CN115159750A - Efficient coking desulfurization waste liquid decoloring method - Google Patents
Efficient coking desulfurization waste liquid decoloring method Download PDFInfo
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- CN115159750A CN115159750A CN202210853218.6A CN202210853218A CN115159750A CN 115159750 A CN115159750 A CN 115159750A CN 202210853218 A CN202210853218 A CN 202210853218A CN 115159750 A CN115159750 A CN 115159750A
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- 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
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
Abstract
A high-efficiency decoloring method for coking desulfurization waste liquid comprises the following three stages of 1) low-temperature plasma oxidative decomposition; 2) Carrying out oxidative decomposition on the persulfate activated by the transition metal ions; 3) Activated carbon activates persulfate for oxidative decomposition and adsorption. Compared with the prior art, the invention has the beneficial effects that: macromolecular organic colored substances which are difficult to treat in the desulfurization waste liquid are oxidized and decomposed into easily-treated micromolecules or colorless micromolecules; the efficient chemical oxidation decoloration and the traditional physical adsorption decoloration are effectively combined, so that the decoloration effect of the desulfurization waste liquid is more efficient and thorough, the using amount of the active carbon is reduced, and the decoloration cost is reduced; other impurities are not introduced in the whole process, so that the subsequent extraction of high-quality salt products is facilitated.
Description
Technical Field
The invention belongs to the field of coal chemical wastewater treatment and resource recycling; in particular to a high-efficiency decoloring method for coking desulfurization waste liquid.
Background
The coking desulfurization waste liquid contains a large amount of thiocyanate, thiosulfate, sulfate and other secondary salts, and the secondary salts are extracted by adopting a decoloring-evaporative concentration-crystallization process commonly in the current coking industry, so that the resource utilization of the coking desulfurization waste liquid is realized. However, the desulfurization catalyst (PDS, HPF, etc.) and the organic matter in the desulfurization waste liquid contain ethylenic bonds, carboxyl groups, amide groups, sulfonamide groups, nitro groups, chromophoric groups such as metal impurity ions, and-NH 2 、—NHR、—NR 2 And the interaction of the chromophoric groups such as-OR, -OH and-SH ensures that the chromaticity of the desulfurization waste liquid is extremely high, and the surface color of the desulfurization waste liquid is generally close to black, thereby greatly influencing the quality of salt products and restricting the sale market of the salt products. Therefore, the decolorization is an important prerequisite for ensuring the extraction of high-quality salt products, so that the desulfurization waste liquid must be subjected to decolorization treatment in the salt extraction process.
At present, the coking industry mainly adopts an activated carbon adsorption method to decolor the desulfurized waste liquid, but the decoloration efficiency of the activated carbon is very low under the condition of low consumption, and the running cost of the desulfurized waste liquid salt extraction process is obviously increased. Meanwhile, a decolouring assistant is required to be added in the using process of some activated carbon. The application number 200910081755.8 Chinese patent document provides a desulfurization waste liquid decolorization auxiliary agent which comprises 18-30 parts of chelating agent, 18-30 parts of precipitator, 3-6 parts of defoaming agent and 2-4 parts of phosphonate, the composition is complex, a large amount of impurity groups are necessarily brought in the use process, for example, water-soluble phosphonate can be remained in thiocyanate when the thiocyanate is crystallized to influence the purity of the thiocyanate product. The application number 201310362603.1 Chinese patent document provides a supported decoloring agent prepared by an impregnation method, the preparation process of the decoloring agent is complicated, and impurities and metal ions in carriers (diatomite, white carbon black, montmorillonite and the like) and active components (calcium chloride, zinc acetate, magnesium sulfate, ferric chloride, aluminum chloride and the like) of the decoloring agent can enter desulfurization waste liquid, so that the components of the desulfurization waste liquid are more complex, and high-quality salt products are more difficult to extract. Therefore, the technology for optimizing the existing activated carbon decoloration and decolorant and decoloration auxiliary agent in the field of coking desulfurization waste liquid is needed.
In addition, various advanced oxidation techniques (AOPs) based on free radical oxidation, such as catalytic wet oxidation, photocatalytic oxidation, UV/H 2 O 2 、UV/O 3 The technologies are more and more concerned by technical workers in the field of wastewater treatment; particularly, the low-temperature plasma technology, as a new AOPs, not only has the commonalities of high-activity free radical oxidation and the like, but also has the characteristics of ultraviolet radiation, high-temperature pyrolysis, liquid electric cavitation and the like which are beneficial to the degradation of organic matters, but the report of AOPs decoloration is not seen in the field of coking desulfurization waste liquid.
Disclosure of Invention
The invention provides a high-efficiency decoloring method for coking desulfurization waste liquid, and aims to improve or optimize a decoloring technology in a salt extraction process of the coking desulfurization waste liquid.
In order to realize the purpose, the invention adopts the following technical scheme:
a high-efficiency decoloring method for coking desulfurization waste liquid comprises the following three stages:
1) Low-temperature plasma oxidative decomposition: high-activity low-temperature plasma (OH, H) generated by pulse corona discharge 2 O 2 、 O 3 Etc.), the low-temperature plasma collides and reacts with the macromolecular organic colored substance molecules in the desulfurization waste liquid, and molecular bonds are broken to form organic colored micromolecules through the actions of free radical oxidation, high-temperature pyrolysis, ultraviolet radiation, liquid electric cavitation and the like;
2) Oxidation and decomposition of persulfate activated by transition metal ions: adding persulfate into the desulfurization waste liquid, and utilizing transition metal ions contained in a catalyst in the desulfurization waste liquid to carry out in-situ homogeneous activation on the persulfate to generate sulfate radicals (SO) with strong oxidizing property 4 - H), carrying out chemical oxidative decomposition on organic colored micromolecules in the desulfurization waste liquid;
3) Activated carbon activated persulfate is subjected to oxidative decomposition and adsorption: adding activated carbon into the desulfurization waste liquid, heterogeneously activating the residual persulfate to generate sulfate radicals, continuously oxidizing and decomposing organic colored micromolecules, and simultaneously removing organic colored substances and inorganic colored substances which are difficult to oxidize and decompose by utilizing the adsorption effect of the activated carbon.
The low-temperature plasma oxidation adopts a multi-needle-plate type reactor.
The needle poles and the plate poles of the reactor are arranged at intervals, the needle poles are provided with small holes, the plate poles are corrugated longitudinally, the desulfurization waste liquid is lifted to the top of the reactor by a water tank through a pump and is sprayed out through a spray head, and the desulfurization waste liquid and air form a gas-liquid mixed two-phase body which falls into the water tank through a plasma area for circular treatment.
Furthermore, the needle pole and the plate pole of the multi-needle plate type reactor are made of 316L materials or industrial titanium; the shell of the reactor is made of insulating materials such as ceramics, glass fiber reinforced plastics and the like.
In the low-temperature plasma oxidative decomposition process: the pulse voltage peak value is 10-15 kV, the discharge time is 20-30 min, the discharge frequency is 60-100 Hz, and the distance between the needle pole and the plate pole is 4-10 mm.
The persulfate is (NH) 4 ) 2 S 2 O 8 、Na 2 S 2 O 8 、K 2 S 2 O 8 One of them, when the desulfurization alkali source is ammonia or ammonia water, (NH) is selected 4 ) 2 S 2 O 8 (ii) a When the desulfurization alkali source is Na 2 CO 3 Or NaOH, na is selected 2 S 2 O 8 (ii) a When the desulfurization alkali source is K 2 CO 3 Or, when KOH, K is selected 2 S 2 O 8 . Thus, the persulfate and the secondary salt (NH) in the desulfurization waste liquid of different alkali sources 4 SCN、(NH 4 ) 2 S 2 O 3 、(NH 4 ) 2 SO 4 ; NaSCN、Na 2 S 2 O 3 、Na 2 SO 4 ;KSCN、K 2 S 2 O 3 、K 2 SO 4 ) The method is matched, so that the secondary salt components in the desulfurization waste liquid are not influenced, and the final extraction of high-quality salt products is facilitated.
The transition metal ions are transition metal ions contained in desulfurization catalysts PDS, HPF and the like in the desulfurization waste liquid without addition, wherein the transition metal ions areThe key point of activating persulfate to generate strong oxidizing sulfate radical is transition metal Co in PDS 2+ Can activate persulfate alone and transition metal Co in HPF 2+ 、Fe 2+ Can synergistically activate persulfate. Because the desulfurization waste liquid contains a large amount of thiosulfate with reducibility, fe is effectively avoided 2+ Is oxidized to Fe 3+ And further with SCN - And (3) forming bloody red ferric thiocyanate, and further avoiding forming new colored substances in the decoloring process.
The process parameters of the step 2) are as follows: persulfate (S) 2 O 8 2- ) The dosage and the transition metal ion Co in the desulfurization waste liquid 2+ And or Fe 2+ The mass ratio of (1); the oxidative decomposition temperature is 25-50 ℃, the time is 0.5-1 h, and the stirring speed is 20-35 r/min.
When the catalyst in the desulfurization waste liquid contains single transition metal ions, the oxidative decomposition temperature is 40-50 ℃, and the persulfate is activated by the auxiliary transition metal ions through thermal activation; when the desulfurization catalyst contains two or more than two transition metal ions, the transition metal ions can synergistically activate persulfate, the oxidative decomposition temperature is 25-40 ℃, and the low temperature can reduce the decolorization cost.
The process parameters of the step 3) are as follows: 0.5-1 kg of active carbon/m 3 The temperature of the desulfurized waste liquid is 50-85 ℃, the time is 0.5-1 h, and the stirring speed is 35-50 r/min.
The active carbon in the step 3) is granular active carbon or powdered active carbon which is soaked, cleaned and dried by 5-10 wt% of dilute sulfuric acid. After the activated carbon is soaked in the dilute acid, not only can the impurities such as oil stains and the like be removed, but also the impurities are prevented from being introduced into the desulfurization waste liquid to influence the quality of subsequent salt products; and the surface of the activated carbon is acidic after being soaked in the dilute acid, which is beneficial to activating persulfate and adsorbing processes. Preferably, the invention chooses to soak with dilute sulphuric acid, considering that the sulphate-containing salt in the secondary salt in the desulphurized waste liquid does not affect the quality of the subsequent salt product.
According to the efficient decoloring method for the coking desulfurization waste liquid, low-temperature plasma oxidative decomposition, transition metal ion activated persulfate oxidative decomposition and chemical oxidation technology are used for removing colored substances, activated carbon activated persulfate oxidative decomposition and adsorption are used for removing the colored substances through physical adsorption and chemical oxidation technology, the chemical oxidation decoloring and the physical adsorption decoloring are combined, homogeneous and heterogeneous decoloring technologies are combined, the colored substances are efficiently removed in a synergistic manner, and the chroma removal rate reaches 99%.
Compared with the prior art, the invention has the beneficial effects that:
1) By utilizing the characteristics of low-temperature plasma free radical oxidation, high-temperature pyrolysis, ultraviolet radiation, liquid electric cavitation and the like, macromolecular organic colored substances which are difficult to treat in the desulfurization waste liquid are oxidized and decomposed into easily treated micromolecules or colorless micromolecules;
2) By utilizing the advantage that persulfate can generate strong-oxidative sulfate radical (SO 4-) under the activation condition to efficiently oxidize and decompose organic matters, the efficient chemical oxidation decoloration and the traditional physical adsorption decoloration are effectively combined, SO that the decoloration effect of the desulfurization waste liquid is more efficient and thorough, the consumption of activated carbon is reduced, and the decoloration cost is reduced;
3) The method fully utilizes the transition metal ions contained in the existing catalyst in the desulfurization waste liquid, simultaneously considers the secondary salts (thiocyanate, thiosulfate and sulfate) in the desulfurization waste liquid, ingeniously selects persulfate, belongs to the sulfur-containing salt, and the byproduct sulfate generated in the activation process is also the secondary salt component in the desulfurization waste liquid, so that other impurities are not introduced in the whole process, and the method is favorable for extracting high-quality salt products subsequently.
Drawings
FIG. 1 is a schematic view of an apparatus for low temperature plasma oxidation in the present invention.
In the figure: 1-a pin pole; 2-ground (plate) electrode; 3-a water tank; 4-a pump; 5-a spray head; 6-high voltage pulse power supply; 7-reactor shell.
Detailed Description
The following examples are carried out on the premise of the technical scheme of the invention, and detailed embodiments and specific operation processes are given, but the scope of the invention is not limited to the following examples.
Example 1:
the coking desulfurization waste liquid to be treated in the embodiment is sodium desulfurization waste liquid with PDS as a catalyst, and mainly comprises the following components: pH 7.90, co 2+ 0.025g/L, chroma 3503PCU, naSCN 105g/L, na 2 S 2 O 3 48g/L,Na 2 SO 4 24g/L。
As shown in FIG. 1, 300mL of the desulfurized waste liquid is taken in a water tank 3; starting a pulse power supply 6 switch, controlling the discharge frequency to be 80Hz, enabling the pulse voltage peak value to reach 10kV, and starting discharge between a pin electrode 1 and a plate electrode 2 (three pin electrodes and four plate electrodes are arranged at intervals, the distance is 5mm, and the material of the two is 316L) to generate plasma; starting a water pump 4 to atomize the desulfurization waste liquid through a spray head 5 and form a gas-liquid mixed two-phase body with air to enter between a needle pole 1 and a plate pole 2; and (3) treating the desulfurization waste liquid by using the plasma, then feeding the treated desulfurization waste liquid into a water inlet tank 3, circularly treating the desulfurization waste liquid by using a pump 4 for 20min, and finishing the treatment.
250mL of the desulfurization waste liquid after the plasma treatment is added into a 500mL three-neck flask according to the formula Co 2+ Adding 0.41g of sodium persulfate into the mixture according to the mass ratio of the sodium persulfate to the sodium persulfate being 10, heating the mixture to 50 ℃, stirring the mixture for 0.5h at the rotating speed of 30r/min, and observing the color change of the desulfurized waste liquid; when the color of the desulfurization waste liquid is not changed any more, 0.2g of powdered activated carbon is added, the temperature is raised to 65 ℃, the mixture is stirred for 1 hour at the rotating speed of 45r/min, and the chroma of the filtered desulfurization waste liquid is 32PCU.
Example 2:
the coking desulfurization waste liquid treated by the embodiment is ammonia desulfurization waste liquid of catalyst HPF, and mainly comprises the following components: pH 8.01 (Fe) 2+ 0.038g/L,Co 2+ 0.020g/L, chroma 3986PCU 4 SCN 132g/L,(NH 4 ) 2 S 2 O 3 69g/L, (NH 4 ) 2 SO 4 33g/L。
As shown in FIG. 1, 300mL of the desulfurized waste liquid is taken in a water tank 3; starting a pulse power supply 6 switch, controlling the discharge frequency to be 100Hz, enabling the pulse voltage peak value to reach 10kV, and starting discharge between a pin electrode 1 and a plate electrode 2 (three pin electrodes and four plate electrodes are arranged at intervals, and the material of the pin electrode and the plate electrodes is 316L at intervals of 5 mm) to generate plasma; starting a water pump 4 to atomize the desulfurization waste liquid through a spray head 5 and form a gas-liquid mixed two-phase body with air to enter between a needle pole 1 and a plate pole 2; and (3) treating the desulfurization waste liquid by using the plasma, then feeding the treated desulfurization waste liquid into a water inlet tank 3, circularly treating the desulfurization waste liquid by using a pump 4 for 30min, and finishing the treatment.
Adding 250mL of desulfurized waste liquid after the plasma treatment into a 500mL three-neck flask according to Fe 2+ 、Co 2+ Adding 0.93g of sodium persulfate into the mixture according to the mass ratio of the mixture to the sodium persulfate of 10; when the color of the desulfurization waste liquid is not changed any more, 0.25g of powdered activated carbon is added, the temperature is increased to 80 ℃, the mixture is stirred for 1 hour at the rotating speed of 50r/min, and the chroma of the filtered desulfurization waste liquid is 24PCU.
It will be understood by those skilled in the art that the foregoing is merely a preferred embodiment of the present invention, and that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention.
Claims (8)
1. The efficient decolorizing method of the coking desulfurization waste liquid is characterized in that the decolorizing process is divided into the following three stages:
1) Low-temperature plasma oxidative decomposition: generating high-activity low-temperature plasma by using pulse corona discharge, and enabling the low-temperature plasma to collide and react with molecules of macromolecular organic colored substances in the desulfurization waste liquid to break molecular bonds to form organic colored micromolecules;
2) Oxidative decomposition of transition metal ion activated persulfate: adding persulfate into the desulfurization waste liquid, carrying out in-situ homogeneous phase activation on the persulfate by using transition metal ions contained in a catalyst in the desulfurization waste liquid to generate sulfate radicals, and carrying out chemical oxidative decomposition on organic colored micromolecules in the desulfurization waste liquid;
3) Activated carbon activated persulfate is subjected to oxidative decomposition and adsorption: adding activated carbon into the desulfurization waste liquid, heterogeneously activating the residual persulfate to generate sulfate radicals, continuously oxidizing and decomposing organic colored micromolecules, and simultaneously removing organic colored substances and inorganic colored substances which are difficult to oxidize and decompose by utilizing the adsorption effect of the activated carbon.
2. The method for efficiently decoloring coking desulfurization waste liquid according to claim 1, characterized in that a multi-needle-plate type reactor is adopted for the low-temperature plasma oxidation.
3. The method for efficiently decoloring coking desulfurization waste liquid according to claim 1 or 2, characterized in that in the low-temperature plasma oxidative decomposition process: the peak value of the pulse voltage is 10-15 kV, the discharge time is 20-30 min, the discharge frequency is 60-100 Hz, and the distance between the needle electrode and the plate electrode is 4-10 mm.
4. The method for efficiently decoloring coking desulfurization waste liquid according to claim 1, characterized in that the persulfate is (NH) 4 ) 2 S 2 O 8 、Na 2 S 2 O 8 、K 2 S 2 O 8 One of them, when the desulfurization alkali source is ammonia or ammonia water, (NH) 4 ) 2 S 2 O 8 (ii) a When the desulfurization alkali source is Na 2 CO 3 Or NaOH, na is selected 2 S 2 O 8 (ii) a When the desulfurization alkali source is K 2 CO 3 Or KOH, K is selected 2 S 2 O 8 。
5. The efficient coking desulfurization waste liquid decoloring method according to claim 1, wherein the process parameters of the step 2) are as follows: the consumption of persulfate and the transition metal ion Co in the desulfurization waste liquid 2+ And or Fe 2+ The mass ratio of (1); the oxidative decomposition temperature is 25-50 ℃, the time is 0.5-1 h, and the stirring speed is 20-35 r/min.
6. The method for efficiently decoloring coking desulfurization waste liquid according to claim 5, characterized in that when a catalyst in the desulfurization waste liquid contains a single transition metal ion, the oxidative decomposition temperature is 40-50 ℃; when the desulfurization catalyst contains two or more transition metal ions; the oxidative decomposition temperature is 25-40 ℃.
7. According toThe method for efficiently decoloring coking desulfurization waste liquid of claim 1, characterized in that the process parameters of the step 3) are as follows: 0.5-1 kg of active carbon/m 3 The temperature of the desulfurized waste liquid is 50-85 ℃, the time is 0.5-1 h, and the stirring speed is 35-50 r/min.
8. The method for efficiently decoloring coking desulfurization waste liquid according to claim 1, wherein the activated carbon in the step 3) is granular activated carbon or powdered activated carbon which is soaked, cleaned and dried by 5-10 wt% of dilute sulfuric acid.
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