CN114291916A - System and method for recycling o-aminophenol from o-aminophenol acidification wastewater - Google Patents
System and method for recycling o-aminophenol from o-aminophenol acidification wastewater Download PDFInfo
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- CN114291916A CN114291916A CN202111669522.7A CN202111669522A CN114291916A CN 114291916 A CN114291916 A CN 114291916A CN 202111669522 A CN202111669522 A CN 202111669522A CN 114291916 A CN114291916 A CN 114291916A
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- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 title claims abstract description 162
- 239000002351 wastewater Substances 0.000 title claims abstract description 127
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000004064 recycling Methods 0.000 title claims abstract description 22
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- 229920005989 resin Polymers 0.000 claims abstract description 160
- 239000011347 resin Substances 0.000 claims abstract description 160
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- 239000007788 liquid Substances 0.000 claims abstract description 57
- 238000003795 desorption Methods 0.000 claims abstract description 30
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- 239000000706 filtrate Substances 0.000 claims description 35
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- 239000000126 substance Substances 0.000 claims description 8
- 238000007667 floating Methods 0.000 claims description 7
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
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- 238000005086 pumping Methods 0.000 claims description 5
- 238000004457 water analysis Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
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- 125000004122 cyclic group Chemical group 0.000 abstract description 2
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 abstract 1
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- 238000011001 backwashing Methods 0.000 description 9
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
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- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- CNGYZEMWVAWWOB-VAWYXSNFSA-N 5-[[4-anilino-6-[bis(2-hydroxyethyl)amino]-1,3,5-triazin-2-yl]amino]-2-[(e)-2-[4-[[4-anilino-6-[bis(2-hydroxyethyl)amino]-1,3,5-triazin-2-yl]amino]-2-sulfophenyl]ethenyl]benzenesulfonic acid Chemical compound N=1C(NC=2C=C(C(\C=C\C=3C(=CC(NC=4N=C(N=C(NC=5C=CC=CC=5)N=4)N(CCO)CCO)=CC=3)S(O)(=O)=O)=CC=2)S(O)(=O)=O)=NC(N(CCO)CCO)=NC=1NC1=CC=CC=C1 CNGYZEMWVAWWOB-VAWYXSNFSA-N 0.000 description 1
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Abstract
The invention particularly relates to a method for recovering and treating o-aminophenol in o-aminophenol acidified wastewater, and also relates to improvement of a recovery and treatment system. A recovery processing system of ortho-aminophenol in ortho-aminophenol acidized waste water includes: the system comprises an o-aminophenol acidification wastewater pool, a wastewater filter tank, a macroporous resin adsorption and desorption treatment device, a desorption liquid collection device and a sewage discharge pool; the method comprises the steps of settling and filtering the waste water, adjusting the pH to be 5-6, adsorbing the waste water by a macroporous resin adsorption column, carrying out thermokalite hydrolysis and precipitation after saturation failure, collecting analytic liquid, returning the analytic liquid to a production workshop for cyclic application treatment, and realizing colorless transparency and standard discharge of the waste water after series adsorption treatment, thereby solving the problem that the water treatment of enterprises does not reach the standard, improving the economic benefit to the maximum extent and realizing waste water treatment and resource recycling.
Description
Technical Field
The invention relates to a wastewater treatment method in chemical production, in particular to a method for recovering and treating o-aminophenol in o-aminophenol acidification wastewater, and also relates to improvement of a matched recovery treatment device structure.
Background
Ortho-aminophenol, 2-aminophenol, it is an important pharmaceutical fine chemical intermediate, the chemical formula is CH (OH) NH, white or light gray crystalline powder, change into brown or black when standing for a long time, apply to making sulfur dyes, azo dyes, fur dyes and fluorescent brightener, and medicine, plastics curing agent, etc. extensively, with the rapid development of medicine and dyeing and printing industry, the market demand to ortho-aminophenol this chemical intermediate is continuously rising, its price position rises and rises with the ship, but the domestic large-scale ortho-aminophenol production technology of the present time is mainly to catalyze the hydrogenation method, the waste water produced in the production process has high salt content, water yield is large, the organic matter concentration is high, difficult biochemistry and have certain toxicity, not only cause the discharge burden of the production enterprise, and because the ortho-aminophenol that contains in the production waste water can not be reclaimed and cause the economic loss of the enterprise, therefore, the wastewater treatment is imminent.
The prior process for treating and applying the ortho-aminophenol acidification wastewater mainly comprises the following steps: firstly, the decolorization of the activated carbon is matched with a Fenton oxidation method, but a large amount of sludge becomes dangerous waste, and the o-aminophenol in the sludge cannot be recycled, so that certain economic loss is caused; the other is electrochemical oxidation process, which features the electrochemical oxidation process of treating o-aminophenol waste water deeply in a single chamber reactor comprising three-dimensional electrode system. But the process is more complex, and the use is limited due to high requirements on personnel and equipment; thirdly, the treatment of the ortho-aminophenol acidification wastewater is carried out by matching with the Fenton oxidation method, the treatment method combines the micro-electrolysis method and the Fenton oxidation method, the process is relatively complex, the operation difficulty is higher, a large amount of corrosive liquids such as acid, alkali and the like are used in the process, the treatment risk is increased, the treatment cost is higher, and the treatment efficiency is relatively lower.
In recent years, there have been cases of application of resins to the treatment of o-aminophenol wastewater, such as: the publication No. CN102910757A [ a process for treating wastewater from o-nitrophenol production ] proposes a method for treating wastewater from o-nitrophenol production by XDA series macroporous adsorbent resins, and uses ozone to oxidize the residual organic matters in the adsorbent solution.
The publication No. CN 107129078A (ortho-aminophenol wastewater treatment and recycling method) combines a treatment method combining resin adsorption, micro-electrolysis and Fenton oxidation to treat the ortho-aminophenol wastewater and efficiently remove the ortho-aminophenol and the chroma in the wastewater, but the treatment method has the defects of relatively complex process, high operation difficulty, large consumption of corrosive liquids such as acid, alkali and the like during the treatment and higher treatment cost.
The publication number is CN108793493A [ a method for recovering and treating o-aminophenol in strong brine ], which discloses a method for recovering and utilizing a large amount of o-aminophenol contained in high-salinity wastewater by utilizing a physical adsorption method, wherein the method comprises the steps of adjusting the pH value of high-concentration o-aminophenol production wastewater in strong brine, introducing the high-concentration o-aminophenol production wastewater into macroporous styrene-based adsorption resin, adsorbing o-aminophenol on the macroporous styrene-based adsorption resin, eluting the saturated adsorption macroporous styrene-based adsorption resin by using an organic solvent, and finally recovering o-aminophenol from a solvent desorption solution. The process mainly aims at the treatment of high-salinity wastewater, and the technical scheme has the defects that firstly, concentrated sulfuric acid is used for adjusting the pH to about 2, namely, the concentrated sulfuric acid passes through an adsorption column under the condition of strong acid, the strong acid condition has high requirements on equipment, and potential safety hazards exist; secondly, after adsorption, an organic solvent (industrial methanol is indicated in the specific embodiment) is used for desorption and regeneration, and a rectification system is required to be added for recycling the organic solvent in the later period, so that the equipment cost and the recycling process flow are increased; thirdly, the desorption liquid is required to be subjected to the recovery treatment of the aminophenol finished product, and the recovery operation cost is also increased.
Therefore, it is very important to research an o-aminophenol process wastewater treatment and recovery method which has good treatment effect, low operation cost, simple operation, large o-aminophenol recovery amount and is suitable for industrial scale treatment.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a system for recovering and treating o-aminophenol in o-aminophenol acidified wastewater, which is modified by using the existing equipment, can realize the treatment of wastewater, and has the advantages of lower treatment cost and higher treatment efficiency.
The invention also provides a method for recycling the o-aminophenol in the o-aminophenol acidified wastewater, which aims to solve the problem of enterprise emission, save a large amount of water resources, realize environmental management and resource utilization and greatly improve the economic benefit of enterprises.
In order to achieve the above object, the present invention adopts the following technical solution, and a system for recovering and treating ortho-aminophenol from ortho-aminophenol acidified wastewater comprises:
an o-aminophenol acidification wastewater pool for wastewater storage and sedimentation;
the wastewater filtering tank is used for filtering the settled wastewater to obtain clear and transparent filtrate without floating oil substances;
the macroporous adsorption resin desorption treatment device is used for adsorbing o-aminophenol contained in the wastewater filtrate, and after adsorption saturation, desorption treatment is carried out in a hot alkali spraying mode to obtain desorption liquid;
the analysis liquid collecting tank is used for collecting the analysis liquid after the macroporous resin adsorption and analysis treatment;
the sewage discharge tank is used for discharging the treated wastewater after reaching the standard or recycling the wastewater, so that water resources are saved;
the waste water in the o-aminophenol acidification waste water pool enters a waste water filter tank for filtering after being settled, enters a macroporous adsorption resin analysis treatment device after being subjected to ph value adjustment, and the analysis liquid obtained after the adsorption, failure, water back flushing, alkali washing and acid circulation treatment in the macroporous adsorption resin analysis treatment device enters an analysis liquid collection tank, and the treated waste water reaching the qualified discharge standard enters a sewage discharge pool.
Furthermore, the macroporous adsorption resin analysis treatment device is composed of at least one group of macroporous adsorption resin components, preferably two groups of macroporous adsorption resin components, each group of macroporous adsorption resin components comprises three macroporous adsorption resin columns, the three macroporous adsorption resin columns are connected in series by adopting two adsorption columns for adsorption, and the other adsorption column is used for analysis.
Preferably, the macroporous adsorbent resin desorption treatment device is composed of 6 macroporous adsorbent resin columns, which are four 1200 × 3000 mm-sized columns and two 1600 × 3000 mm-sized columns, wherein three 1200 × 3000 resin columns are a group of macroporous resin adsorption modules, and the other 1200 × 3000 resin columns and two 1600 × 3000 resin columns are another group of macroporous resin adsorption modules.
Preferably, the 1200 x 3000 size column is intended to be filled with 3 squares of resin and the 1600 x 3000 size column is filled with 4 squares of resin.
Preferably, the macroporous adsorption resin columns are all rubber-lined resin columns.
The method for recovering and treating the o-aminophenol in the o-aminophenol acidified wastewater based on the o-aminophenol recovery and treatment system comprises the following steps:
s1 pretreatment: after the wastewater is settled and filtered (clear and transparent without floating oil substances), the pH value is adjusted to 5-6, the pH value is adjusted to be weak acid, alkaline impurities in the wastewater can be removed, and the macroporous adsorption resin column is favorable for better adsorbing o-aminophenol in a wastewater filtrate in an acidic environment;
s2 adsorption treatment: adjusting the water inlet temperature of the wastewater filtrate to be more than or equal to 30 ℃, preventing crystallization of o-aminophenol from separating out and blocking a pipeline, enabling the wastewater filtrate to enter a group of macroporous adsorption resin adsorption components through a wastewater pump and a feed pipeline, enabling the components to comprise No. 1, No. 2 and No. 3 resin columns, enabling the wastewater filtrate to enter the resin columns in series connection with No. 1 and No. 2 for adsorption, and directly discharging the adsorbed wastewater filtrate into a sewage discharge pool when the effluent at the bottom of No. 2 is qualified;
and S3 failure treatment: when the water outlet at the bottom of the No. 2 resin column is unqualified, the No. 1 resin column connected in series with the No. 2 resin column is failed, the wastewater filtrate is stopped from entering the No. 1 resin column, the serial connection state of the No. 1 and the No. 2 is disconnected, the serial connection of the No. 2 and the No. 3 is started, and the wastewater filtrate enters the No. 2 and the No. 3 resin column connected in series through a wastewater pump and a feed pipeline for adsorption;
s4 backflushing treatment: carrying out positive and negative water flushing on the failed 1# resin column through a circulating water pump and a circulating water pipeline so as to remove residual wastewater filtrate in a 1# resin pore passage, and discharging outlet water into a raw water pool through the positive and negative flushing pipeline;
s5 analysis and regeneration process: introducing hot alkali liquor in a dilute alkali tank heated to 80 ℃ into a 1# resin column subjected to back flushing treatment through an alkali inlet pump and an alkali inlet pipeline, and sending the desorption liquor into a desorption liquor collecting tank through a desorption liquor pipeline at the bottom of the 1# resin column when outlet water at the bottom of the 1# resin column is alkaline;
s6 washing with water and alkali treatment: after the hot alkali liquor in the step S5 is completely fed, stopping feeding the hot alkali liquor into the No. 1 resin column, simultaneously opening a circulating water pipeline of the No. 1 resin column for water washing, wherein one part of the washing alkali liquor enters a resolving liquid collecting tank through a resolving liquid pipeline, and the other part of the washing alkali liquor enters a dilute alkali tank through the resolving liquid pipeline for recycling;
s7 acid circulation treatment: and (3) pumping a certain amount of dilute hydrochloric acid into the No. 1 resin column treated by the S6 through a dilute acid pump and a dilute acid pipeline, circulating for a certain time, and ending the circulation when the PH value in the resin column is about 3.
Preferably, the water inlet temperature of the wastewater filtrate is adjusted to 30-80 ℃ in S2, so that the o-aminophenol is prevented from crystallizing out and blocking the pipeline.
Furthermore, the No. 1, the No. 2 and the No. 3 are separated independent resin columns, two resin columns are used in series every time, once the water quality at the back of the series is found to be unqualified, the former resin columns are immediately switched to be invalid, the other two resin columns are used in series, and the invalid resin columns are sequentially subjected to circulating water back flushing, hot alkali water analysis, analysis liquid collection and acid circulation treatment.
Preferably, the analysis liquid in the analysis liquid collection tank described in S5 can be directly returned to the production plant for use, and the recycling of the finished product is not required, i.e., the treatment is recycled.
Preferably, the effluent is alkaline in S5, which means that the pH value is 10-12, specifically, the effluent is determined by sampling the bottom of the No. 1 resin column and measuring the pH by a pH test paper.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the method collects high-concentration o-aminophenol production wastewater in the aminophenol acidified wastewater and passes through an adsorption column filled with macroporous resin, so that o-aminophenol contained in the wastewater is adsorbed on the adsorption resin, the resin saturated in adsorption is eluted by hot alkali water, and the eluted alkali water containing o-aminophenol can be directly returned to a production workshop for recycling; the physical adsorption and temperature-rising analysis modes are adopted, organic solvent desorption is not adopted, strong acid and strong base are not adopted, and the like, so that the recovery operation cost is greatly reduced;
(2) the treatment process has the advantages that two adsorption columns are connected in series for adsorption, and the other adsorption column is used for resolving, so that the treatment process is simple and reasonable in structure, not only can a large amount of o-aminophenol and chromaticity in the wastewater be efficiently recovered, but also the treatment efficiency is improved, and the wastewater subjected to series adsorption treatment is colorless and transparent, so that the problem that the water treatment of enterprises does not reach the standard is solved, the economic benefit is improved to the maximum extent, and the wastewater treatment and resource recycling are realized;
(3) the analytic solution collected by the analytic regeneration treatment, namely the alkali water eluent containing the o-aminophenol, is directly returned to a production workshop for recycling, finished products are not required to be recovered, and post-recovery treatment equipment and processes are saved, so that the recovery process is greatly simplified, the recovery operation cost is reduced, and the economic benefit of an enterprise is improved.
Drawings
FIG. 1 is a schematic diagram of the configuration of the recycling system of the present invention;
FIG. 2 is a flow diagram of an adsorption process according to an embodiment of the recovery process of the present invention;
FIG. 3 is a flowchart of the failure handling of one embodiment of the reclamation processing method of the present invention;
FIG. 4 is a flow diagram of a backflushing process according to one embodiment of the present invention in a recycling process;
FIG. 5 is a flow chart of an analysis process according to an embodiment of the recycling process of the present invention;
FIG. 6 is a flow chart of a regeneration process according to an embodiment of the recycling process of the present invention;
FIG. 7 is a flow diagram of an alkaline water wash treatment process according to an embodiment of the present invention;
FIG. 8 is a flow diagram of the acid recycle of one embodiment of the recovery process of the present invention.
Detailed Description
The invention will be further explained with reference to specific embodiments, without limiting the invention.
In the following examples, unless otherwise specified, the methods used were conventional, and the reagents used were all commercially available.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the accompanying drawings of the present invention, and the described embodiments are only a part of the embodiments of the present invention and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, in the figure, 1, 2, and 3 are wastewater filtrate feed valves, 4, 5, and 6 are wastewater filtrate discharge valves, 7, 8, and 9 are backwash valves, 10, 11, and 12 are forward wash valves, 13, 14, and 15 are alkali inlet valves, 16, 17, and 18 are desorption liquid discharge valves, 19, 20, and 21 are top circulation water valves, 22, 23, and 24 are bottom circulation water valves, 25, 26, and 27 are bottom acid valves, 28, 29, and 30 are top acid valves, 31, 32, and 33 are bottom string valves, 34, 35, and 36 are top string valves, and 37, 38, and 39 are string switching valves.
The invention relates to a system for recovering and treating o-aminophenol in o-aminophenol acidification wastewater, which comprises: an o-aminophenol acidification wastewater pool for wastewater storage and sedimentation;
the wastewater filtering tank is used for filtering the settled wastewater to obtain clear and transparent filtrate without floating oil substances;
the macroporous adsorption resin desorption treatment device is used for adsorbing o-aminophenol contained in the wastewater filtrate, and after adsorption saturation, desorption treatment is carried out in a hot alkali spraying mode to obtain desorption liquid; the macroporous adsorption resin analysis treatment device is composed of a group of macroporous adsorption resin components, wherein the macroporous adsorption resin components comprise No. 1, No. 2 and No. 3 which are separated and independent and are rubber-lined resin columns, two of the components are used in series every time, once the water quality after the components are connected in series is found to be unqualified, the former components are immediately switched to be invalid, the other two components are simultaneously used in series, and the invalid components are sequentially subjected to circulating water back flushing, hot alkali water analysis, analysis liquid collection and acid circulation treatment;
specifically, external connecting pipelines and control valves of the No. 1, the No. 2 and the No. 3 are the same, namely the top parts of the No. 1, the No. 2 and the No. 3 are provided with feed valves, the bottom parts of the No. 1, the No. 2 and the No. 3 are provided with discharge valves, the feed valves are communicated with a wastewater filtrate feed pipeline, the discharge valves are communicated with a water outlet pipeline, and the water outlet pipeline is communicated with a sewage collecting pool; series valves are arranged at the top and the bottom of the 1#, the 2#, and the 3#, the three columns can form a series pipeline through the series valves, and the series valves can be communicated with the series pipeline; the top and the bottom of the 1#, the 2#, and the 3# are respectively provided with a circulating water valve, the three columns can form a circulating water pipeline through the circulating water valves, and the circulating water valves can be communicated with the circulating water pipeline; the top parts of 1#, 2# and 3# are all provided with a backwashing valve, the bottom parts of the three columns are all provided with a forward washing valve, the three columns can form a forward backwashing pipeline through the forward washing valve and the backwashing valve, the forward washing valve and the backwashing valve are both communicated with the forward backwashing pipeline, and the forward backwashing pipeline is communicated with a north raw water pool; the bottoms of the No. 1, the No. 2 and the No. 3 are provided with analytic liquid discharge valves which are communicated with an analytic liquid pipeline which is communicated with an analytic liquid collecting tank; the tops of No. 1, No. 2 and No. 3 are all provided with an alkali inlet valve which is communicated with an alkali circulating pipeline, one side of the alkali circulating pipeline is used for discharging alkali liquor from the dilute alkali tank, and the other side of the alkali circulating pipeline is returned to the dilute alkali tank through a solution pipeline; acid inlet valves are arranged at the tops of the 1#, the 2#, and the 3#, acid circulating valves are arranged at the bottoms of the three columns, the three columns can form an acid circulating pipeline through the acid inlet valves and the acid circulating valves, and the acid inlet valves and the acid circulating valves can be communicated with the acid circulating pipeline;
the analysis liquid collecting tank is used for collecting the analysis liquid after the macroporous resin adsorption and analysis treatment, and the analysis liquid collecting tank is respectively communicated with No. 1, No. 2 and No. 3 through an analysis liquid pipeline and analysis liquid discharge valves at the bottoms of the three resin columns;
the sewage discharge tank is used for discharging the treated wastewater after reaching the standard or recycling the treated wastewater, so that water resources are saved, and the sewage discharge tank can be communicated with No. 1, No. 2 and No. 3 through a water outlet pipeline and discharge valves at the bottoms of the three resin columns respectively;
the waste water in the ortho-aminophenol acidification waste water pool enters a waste water filter tank for filtering after being settled, the temperature is raised to be more than or equal to 30 ℃ after the pH value is adjusted to be 5-6, the waste water enters a macroporous adsorption resin analysis treatment device, the analysis liquid obtained after adsorption, invalidation, water back flushing, water alkali washing and acid circulation treatment in the macroporous adsorption resin analysis treatment device enters an analysis liquid collecting tank, and the treated waste water reaching the qualified discharge standard enters a sewage discharge pool.
Referring to fig. 2 to 8, the method for recovering and treating ortho-aminophenol in ortho-aminophenol acidified wastewater based on the above system for recovering and treating ortho-aminophenol in ortho-aminophenol acidified wastewater specifically includes the following steps:
s1 pretreatment: after the wastewater is settled and filtered (clear and transparent without floating oil substances), the pH value is adjusted to 5-6, the pH value is adjusted to be weak acid, alkaline impurities in the wastewater can be removed, and the macroporous adsorption resin column is favorable for better adsorbing o-aminophenol in a wastewater filtrate in an acidic environment;
s2 adsorption treatment: opening a feeding valve at the upper part of a 1# column, opening a serial valve at the bottom of the 1# column, opening a serial valve at the upper part of a 2# tree column, opening a discharging valve at the bottom of the 2# column, starting a wastewater pump when the two columns are in a serial state, adjusting the pH value of wastewater filtrate to 5-6, adjusting the temperature to be more than or equal to 30 ℃, removing alkaline impurities in the wastewater under a weak acid condition, facilitating a macroporous adsorption resin column to better adsorb the o-aminophenol in the wastewater filtrate in an acid environment, ensuring that the flow rate is 6 cubic/h, and allowing qualified wastewater after serial adsorption to enter a sewage discharging pool from the discharging valve at the bottom of the 2# resin column through a water outlet pipeline;
and S3 failure treatment: after the water outlet at the bottom of the No. 2 column is unqualified, closing a feed valve at the upper part of the No. 1 column, connecting the feed valves in series at the bottom, simultaneously closing a series valve at the upper part of the No. 2 column, simultaneously opening a feed valve at the upper part of the No. 2 column, closing a discharge valve at the bottom of the No. 2 column, opening a series valve at the bottom of the No. 2 column, connecting a series valve at the upper part of the No. 3 column, opening a discharge valve at the bottom of the No. 3 column, and connecting the No. 2 column and the No. 3 column in series;
s4 backflushing treatment: opening a positive backwashing valve at the upper part of the 1# column after the 1# column is out of service, simultaneously opening a circulating water valve at the bottom of the 1# column to perform backwashing on the resin, wherein the total water consumption is 5-6 cubic, the water temperature is 50-80 ℃, the flow rate is 12 cubic/h for about 10-30 minutes, and the effluent enters a raw water pool at the north side through a positive and negative washing pipeline at the upper part;
s5 analysis and regeneration process: opening an alkali inlet valve at the top of the No. 1 resin column, simultaneously opening a forward and reverse washing valve at the bottom of the No. 1 resin column, starting an alkali inlet pump, heating to 80 ℃ with 4 percent of total alkali consumption of 6 cubic meters (2BV) and flow rate of 3-4.5 cubic meters per hour (1-1.5BV), wherein the total time is more than 2 hours, feeding effluent into a northern raw water tank through a forward and reverse washing pipeline, and feeding the effluent into an analysis liquid collecting tank through an analysis liquid discharging valve at the bottom of the No. 1 resin column after the effluent is alkaline, namely when the PH is 10-12; (the water outlet condition is determined by measuring a PH test paper after discharging through a No. 1 resin column discharge valve, and the discharge valve is used for sampling or overhauling a discharged material);
s6 washing with water and alkali treatment: after hot alkali enters, closing an alkali inlet valve at the top of the 1# column, closing a forward backwashing valve at the bottom of the 1# resin column, opening a circulating water valve at the top of the 1# resin column, opening a desorption liquid discharge valve at the bottom of the 1# resin column, wherein the total water consumption for washing is about 6 cubic meters, the flow rate is 3 cubic meters/H, the first 1 hour and 3 cubic meters enter a 1# desorption liquid collecting tank through a desorption liquid pipeline, opening a feeding valve at the top of a dilute alkali tank, closing a feeding valve of the 1# desorption liquid collecting tank, and the later 1 hour and 3 cubic meters enter the dilute alkali tank through the desorption liquid pipeline;
s7 acid circulation treatment: opening an acid circulating valve at the bottom of the No. 1 resin column, opening an acid inlet valve at the top of the No. 1 resin column, pumping a certain amount of dilute hydrochloric acid into a dilute acid tank, starting a dilute acid pump, pumping into the resin column through a dilute acid pipeline, circulating for a certain time, ensuring that the PH in the resin column is about 3, and finishing the circulation.
Furthermore, the No. 1, the No. 2 and the No. 3 are separated independent resin columns, two resin columns are used in series every time, once the water quality at the back of the series is found to be unqualified, the former resin columns are immediately switched to be invalid, the other two resin columns are used in series, and the invalid resin columns are sequentially subjected to circulating water back flushing, hot alkali water analysis, analysis liquid collection and acid circulation treatment.
Specifically, the inlet water temperature of the wastewater filtrate is adjusted to be 30-80 ℃, and the temperature is more than or equal to 30 ℃, so that the o-aminophenol can be prevented from crystallizing and separating out to block the pipeline.
Specifically, the analytic liquid in the analytic liquid collecting tank can be directly returned to a production workshop for use, finished products do not need to be recovered, the cyclic mechanical treatment is adopted, the operation cost is greatly reduced, the recovery treatment equipment is simplified, and the economic benefit of an enterprise is improved.
Example 2:
the macroporous adsorption resin analysis treatment device is composed of two groups of macroporous adsorption resin components, each group of macroporous adsorption resin components comprises three macroporous adsorption resin columns, the three macroporous adsorption resin columns are connected in series by adopting two adsorption columns for adsorption, and the other adsorption column is used for analysis; specifically, the macroporous adsorption resin analysis treatment device is composed of 6 macroporous adsorption resin columns, wherein the four macroporous adsorption resin columns are 1200 × 3000mm in size and the two macroporous adsorption resin columns are 1600 × 3000mm in size, three 1200 × 3000 resin columns are one group of macroporous adsorption resin adsorption modules, the other 1200 × 3000 resin column and two 1600 × 3000 resin columns are the other group of macroporous adsorption resin adsorption modules, the 1200 × 3000 resin columns are planned to be filled with 3-square resin, the 1600 × 3000 resin columns are filled with 4-square resin, and the macroporous adsorption resin columns are all rubber-lined resin columns.
Example 3
The method for recovering and treating the o-aminophenol in the o-aminophenol acidification wastewater specifically comprises the following steps: firstly, after 15 cubic o-aminophenol content in workshop o-aminophenol sewage is settled by a settling tank and filtered by a filter tank, removing bottom sludge, floating oil stain and other impurities; secondly, adjusting the pH value of wastewater filtrate filtered by the filter tank to be 5-6, then feeding the wastewater filtrate into a No. 1 resin column through a wastewater pump through a feed valve, and simultaneously connecting the wastewater filtrate in series through a No. 2 resin column, wherein the No. 1 and No. 2 resin columns are all 1200 x 3000 rubber-lined resin columns, ADS600 polystyrene resin is filled in each resin column for 3 days, and the adsorption efficiency is about 6 days/hour; secondly, the resin column 1 which is out of work in the step 2 is washed by the circulating water, the waste water filtrate remained in the pore channel can be removed after about 30 minutes, and the water washing liquid is led into a raw water pool on the north side through a positive and negative washing pipeline on the top; and secondly, resolving the resin column treated by the S3 by using 6 cubic meters of 4% sodium hydroxide solution at 80 ℃ to obtain a resolving liquid, collecting the resolving liquid into a resolving liquid collecting tank, pumping the resolving liquid back to a workshop through a pump for recycling, wherein the content of o-aminophenol in the liquid of the resolving liquid collecting tank is 0.75%, and the resolving liquid contains about 45kg of pure o-aminophenol.
After three samples are taken and the recovery processing method is adopted, the COD index and the chroma index are respectively detected, and the specific data are as follows:
(Table 1)
From (table 1), the average removal rate of COD in the wastewater reaches 99.20%, and the removal rate of chroma is 99.17%;
from (Table 1), it is known that the average recovery rate per liter of the product in the wastewater is as high as 8.19 g.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. Recovery processing system of ortho-aminophenol in ortho-aminophenol acidizing waste water, its characterized in that: the method comprises the following steps:
an o-aminophenol acidification wastewater pool for wastewater storage and sedimentation;
the wastewater filtering tank is used for filtering the settled wastewater to obtain clear and transparent filtrate without floating oil substances;
the macroporous adsorption resin desorption treatment device is used for adsorbing o-aminophenol contained in the wastewater filtrate, and after adsorption saturation, desorption treatment is carried out in a hot alkali spraying mode to obtain desorption liquid;
the analysis liquid collecting tank is used for collecting the analysis liquid after the macroporous resin adsorption and analysis treatment;
the sewage discharge tank is used for discharging the treated wastewater after reaching the standard or recycling the wastewater, so that water resources are saved;
the waste water in the o-aminophenol acidification waste water pool enters a waste water filter tank for filtering after being settled, enters a macroporous adsorption resin analysis treatment device after being subjected to ph value adjustment, and the analysis liquid obtained after the adsorption, failure, water back flushing, alkali washing and acid circulation treatment in the macroporous adsorption resin analysis treatment device enters an analysis liquid collection tank, and the treated waste water reaching the qualified discharge standard enters a sewage discharge pool.
2. The system for recovering and treating o-aminophenol from an o-aminophenol-acidifying wastewater as set forth in claim 1, wherein: the macroporous adsorption resin analysis treatment device is a treatment process comprising at least one group of macroporous adsorption resin components, preferably two groups of macroporous adsorption resin components, wherein each group of macroporous adsorption resin components comprises three macroporous adsorption resin columns, the three macroporous adsorption resin columns are connected in series by adopting two adsorption columns for adsorption, and the other adsorption column is used for analysis.
3. The system for recovering and treating o-aminophenol from an o-aminophenol-acidifying wastewater as set forth in claim 2, wherein: the macroporous adsorption resin analysis treatment device is composed of 6 macroporous adsorption resin columns, wherein the four macroporous adsorption resin columns are 1200 mm by 3000mm in size and the two macroporous adsorption resin columns are 1600 mm by 3000mm in size, three 1200 mm by 3000 resin columns are a group of macroporous adsorption components, and the other 1200 mm by 3000 resin columns and two 1600 mm by 3000 resin columns are the other group of macroporous adsorption components.
4. The system for recovering and treating o-aminophenol from an o-aminophenol-acidifying wastewater as set forth in claim 3, wherein: the 1200 x 3000 size resin column plan to be filled with 3 square resin, 1600 x 3000 size resin column filled with 4 square resin.
5. The system for recovering and treating o-aminophenol from an o-aminophenol acidification wastewater as claimed in claim 2, 3 or 4, wherein: the macroporous adsorption resin columns are all rubber-lined resin columns.
6. The recovery processing method of the recovery processing system of the ortho-aminophenol in the ortho-aminophenol acidified wastewater according to claim 1, comprising the steps of:
s1 pretreatment: after the wastewater is settled and filtered (clear and transparent without floating oil substances), the pH value is adjusted to 5-6, the pH value is adjusted to be weak acid, alkaline impurities in the wastewater can be removed, and the macroporous adsorption resin column is favorable for better adsorbing o-aminophenol in a wastewater filtrate in an acidic environment;
s2 adsorption treatment: adjusting the water inlet temperature of the wastewater filtrate to be more than or equal to 30 ℃, preventing crystallization of o-aminophenol from separating out and blocking a pipeline, enabling the wastewater filtrate to enter a group of macroporous adsorption resin adsorption components through a wastewater pump and a feed pipeline, enabling the components to comprise No. 1, No. 2 and No. 3 resin columns, enabling the wastewater filtrate to enter the resin columns in series connection with No. 1 and No. 2 for adsorption, and directly discharging the adsorbed wastewater filtrate into a sewage discharge pool when the effluent at the bottom of No. 2 is qualified;
and S3 failure treatment: when the water outlet at the bottom of the No. 2 resin column is unqualified, the No. 1 resin column connected in series with the No. 2 resin column is failed, the wastewater filtrate is stopped from entering the No. 1 resin column, the serial connection state of the No. 1 and the No. 2 is disconnected, the serial connection of the No. 2 and the No. 3 is started, and the wastewater filtrate enters the No. 2 and the No. 3 resin column connected in series through a wastewater pump and a feed pipeline for adsorption;
s4 backflushing treatment: carrying out positive and negative water flushing on the failed 1# resin column through a circulating water pump and a circulating water pipeline so as to remove residual wastewater filtrate in a 1# resin pore passage, and discharging outlet water into a raw water pool through the positive and negative flushing pipeline;
s5 analysis and regeneration process: introducing hot alkali liquor in a dilute alkali tank heated to 80 ℃ into a 1# resin column subjected to back flushing treatment through an alkali inlet pump and an alkali inlet pipeline, and sending the desorption liquor into a desorption liquor collecting tank through a desorption liquor pipeline at the bottom of the 1# resin column when outlet water at the bottom of the 1# resin column is alkaline;
s6 washing with water and alkali treatment: after the hot alkali liquor in the step S5 is completely fed, stopping feeding the hot alkali liquor into the No. 1 resin column, simultaneously opening a circulating water pipeline of the No. 1 resin column for water washing, wherein one part of the washing alkali liquor enters a resolving liquid collecting tank through a resolving liquid pipeline, and the other part of the washing alkali liquor enters a dilute alkali tank through the resolving liquid pipeline for recycling;
s7 acid circulation treatment: and (3) pumping a certain amount of dilute hydrochloric acid into the No. 1 resin column treated by the S6 through a dilute acid pump and a dilute acid pipeline, circulating for a certain time, and ending the circulation when the PH value in the resin column is about 3.
7. The method for recovering and treating o-aminophenol from an o-aminophenol acidified wastewater according to claim 6, characterized in that: and the water inlet temperature of the wastewater filtrate is adjusted to be 30-80 ℃ in S2.
8. The method for recovering and treating o-aminophenol from an o-aminophenol acidified wastewater according to claim 6, characterized in that: 1#, 2# and 3# are separated independent resin columns, two resin columns are used in series every time, once the water quality at the back of the series is found to be unqualified, the former resin columns are switched to fail, the other two resin columns are used in series, and the failed resin columns are subjected to circulating water back flushing, hot-alkali water analysis, analysis liquid collection and acid circulation treatment in sequence.
9. The method for recovering and treating the ortho-aminophenol in the ortho-aminophenol acidified wastewater according to claim 6, wherein the desorption solution in the desorption solution collection tank in S5 can be directly returned to a production workshop for use, i.e., recycling treatment.
10. The method for recovering and treating o-aminophenol from an o-aminophenol acidified wastewater according to claim 6, wherein said effluent is alkaline at a pH of 10 to 12 in S5, specifically, the effluent is measured by a pH test paper by sampling from the bottom of a No. 1 resin column.
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