supplementing flow is controlled to be 15-20 m/h. The preferred scheme is more beneficial to capturing bromine escaping from the circulating absorption tower.
More preferably, the innocent treatment method further includes: if the pH value of the absorption liquid in the circulating absorption tower is monitored to be higher than 10, the introduction of the sodium hydroxide solution into the circulating absorption tower is stopped. The pH value of the absorption liquid in the circulating absorption tower is higher than 10, so that the sodium hydroxide solution in the circulating absorption tower is sufficient for quickly absorbing bromine without supplementing.
In the invention, the crushing device, the colorimeter, the pH meter, the circulating absorption tower, the flow control and the like can be automatically controlled through interlocking control without manual adjustment.
In a second aspect, the present invention provides a system for innocent treatment of high-purity bromine, which is used for performing the method for innocent treatment of Gao Chunxiu elements according to the first aspect.
The innocent treatment system of the invention comprises:
a ceramic pot in which high-purity bromine is contained;
a metal box with an opening at the upper end and a sodium hydroxide solution placed therein, wherein a first pH meter is arranged in the metal box and is contacted with the sodium hydroxide solution; the ceramic pot is arranged in the metal box;
the metal box is positioned in the closed chamber;
a colorimeter disposed in the closed chamber for monitoring a colorimetric value in the closed chamber;
the crushing device is positioned in the closed chamber and above the metal box, and comprises a hydraulic plate and a plurality of nozzles which are arranged in the hydraulic plate and are used for spraying sodium hydroxide solution, wherein the nozzles are arranged at intervals along the circumferential direction of the edge of the hydraulic plate and spray downwards;
the circulating absorption tower is provided with an air inlet and a liquid inlet at the middle part, a circulating outlet at the bottom, a circulating inlet and an exhaust outlet at the top, wherein the air inlet is communicated with the exhaust outlet of the closed chamber, and the circulating outlet is communicated with the circulating inlet through a circulating pump;
the alkali liquor supply unit comprises a sodium hydroxide solution supply source, a tetramethylammonium hydroxide solution supply source, a supply main pipe, branch pipes and control valves arranged on the pipelines, wherein the two supply sources are communicated with the supply main pipe, and the supply main pipe is respectively communicated with a nozzle of the crushing device, an inner cavity of the metal box and a liquid inlet of the circulating absorption tower through the branch pipes;
and an inlet of the waste gas induced draft fan is communicated with a waste gas outlet of the circulating absorption tower, and a first flowmeter is arranged on a pipeline used for the communication.
It will be appreciated that the size of the hydraulic plate is sufficient to facilitate crushing of the ceramic tank and to allow more sufficient contact of the sprayed sodium hydroxide solution with the gas, and that the size may be selected by one skilled in the art as desired.
The crushing device of the invention can also comprise other necessary components for cooperating with the hydraulic plate to perform the functions of pressing down and spraying sodium hydroxide solution, for example, a driving mechanism for driving the hydraulic plate to press down, and the like.
The door of the closed chamber of the present invention is preferably provided to be transparent so that an outdoor person can observe the operation of the crushing apparatus.
In some preferred embodiments of the invention, the innocent treatment system further comprises an interlocking control system, wherein the interlocking control system is respectively connected with the pH meter, the colorimeter, the crushing device, the circulating absorption tower, the control valve on each pipeline of the alkali liquor supply unit, the waste gas induced draft fan and the flowmeter in an interlocking manner and used for performing interlocking control. The preferable scheme is more beneficial to realizing automatic real-time control and does not need manual operation.
In some preferred embodiments of the invention, the innocent treatment system further comprises a salt-containing wastewater treatment system in communication with the liquid outlet of the metal tank. Of course, the saline wastewater may be manually transferred to a saline wastewater treatment system, or mechanically transferred.
In some preferred embodiments of the present invention, the circulating absorption tower is provided with an upper packing layer and a lower packing layer, the air inlet is positioned below the two packing layers, the liquid inlet is positioned in the two packing layers, and the circulating inlet is positioned above the two packing layers, which is more favorable for bromine absorption.
Preferably, a liquid level meter is arranged on the circulating absorption tower so as to monitor the liquid level of the circulating absorption tower.
In some preferred embodiments of the present invention, the structure that the circulation outlet is communicated with the circulation inlet through the circulation pump includes a first circulation pump and a second circulation pump which are connected in parallel, and a connecting pipeline thereof, wherein a second flowmeter is arranged on a downstream connecting pipeline of the first circulation pump and the second circulation pump, and a sewage discharge pipe is also arranged on a downstream connecting pipeline of the second flowmeter, which can increase the circulation amount and maximally promote the absorption reaction of bromine.
In some preferred embodiments of the invention, a second pH meter is disposed within the recycle absorber and contacts the bottom absorption liquid.
The following detailed description of the embodiments of the invention is exemplary and is merely illustrative of the invention and not to be construed as limiting the invention.
Example 1
A harmless treatment method of high-purity bromine is carried out in a harmless treatment system shown in fig. 1, and comprises the following steps:
s110, placing a ceramic pot 1 (Gao Chunxiu element is 100 kg) filled with Gao Chunxiu element with bromine content more than or equal to 98.5wt% into a metal box 2 with an opening at the upper end, placing sodium hydroxide solution in the metal box 2, placing the metal box 2 in a closed chamber 3, setting a first pH meter 5a in the metal box 2, and contacting the first pH meter 5a with the sodium hydroxide solution; the colorimeter 4 and the crushing device 7 are arranged in the closed chamber 3, the crushing device 7 comprises a hydraulic plate 701 and a plurality of spray nozzles 702 which are arranged in the hydraulic plate 701 and are used for spraying sodium hydroxide solution, and the spray nozzles 702 are arranged at intervals along the circumferential direction of the edge of the hydraulic plate 701 and spray downwards; the amount of sodium hydroxide solution placed in the metal tank 2 was such that the liquid level was above the top surface of the ceramic tank 1 and a distance exceeding the top surface of the ceramic tank 1 was 40cm.
S120, introducing tail gas in the closed chamber 3 into the circulating absorption tower 8, introducing sodium hydroxide solution into the circulating absorption tower 8, and circulating bottom absorption liquid of the circulating absorption tower 8 to the top of the circulating absorption tower 8 for circulating absorption; the waste gas of the circulating absorption tower 8 is led out through a waste gas induced draft fan 6; simultaneously starting the circulating absorption tower 8 and the waste gas induced draft fan 6, controlling the air quantity of the waste gas induced draft fan 6 to be 2200 m/h, and controlling the circulating absorption liquid flow in the circulating absorption tower 8 to be 2 m/h; sodium hydroxide solution was introduced into the circulating absorption column 8 so that the liquid level was 60cm.
The circulating absorption tower 8 is provided with an air inlet 801 and a liquid inlet 802 at the middle part, a circulating outlet 803 at the bottom, a circulating inlet 804 and an exhaust outlet 805 at the top, wherein the air inlet 801 is communicated with the exhaust outlet of the closed chamber 3, and the circulating outlet 803 is communicated with the circulating inlet 804 through a circulating pump; an upper packing layer and a lower packing layer are arranged in the circulating absorption tower 8, the air inlet 801 is positioned below the two packing layers, the liquid inlet 802 is positioned in the two packing layers, and the circulating inlet 804 is positioned above the two packing layers; a liquid level meter 11 is arranged on the circulating absorption tower 8; the structure that the circulation outlet 803 is communicated with the circulation inlet 804 through a circulation pump comprises a first circulation pump 10a, a second circulation pump 10b and a connecting pipeline thereof which are connected in parallel, wherein a second flowmeter 10c is arranged on a downstream connecting pipeline of the first circulation pump 10a and the second circulation pump 10b, and a sewage discharge pipe is also arranged on a downstream connecting pipeline of the second flowmeter 10 c; a second pH meter 5b is provided in the circulating absorption tower 8 and the second pH meter 5b contacts the bottom absorption liquid. The inlet of the exhaust gas induced draft fan 6 is communicated with the exhaust gas outlet 805 of the circulating absorption tower 8, and a first flowmeter 601 is arranged on a pipeline used for the communication.
The alkali liquor supply unit 9 is further arranged and comprises a sodium hydroxide solution supply source, a tetramethylammonium hydroxide solution supply source, a supply header 901, branch pipes and control valves arranged on the pipelines, wherein the two supply sources are communicated with the supply header 901, and the supply header 901 is respectively communicated with the nozzle 702 of the crushing device 7, the inner cavity of the metal box 2 and the liquid inlet 802 of the circulating absorption tower 8 through the branch pipes. An interlocking control system is also arranged and is respectively connected with the pH meter, the colorimeter 4, the crushing device 7, the circulating absorption tower 8, the control valve on each pipeline of the alkali liquor supply unit 9, the waste gas induced draft fan 6 and the flowmeter in an interlocking way and is used for interlocking control.
S130, when the pH value of the solution in the metal box 2 is monitored to be 13-14, starting a crushing device 7, moving a hydraulic plate 701 to the crushing ceramic tank 1 towards the metal box 2, spraying sodium hydroxide solution from top to bottom through a nozzle 702 while crushing, and carrying out full absorption reaction on the volatilized bromine after crushing together by matching with the sodium hydroxide solution arranged at the bottom in the metal box 2; the spraying flow of the sodium hydroxide solution from top to bottom through the nozzle 702 was 1.5 m/h.
S140, after crushing, if the pH value of the solution in the metal box 2 is monitored to be lower than 10, spraying the solution into the metal box 2 through a nozzle 702 of a hydraulic plate 701 to additionally supplement sodium hydroxide solution, wherein the supplement flow is 18 m/h; if the colorimeter 4 test value in the closed chamber 3 is monitored to exceed 10 degrees, additionally introducing a tetramethyl ammonium hydroxide solution into the circulating absorption tower 8, wherein the introduction flow rate is 18m cm < hr >; the concentration of the sodium hydroxide solution is 50wt%, and the concentration of the tetramethyl ammonium hydroxide solution is 50wt%; if the pH value of the absorption liquid in the circulating absorption tower 8 is monitored to be lower than 8.5, adding sodium hydroxide solution into the circulating absorption tower 8 additionally, and controlling the adding flow to be 18 m/h; if the pH value of the absorption liquid in the circulating absorption tower 8 is monitored to be higher than 10, the introduction of the sodium hydroxide solution into the circulating absorption tower 8 is stopped.
And S150, when the pH value of the absorption liquid in the metal box 2 is monitored to be not lower than 13 and maintained for 5min, reducing the frequency of the waste gas induced draft fan 6, removing residues in the closed chamber 3, and transferring the absorption liquid in the metal box 2 to a salt-containing wastewater treatment system for treatment.
The bromine conversion of this example was 100% (i.e., the bromine was completely absorbed to form the corresponding salt) as measured by gas chromatography (see chromatographic analysis in the fourth handbook of analytical chemistry, chemical industry Press).
Example 2
The procedure of example 1 was carried out, except that the spraying flow rate of the sodium hydroxide solution was 1 m/h by spraying the sodium hydroxide solution from top to bottom through the nozzle.
In the corresponding test, the bromine conversion of this example was 85%.
Example 3
The method according to example 1 was performed, except that the pH of the absorption liquid in the circulating absorption column was monitored to be lower than 8.5 in S140, without additional replenishment of sodium hydroxide solution in the circulating absorption column.
In the corresponding test, the bromine conversion of this example was 93%.
Comparative example 1
The procedure of example 1 was carried out without providing a colorimeter in the closed chamber, without performing a colorimetric test, and without introducing a tetramethylammonium hydroxide solution in S140.
In the corresponding test, the bromine conversion of this comparative example was 63%.
Comparative example 2
The procedure of example 1 was carried out, except that no pH meter was provided in the metal tank, and no additional sodium hydroxide solution was added to the metal tank in S140.
In the corresponding test, the bromine conversion of this comparative example was 76%.
From the above examples and comparative examples, it can be seen that the treatment of high purity bromine can be achieved and the conversion rate is high by adopting the embodiment of the present invention. Further according to the preferred embodiment of the present invention, as shown in examples 1 and examples 2-3, the conversion of bromine is further improved.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. The harmless treatment method of the high-purity bromine is characterized by comprising the following steps of:
s110, placing a ceramic tank filled with Gao Chunxiu element with bromine content more than or equal to 98.5wt% into a metal box with an opening at the upper end, placing sodium hydroxide solution in the metal box, and placing the metal box in a closed chamber; the colorimeter and the crushing device are arranged in the closed chamber, the crushing device comprises a hydraulic plate and a plurality of nozzles which are arranged in the hydraulic plate and are used for spraying sodium hydroxide solution, and the nozzles are arranged at intervals along the circumferential direction of the edge of the hydraulic plate and spray downwards;
s120, introducing tail gas in the closed chamber into a circulating absorption tower, introducing sodium hydroxide solution into the circulating absorption tower, and circulating bottom absorption liquid of the circulating absorption tower to the top of the circulating absorption tower for circulating absorption; the waste gas of the circulating absorption tower is led out through a waste gas induced draft fan; simultaneously starting a circulating absorption tower and an exhaust gas induced draft fan, controlling the air quantity of the exhaust gas induced draft fan to be 1950-2850 m/h, and controlling the flow quantity of circulating absorption liquid in the circulating absorption tower to be 1.5-2.5 m/h;
s130, when the pH value of the solution in the metal box is monitored to be 13-14, starting a crushing device, moving the hydraulic plate to the crushing ceramic tank towards the direction of the metal box, spraying sodium hydroxide solution from top to bottom through a nozzle during crushing, and carrying out full absorption reaction on the volatilized bromine after crushing together by matching with the sodium hydroxide solution arranged at the bottom of the metal box;
s140, after crushing, if the pH value of the solution in the metal box is monitored to be lower than 10, adding sodium hydroxide solution or sodium hydroxide solid into the metal box; if the colorimeter test value in the closed chamber is monitored to be more than 10 degrees, additionally introducing tetramethylammonium hydroxide solution into the circulating absorption tower;
and S150, when the pH value of the absorption liquid in the metal box is not lower than 13 and is maintained for 4-6min, reducing the frequency of the waste gas induced draft fan, removing residues in the closed chamber, and transferring the absorption liquid in the metal box.
2. The method for innocuous treatment of Gao Chunxiu element according to claim 1, wherein,
in S110, placing sodium hydroxide solution in the metal box in an amount such that the liquid level is above the top surface of the ceramic tank and exceeds the top surface of the ceramic tank by 30-50cm;
in S120, introducing sodium hydroxide solution into the circulating absorption tower to enable the liquid level to be 50-80cm;
in S130, the spraying flow of the sodium hydroxide solution sprayed from top to bottom through the nozzle is 1-2 m/h.
3. The method for innocuous treatment of Gao Chunxiu according to claim 1, wherein the concentration of the sodium hydroxide solution is 45-55wt%, and the concentration of the tetramethylammonium hydroxide solution is 45-55wt%.
4. The method for innocuous treatment of Gao Chunxiu according to claim 3, wherein in S140, the additional flow rate of the additional sodium hydroxide solution in the metal tank is 15-20 m/h, and the additional flow rate of the additional tetramethylammonium hydroxide solution in the circulating absorption tower is 15-20 m/h.
5. The method for innocuous treatment of Gao Chunxiu according to claim 4, wherein in S140, the additional sodium hydroxide solution is sprayed and supplemented through the nozzle of the hydraulic plate.
6. The method for innocuous treatment of Gao Chunxiu according to claim 1, further comprising: in S140, after crushing, if the pH value of the absorption liquid in the circulating absorption tower is monitored to be lower than 8.5, the sodium hydroxide solution is additionally supplemented in the circulating absorption tower, and the supplementing flow is controlled to be 15-20 m/h.
7. The method for innocuous treatment of Gao Chunxiu element according to claim 6, further comprising: if the pH value of the absorption liquid in the circulating absorption tower is monitored to be higher than 10, the introduction of the sodium hydroxide solution into the circulating absorption tower is stopped.
8. A harmless treatment system of high-purity bromine, for performing the method of harmless treatment of Gao Chunxiu element according to any one of claims 1 to 7, comprising:
a ceramic pot in which high-purity bromine is contained;
a metal box with an opening at the upper end and a sodium hydroxide solution placed therein, wherein a first pH meter is arranged in the metal box and is contacted with the sodium hydroxide solution; the ceramic pot is arranged in the metal box;
the metal box is positioned in the closed chamber;
a colorimeter disposed in the closed chamber;
the crushing device is positioned in the closed chamber and above the metal box, and comprises a hydraulic plate and a plurality of nozzles which are arranged in the hydraulic plate and are used for spraying sodium hydroxide solution, wherein the nozzles are arranged at intervals along the circumferential direction of the edge of the hydraulic plate and spray downwards;
the circulating absorption tower is provided with an air inlet and a liquid inlet at the middle part, a circulating outlet at the bottom, a circulating inlet and an exhaust outlet at the top, wherein the air inlet is communicated with the exhaust outlet of the closed chamber, and the circulating outlet is communicated with the circulating inlet through a circulating pump;
the alkali liquor supply unit comprises a sodium hydroxide solution supply source, a tetramethylammonium hydroxide solution supply source, a supply main pipe, branch pipes and control valves arranged on the pipelines, wherein the two supply sources are communicated with the supply main pipe, and the supply main pipe is respectively communicated with a nozzle of the crushing device, an inner cavity of the metal box and a liquid inlet of the circulating absorption tower through the branch pipes;
and an inlet of the waste gas induced draft fan is communicated with a waste gas outlet of the circulating absorption tower, and a first flowmeter is arranged on a pipeline used for the communication.
9. The harmless treatment system according to claim 8, further comprising an interlocking control system, wherein the interlocking control system is in interlocking connection with a pH meter, a colorimeter, a crushing device, a circulating absorption tower, a control valve on each pipeline of the alkali liquor supply unit, an exhaust gas induced draft fan and a flowmeter, respectively;
and/or the number of the groups of groups,
the innocent treatment system further comprises a salt-containing wastewater treatment system which is communicated with the liquid outlet of the metal box.
10. The harmless treatment system according to claim 8, wherein an upper packing layer and a lower packing layer are arranged in the circulating absorption tower, the air inlet is positioned below the two packing layers, the liquid inlet is positioned in the two packing layers, and the circulating inlet is positioned above the two packing layers; a liquid level meter is arranged on the circulating absorption tower;
and/or the number of the groups of groups,
the structure that the circulating outlet is communicated with the circulating inlet through the circulating pump comprises a first circulating pump, a second circulating pump and a connecting pipeline thereof which are connected in parallel, wherein a second flowmeter is arranged on a downstream connecting pipeline of the first circulating pump and the second circulating pump, and a sewage discharge pipe is also arranged on a downstream connecting pipeline of the second flowmeter; a second pH meter is arranged in the circulating absorption tower and contacts the bottom absorption liquid.
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