CN114890594A - Treatment process and system for high-salt-content refractory organic wastewater capable of recycling resources - Google Patents
Treatment process and system for high-salt-content refractory organic wastewater capable of recycling resources Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 38
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- 238000004064 recycling Methods 0.000 title description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 49
- 230000003647 oxidation Effects 0.000 claims abstract description 48
- 239000000706 filtrate Substances 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005917 acylation reaction Methods 0.000 claims abstract description 24
- 239000012065 filter cake Substances 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 230000010933 acylation Effects 0.000 claims abstract description 17
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 12
- -1 aluminum ions Chemical class 0.000 claims abstract description 12
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
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- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 3
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- 238000003756 stirring Methods 0.000 claims description 18
- 238000004062 sedimentation Methods 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 230000015556 catabolic process Effects 0.000 claims description 12
- 238000006731 degradation reaction Methods 0.000 claims description 12
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- 229910052719 titanium Inorganic materials 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- DPGAAOUOSQHIJH-UHFFFAOYSA-N ruthenium titanium Chemical compound [Ti].[Ru] DPGAAOUOSQHIJH-UHFFFAOYSA-N 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 229910003460 diamond Inorganic materials 0.000 claims description 6
- 239000010432 diamond Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical group [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000010815 organic waste Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 8
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
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- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 26
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 9
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- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
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- 125000002252 acyl group Chemical group 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
- C01F7/57—Basic aluminium chlorides, e.g. polyaluminium chlorides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a treatment process and a system for high-salt-content refractory organic wastewater capable of resource recovery, wherein the process comprises the following steps: (1) adjusting the pH value of the acylation wastewater to be alkaline to obtain a suspension containing aluminum hydroxide precipitate, and filtering the suspension to obtain an aluminum hydroxide filter cake and a filtrate; (2) performing electrocatalytic oxidation treatment on the filtrate, and discharging the filtrate after reaching the standard; (3) and adding concentrated hydrochloric acid into the filter cake, heating and dissolving, adding an auxiliary agent, and polymerizing to obtain the polyaluminum chloride. The treatment process of the resource-recyclable high-salt-content refractory organic wastewater takes electrocatalytic oxidation treatment as a core, quickly removes organic pollutants in the wastewater, extracts aluminum ions to produce water treatment medicament polyaluminium chloride, realizes the purpose of changing waste into valuable, and has important application value.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a treatment process and a treatment system for high-salt-content degradation-resistant organic wastewater capable of recycling resources.
Background
Friedel-Crafts acylation is an organic reaction of great importance in the industrial production of fine chemicals, specialty chemicals and pharmaceutical intermediates (proceedings of the university of Changzhou (Nature science edition), 2010,22(02): 28-30.). Mainly means that acyl halide reacts with aromatic compound under the catalysis of Lewis acid (such as aluminum trichloride), so as to introduce acyl on aromatic ring.
Although Friedel-Crafts acylation reaction is an important organic reaction, the industrial application of Friedel-Crafts acylation reaction still has great limitation, mainly because the acylation reaction can generate a large amount of industrial wastewater with high salt content and high toxicity. Mainly because the solvent used in the acylation reaction (1) is mainly nitrobenzene, a large amount of nitrobenzene still exists in the acylation reaction wastewater, and the nitrobenzene has strong toxicity and is an important carcinogenic substance; (2) aluminum trichloride is the most commonly used catalyst for catalytic acylation reaction, has the advantages of high catalytic activity and mild reaction conditions, but most of the aluminum trichloride enters wastewater after the reaction and has higher concentration in the wastewater; (3) small amounts of acylating agents, benzene series and acylated products may also be present in the wastewater. Therefore, the waste water after the acylation reaction is mainly high-toxicity and high-salt-content organic waste water which is difficult to biodegrade (Table 1), and is extremely difficult to treat. Under the current increasingly strict environmental regulations, the difficultly biodegradable organic wastewater generated by the acylation reaction is the main symptom limiting the industrialization of the Friedel-Crafts acylation reaction.
TABLE 1 quality of acylated wastewater
The electrochemical oxidation method is an effective method for treating high-salinity high-toxicity nonbiodegradable organic wastewater, and the working principle of the electrochemical oxidation method is divided into two types, namely a direct oxidation mechanism and an indirect oxidation mechanism. The direct oxidation mechanism is that organic matters are oxidized and degraded on the surface of the anode, and the indirect oxidation is that oxidation reaction is carried out on the surface of the anode and the filling particles in the oxidation process to generate a plurality of intermediate products, such as ozone and HO 2 ]、[O]And the intermediates have certain mineralization effect on organic matters, and can convert the macromolecular organic matters which are difficult to degrade into micromolecular organic matters, carbon dioxide and water.
Therefore, it is necessary to research a method for realizing standard discharge of wastewater and recycling of aluminum ions and the like aiming at the non-biodegradable organic wastewater generated by the acylation reaction.
Disclosure of Invention
In view of the above, the first objective of the present invention is to provide a treatment process for high-salt-content refractory organic wastewater capable of resource recovery, which takes electrocatalytic oxidation treatment as a core, rapidly removes organic pollutants in the wastewater, extracts aluminum ions to produce water treatment agent polyaluminium chloride, achieves the purpose of turning waste into wealth, and has important application value.
The second purpose of the invention is to provide a treatment system of high-salt-content degradation-resistant organic wastewater capable of resource recovery.
In order to achieve the purpose, a first aspect embodiment of the invention provides a treatment process of resource-recoverable high-salt-content degradation-resistant organic wastewater, which is characterized by comprising the following steps:
(1) adjusting the pH value of the acylation wastewater to be alkaline to obtain a suspension containing aluminum hydroxide precipitate, and filtering the suspension to obtain an aluminum hydroxide filter cake and a filtrate;
(2) performing electrocatalytic oxidation treatment on the filtrate, and discharging the filtrate after reaching the standard;
(3) and adding concentrated hydrochloric acid into the filter cake, heating and dissolving, adding an auxiliary agent, and polymerizing to obtain the polyaluminum chloride.
The treatment process of the resource-recyclable high-salt-content refractory organic wastewater disclosed by the embodiment of the invention takes electrocatalytic oxidation treatment as a core, organic pollutants in the wastewater are quickly removed, aluminum ions are extracted to produce the water treatment agent polyaluminium chloride, the purpose of changing waste into valuable is realized, and the treatment process has an important application value.
In some embodiments of the present invention, in the step (1), the adjusting the pH of the acylated wastewater to alkaline comprises: adjusting the pH value of the acylation wastewater to 8-10 by adopting an alkali raw material, wherein the alkali raw material is one or more than two of sodium hydroxide, potassium hydroxide or liquid ammonia.
In some embodiments of the invention, in step (2), the operating conditions of the electrocatalytic oxidation treatment are: the current density is 10-500mA/cm 2 The pH value is 3-10, the electrolysis temperature is 15-60 ℃, and the electrolysis time is 3-8 h.
In some embodiments of the invention, in step (2), the electrocatalytic oxidation treatment is performed in an electrocatalytic oxidation device.
In some embodiments of the invention, the electrocatalytic oxidation apparatus comprises an electrochemical reactor and a regulated dc power supply; the electrochemical reactor comprises a water bath and an electrolytic bath; the electrolytic bath is arranged in the water bath kettle, and an anode and a cathode are arranged in the electrolytic bath; the anode is connected with the anode of the direct current stabilized power supply, and the cathode is connected with the cathode of the direct current stabilized power supply.
In some embodiments of the invention, the anode is one of a boron doped diamond film electrode, a ruthenium titanium electrode, a titanium suboxide electrode; the cathode is one of a stainless steel electrode, a titanium electrode and a ruthenium-titanium electrode.
In some embodiments of the invention, the electrocatalytic oxidation apparatus further comprises a stirring unit; the stirring unit is arranged in the electrolytic bath and is a magneton, and the water bath is a magnetic stirring water bath.
In some embodiments of the invention, in step (3), the temperature for heating and dissolving is 40-50 ℃, and the weight ratio of the filter cake to the concentrated hydrochloric acid is 0.5-2.5: 1; in the step (3), the addition amount of the auxiliary agent is 2-10 wt% of the dry weight of the filter cake, and the auxiliary agent is calcium aluminate or/and magnesium aluminate.
In order to achieve the above object, a treatment system for refractory organic wastewater with high salt content capable of resource recovery comprises:
the sedimentation tank is used for generating aluminum hydroxide sediment;
the inlet of the filtering unit is communicated with the outlet of the sedimentation tank;
the inlet of the electrocatalytic oxidation device is communicated with the filtrate outlet of the filtering unit, and the outlet of the electrocatalytic oxidation device is communicated with a wastewater standard discharge pipeline;
the outlet of the dissolving tank is communicated with the filter cake outlet of the filtering unit, and the dissolving tank is provided with a concentrated hydrochloric acid inlet;
and the inlet of the reaction kettle is communicated with the outlet of the dissolving tank.
The treatment system for the high-salt-content refractory organic wastewater capable of being recycled in the embodiment of the invention has the same beneficial effects as the treatment process for the high-salt-content refractory organic wastewater capable of being recycled in the embodiment of the invention, and the details are not repeated herein.
In some embodiments of the invention, the electrocatalytic oxidation apparatus comprises an electrochemical reactor and a regulated dc power supply; the electrochemical reactor comprises a water bath and an electrolytic bath; the electrolytic bath is arranged in the water bath kettle, and an anode and a cathode are arranged in the electrolytic bath; the anode is connected with the anode of the direct current stabilized power supply, and the cathode is connected with the cathode of the direct current stabilized power supply; the anode is one of a boron-doped diamond film electrode, a ruthenium-titanium electrode and a titanium suboxide electrode; the cathode is one of a stainless steel electrode, a titanium electrode and a ruthenium-titanium electrode.
In some embodiments of the invention, the electrocatalytic oxidation apparatus further comprises a stirring unit; the stirring unit is arranged in the electrolytic bath, the stirring unit is a magneton, and the water bath is a magnetic stirring water bath; the filtering unit is a plate-and-frame filter press.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a flow chart of a treatment process of a high-salinity refractory organic wastewater capable of resource recovery according to an embodiment of the invention (i.e. a simple structure diagram of a treatment system of the high-salinity refractory organic wastewater capable of resource recovery).
FIG. 2 is a schematic diagram of a simplified structure of an electrocatalytic oxidation apparatus according to an embodiment of the present invention.
FIG. 3 is a diagram showing the change of COD in the electrocatalytic oxidation treatment process of treating the acylation wastewater by the treatment process of the resource-recoverable high-salt-content degradation-resistant organic wastewater in the embodiment 1 of the invention.
FIG. 4 is a diagram showing the change of COD in the electrocatalytic oxidation treatment process of treating the acylation wastewater by the treatment process of the resource-recoverable high-salt-content degradation-resistant organic wastewater in example 2 of the invention.
FIG. 5 is a diagram showing the change of COD in the electrocatalytic oxidation treatment process of treating the acylation wastewater by the treatment process of the resource-recoverable high-salt-content degradation-resistant organic wastewater in example 3 of the invention.
Reference numerals:
1-a regulating reservoir; 2-a sedimentation tank; 3-a filtration unit; 4-electrocatalytic oxidation device; 401-water bath; 402-an electrolytic cell; 403-an anode; 404-a cathode; 405-a stirring unit; 407-hot water bath; 406-regulated dc power supply; 5-a dissolving tank; 6-a reaction kettle.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
The treatment process of the resource-recoverable high-salt-content refractory organic wastewater and the treatment system of the resource-recoverable high-salt-content refractory organic wastewater according to the embodiment of the invention are described below with reference to the accompanying drawings.
Fig. 1 is a flow chart of a treatment process of resource-recoverable high-salt-content refractory organic wastewater (i.e. a simple structure schematic diagram of a treatment system of resource-recoverable high-salt-content refractory organic wastewater) according to an embodiment of the invention.
As shown in FIG. 1, the system for treating and recycling the acylation waste water by the extraction method of the embodiment of the invention comprises a sedimentation tank 2, a filtering unit 3, an electrocatalytic oxidation device 4, a dissolving tank 5 and a reaction kettle 6; the sedimentation tank 2 is used for generating aluminum hydroxide sediment; the inlet of the filtering unit 3 is communicated with the outlet of the sedimentation tank; an inlet of the electrocatalytic oxidation device 4 is communicated with a filtrate outlet of the filtering unit 3, and an outlet of the electrocatalytic oxidation device 4 is communicated with a wastewater discharge pipeline reaching the standard; an outlet of the dissolving tank 5 is communicated with a filter cake outlet of the filtering unit 3, and the dissolving tank 5 is provided with a concentrated hydrochloric acid inlet; the inlet of the reaction kettle 6 is communicated with the outlet of the dissolving tank.
Optionally, as shown in fig. 2, the electrocatalytic oxidation apparatus includes an electrochemical reactor and a dc regulated power supply 406; the electrochemical reactor comprises a water bath 401 and an electrolytic bath 402; the electrolytic bath 402 is arranged in the water bath 401, and an anode 403 and a cathode 404 are arranged in the electrolytic bath 402; the anode 403 is connected with the positive pole of the DC stabilized power supply 406, and the cathode 404 is connected with the negative pole of the DC stabilized power supply 406; the anode 403 is one of a boron-doped diamond film electrode, a ruthenium-titanium electrode and a titanium suboxide electrode; the cathode 404 is one of a stainless steel electrode, a titanium electrode, and a ruthenium-titanium electrode.
Optionally, in order to increase the heating area of the electrolytic cell and improve the heating efficiency of the electrolytic cell, the periphery and the bottom of the electrolytic cell are preferably located in the water bath of the water bath, which requires that the periphery and the bottom of the electrolytic cell are spaced from the periphery and the bottom of the water bath, so that the whole electrolytic cell can be fixedly installed in the water bath through a bracket, a first bolt and the like. Optionally, in some embodiments, a thermocouple for measuring the temperature of the water bath in the water bath may be mounted on the water bath.
Optionally, the anode 403 and the cathode 404 may be fixedly installed in the electrolytic cell 402 by a support frame and a second bolt, and in order to ensure the electrocatalytic oxidation effect, a distance is left between the anode and the cathode, and the anode and the cathode are both spaced from the peripheral wall and the bottom of the electrolytic cell.
Optionally, in order to improve the efficiency of the electrocatalytic oxidation, in some embodiments, the electrocatalytic oxidation apparatus further includes a stirring unit 405, the stirring unit 405 is disposed in the electrolytic cell 402, and the stirring unit may be a magneton, a pitched blade stirrer, an anchor stirrer, or the like, preferably a magneton. When the stirring unit selects an inclined paddle type stirrer, an anchor type stirrer and the like, the stirring unit can be fixedly arranged in the electrolytic bath through a mounting frame, a third bolt and the like; when the stirring unit adopts a magneton, the water bath kettle adopts a magnetic stirring water bath kettle, and the electrolytic cell can be directly placed in the water bath kettle.
Optionally, the anode 403 is connected to the anode of the dc regulated power supply 406 through a first cable, the cathode is connected to the cathode of the dc regulated power supply through a second cable, a voltmeter is installed between the first cable and the second cable for measuring the voltage of the electrocatalytic oxidation, and an ammeter is installed on the second cable for measuring the current of the electrocatalytic oxidation.
It should be noted that, in the treatment system for high-salt-content refractory organic wastewater capable of resource recovery according to the embodiment of the present invention, the communication mode between the components can be realized by pipeline communication or transportation by a transport vehicle, etc. according to the properties of the materials, and if the pipeline communication is used, valves and pumps can be installed on the corresponding pipelines as required, which are conventional technologies and do not belong to the key point of the present invention.
Optionally, in order to adjust the water amount, balance the water quality, and pre-treat the acylated wastewater, the treatment system for high-salt-content refractory organic wastewater capable of resource recovery according to the embodiment of the invention further comprises an adjusting tank 1 arranged in front of the sedimentation tank 2. The method comprises the steps of firstly adjusting the water quality and the water quantity of the acylation wastewater in an adjusting tank, pretreating the acylation wastewater, and then feeding the acylation wastewater into a sedimentation tank.
Alternatively, the reaction vessel 6 may be a stainless steel reaction vessel or the like. The sedimentation tank 2 can adopt a horizontal flow sedimentation tank or a vertical flow sedimentation tank, etc., the filtering unit 3 can adopt a plate-and-frame filter press, and the dissolving tank 5 can adopt a conventional dissolving tank.
The working principle of the treatment system for the high-salt-content refractory organic wastewater capable of recycling resources provided by the embodiment of the invention is as follows:
when in use, the acylation wastewater firstly enters the regulating tank 1 to regulate the water quantity, balance the water quality and carry out pretreatment, and then enters the sedimentation tank 2; adjusting the pH of the acylation wastewater entering the sedimentation tank 2 to be alkaline (the pH is about 9) by an alkali source, precipitating aluminum ions in the acylation wastewater into aluminum hydroxide, filtering suspension containing the aluminum hydroxide precipitate in a filtering unit 3, wherein the filtrate enters an electrolytic tank 402 of an electrocatalytic oxidation device 4, simultaneously heating the electrolytic tank 402 by a hot water bath 407 in a water bath kettle, and controlling the current density to be 10-500mA/cm 2 Adjusting the pH value of the filtrate in the electrolytic bath 402 to be between 3 and 10, and the temperature of the filtrate in the electrolytic bath 402 to be between 15 and 60 ℃, electrolyzing the filtrate for 3 to 8 hours, and removing nitrobenzene to ensure that the COD of the final effluent is less than 50mg/L, thereby realizing the standard discharge of the wastewater. And the aluminum hydroxide filter cake discharged from the filtering unit 3 enters a dissolving tank 7, is heated and dissolved under the action of concentrated hydrochloric acid in the dissolving tank 7, then enters a reaction kettle 6, and is polymerized with an auxiliary agent added into the reaction kettle 8 to obtain the water treatment agent polyaluminum chloride, wherein the quality of the obtained polyaluminum chloride meets the national standard of polyaluminum chloride GB/T22627-2014 water treatment agent-polyaluminum chloride.
It should be noted that, the treatment process of the resource-recoverable high-salinity degradation-resistant organic wastewater according to the embodiment of the present invention can be implemented by the treatment system of the resource-recoverable high-salinity degradation-resistant organic wastewater according to the embodiment of the present invention to treat the acylated wastewater and return the resource of the acylated wastewater, but the system device for implementing the treatment process is not limited to the treatment system of the resource-recoverable high-salinity degradation-resistant organic wastewater according to the embodiment of the present invention.
The treatment process of the resource-recoverable high-salt-content refractory organic wastewater provided by the embodiment of the invention is described below by combining specific examples.
Raw material reagents and equipment involved in the examples of the present invention are commercially available reagents and equipment unless otherwise specified; the detection methods and the like involved in the embodiments of the present invention are all conventional methods unless otherwise specified.
The following examples of the present invention were conducted under laboratory conditions, and the suction filtration was performed using a laboratory suction filtration apparatus composed of a buchner funnel, a suction flask, a hose, a suction pump, and filter paper. The stirring units in the electrocatalytic oxidation device all adopt magnetic stirrers.
Example 1
1L of acylation wastewater (COD 6200mg/L, nitrobenzene: 3000mg/L, chloride ion: 3000mg/L, aluminum ion: 3000mg/L) is taken into a beaker, 20g of sodium hydroxide is added, the pH is adjusted to 9.5, and a filter cake and a filtrate are obtained after suction filtration. Transferring the filtrate into an electrolytic bath of an electrocatalytic oxidation device shown in FIG. 2, adjusting pH to 5.0, and electrolyzing, wherein the anode is a diamond film electrode, the cathode is a stainless steel electrode, and the surface areas of the anode and the cathode are both 40cm 2 The current density is 50mA/cm 2 When the electrolysis temperature is 40 ℃, the electrolysis time is 6 hours, the COD of the filtrate in the electrolytic cell is reduced to 50mg/L (as shown in figure 3), the nitrobenzene concentration is 0.5mg/L, and the discharge standard GB8978-1996 integrated wastewater discharge standard (COD)<100mg/L of nitrobenzene<1.0 mg/L). 10000mg of filter cake is added into a dissolving tank containing 5000mL of concentrated hydrochloric acid to be dissolved at 40 ℃, and then the filter cake reacts with 400mg of calcium aluminate at 70 ℃ and 0.5MPa to obtain the polyaluminium chloride product. The detection shows that the main indexes of the obtained product polyaluminium chloride are as follows: the aluminum chloride has the mass fraction of 31 percent, the basicity of 45 percent, the mass fraction of water-insoluble substances of 0.2, the pH value of 5.5 and the iron mass fraction of 1.0 percent, arsenic, lead, chromium, mercury and cadmium are not detected, and all indexes meet the requirements of the national standard GB/T22627-2014 water treatment agent-polyaluminium chloride.
Example 2
1L of the acylated wastewater (COD 7100mg/L, nitrobenzene 3600mg/L, chloride ion 3100mg/L, aluminum ion 3200mg/L) was placed in a beaker, 30g of potassium hydroxide was added, and the pH was adjusted to a value of 3200mg/L9.3, obtaining a filter cake and filtrate after suction filtration. Transferring the filtrate into an electrolytic cell of an electrocatalytic oxidation device shown in FIG. 2, adjusting pH to 4.0, and electrolyzing with an anode of ruthenium-titanium electrode and a cathode of titanium electrode, wherein the surface areas of the anode and the cathode are both 40cm 2 The current density is 70mA/cm 2 When the electrolysis temperature is 35 ℃, after 6 hours of electrolysis, the COD of the filtrate in the electrolytic cell is reduced to 55mg/L (as shown in figure 4), the concentration of nitrobenzene is 0.6mg/L, and the discharge standard GB8978-1996 integrated wastewater discharge standard (COD)<100mg/L of nitrobenzene<1.0 mg/L). 12000mg of filter cake is added into a dissolving tank containing 8000mL of concentrated hydrochloric acid to be dissolved at 45 ℃, and then the filter cake reacts with 600mg of magnesium aluminate at 80 ℃ and 0.6MPa to obtain the polyaluminium chloride product. The detection shows that the main indexes of the obtained product polyaluminium chloride are as follows: the aluminum chloride accounts for 32 percent by mass, the basicity is 65 percent, the mass fraction of water-insoluble substances is 0.2, the pH value is 4.5, the mass fraction of iron is 1.0 percent, arsenic, lead, chromium, mercury and cadmium are not detected, and all indexes meet the requirements of the national standard GB/T22627-2014 water treatment agent-polyaluminium chloride.
Example 3
1L of the acylation wastewater (COD 7100mg/L, nitrobenzene 3600mg/L, chloride ion 3100mg/L, aluminum ion 3200mg/L) is put into a beaker, 23g of sodium hydroxide is added, the pH is adjusted to 9.3, and a filter cake and a filtrate are obtained after suction filtration. Transferring the filtrate into an electrolytic cell of an electrocatalytic oxidation device shown in FIG. 2, adjusting pH to 8.0, and electrolyzing, wherein the anode is titanium suboxide electrode, the cathode is stainless steel electrode, and the surface areas of the anode and the cathode are both 40cm 2 The current density is 50mA/cm 2 When the electrolysis temperature is 50 ℃, the electrolysis time is 6 hours, the COD of the filtrate in the electrolytic cell is reduced to 65mg/L (as shown in figure 5), the nitrobenzene is 0.4mg/L, and the discharge standard GB8978-1996 integrated wastewater discharge standard (COD)<100mg/L of nitrobenzene<1.0 mg/L). 12000mg of filter cake is added into a dissolving tank containing 8000mL of concentrated hydrochloric acid to be dissolved at 50 ℃, and then the filter cake reacts with 500mg of magnesium aluminate at 70 ℃ and 0.5MPa to obtain the polyaluminium chloride product. The detection shows that the main indexes of the obtained product polyaluminium chloride are as follows: the mass fraction of the aluminum chloride is 32 percent, the basicity is 47 percent, the mass fraction of the water-insoluble substances is 0.2,the pH value is 6.5, the mass fraction of iron is 1.0%, arsenic, lead, chromium, mercury and cadmium are not detected, and all indexes meet the requirements of the national standard GB/T22627-2014 water treatment agent-polyaluminium chloride.
Example 4
This example is substantially the same as example 1 except that the electrolysis time was 3 hours and the current density was 250mA/cm 2 。
Example 5
This example is substantially the same as example 1, except that the electrolysis time was 8 hours and the current density was 500mA/cm 2 。
In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A treatment process of resource-recoverable high-salt-content refractory organic wastewater is characterized by comprising the following steps:
(1) adjusting the pH value of the acylation wastewater to be alkaline to obtain a suspension containing aluminum hydroxide precipitate, and filtering the suspension to obtain an aluminum hydroxide filter cake and a filtrate;
(2) performing electrocatalytic oxidation treatment on the filtrate, and discharging the filtrate after reaching the standard;
(3) and adding concentrated hydrochloric acid into the filter cake, heating and dissolving, adding an auxiliary agent, and polymerizing to obtain the polyaluminum chloride.
2. The process for treating resource-recoverable high-salinity degradation-resistant organic wastewater according to claim 1, wherein the step (1) of adjusting the pH of the acylated wastewater to alkaline comprises the following steps: adjusting the pH value of the acylation waste water to 8-10 by adopting an alkali raw material, wherein the alkali raw material is one or more than two of sodium hydroxide, potassium hydroxide or liquid ammonia.
3. The process for treating refractory organic waste water with high salinity according to claim 1, wherein in the step (2), the process comprisesThe working conditions of the electrocatalytic oxidation treatment are as follows: the current density is 10-500mA/cm 2 The pH value is 3-10, the electrolysis temperature is 15-60 ℃, and the electrolysis time is 3-8 h.
4. The process for treating resource-recoverable high-salinity refractory organic wastewater according to claim 1, wherein in the step (2), the electrocatalytic oxidation treatment is carried out in an electrocatalytic oxidation device.
5. The process for treating resource-recoverable high-salinity degradation-resistant organic wastewater according to claim 4, wherein the electrocatalytic oxidation device comprises an electrochemical reactor and a direct-current stabilized power supply; the electrochemical reactor comprises a water bath and an electrolytic bath; the electrolytic bath is arranged in the water bath, and an anode and a cathode are arranged in the electrolytic bath; the anode is connected with the anode of the direct current stabilized power supply, and the cathode is connected with the cathode of the direct current stabilized power supply.
6. The treatment process of the resource-recyclable high-salt-content degradation-resistant organic wastewater as claimed in claim 5, wherein the anode is one of a boron-doped diamond film electrode, a ruthenium titanium electrode and a titanium suboxide electrode; the cathode is one of a stainless steel electrode, a titanium electrode and a ruthenium-titanium electrode.
7. The process for treating resource-recoverable high-salinity refractory organic wastewater according to claim 5 or 6, wherein the electrocatalytic oxidation device further comprises a stirring unit; the stirring unit is arranged in the electrolytic bath and is a magneton, and the water bath is a magnetic stirring water bath.
8. The process for treating resource-recoverable high-salt-content refractory organic wastewater according to claim 1, wherein in the step (3), the heating and dissolving temperature is 40-50 ℃, and the weight ratio of the filter cake to the concentrated hydrochloric acid is 0.5-2.5: 1; in the step (3), the addition amount of the auxiliary agent is 2-10 wt% of the dry weight of the filter cake, and the auxiliary agent is calcium aluminate or/and magnesium aluminate.
9. A treatment system for resource-recoverable high-salt-content refractory organic wastewater is characterized by comprising:
the sedimentation tank is used for generating aluminum hydroxide sediment;
the inlet of the filtering unit is communicated with the outlet of the sedimentation tank;
the inlet of the electrocatalytic oxidation device is communicated with the filtrate outlet of the filtering unit, and the outlet of the electrocatalytic oxidation device is communicated with a wastewater standard discharge pipeline;
the outlet of the dissolving tank is communicated with the filter cake outlet of the filtering unit, and the dissolving tank is provided with a concentrated hydrochloric acid inlet;
and the inlet of the reaction kettle is communicated with the outlet of the dissolving tank.
10. The system for treating high-salinity refractory organic wastewater capable of being recycled according to claim 9, wherein the electrocatalytic oxidation device comprises an electrochemical reactor and a direct-current stabilized power supply; the electrochemical reactor comprises a water bath and an electrolytic bath; the electrolytic bath is arranged in the water bath kettle, and an anode and a cathode are arranged in the electrolytic bath; the anode is connected with the anode of the direct current stabilized power supply, and the cathode is connected with the cathode of the direct current stabilized power supply; the anode is one of a boron-doped diamond film electrode, a ruthenium-titanium electrode and a titanium suboxide electrode; the cathode is one of a stainless steel electrode, a titanium electrode and a ruthenium-titanium electrode;
preferably, the electrocatalytic oxidation device further comprises a stirring unit; the stirring unit is arranged in the electrolytic bath, the stirring unit is a magneton, and the water bath is a magnetic stirring water bath; the filtering unit is a plate-and-frame filter press.
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