CN114212930A - Method for improving purity of wet desulphurization wastewater byproduct - Google Patents
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- CN114212930A CN114212930A CN202111293158.9A CN202111293158A CN114212930A CN 114212930 A CN114212930 A CN 114212930A CN 202111293158 A CN202111293158 A CN 202111293158A CN 114212930 A CN114212930 A CN 114212930A
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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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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C01P2006/80—Compositional purity
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- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- 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
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
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Abstract
The invention discloses a method for controlling the purity of a byproduct of wet desulphurization wastewater, which comprises the steps of adjusting the pH value of the wet desulphurization wastewater to 6-9, and then mixing the wet desulphurization wastewater with ferrous salt for reaction to obtain a mixed solution; and (3) concentrating and carrying out solid-liquid separation on the mixed solution to obtain low-chlorine calcium sulfate and ferrous ammonium sulfite products as solids and high-chlorine concentrated brine as liquid. The method can effectively improve the quality of the gypsum which is a byproduct of the wet desulphurization wastewater, replaces the traditional filtering method of a disc vacuum filter, greatly simplifies the operation, and reduces the energy consumption and the water consumption; but also can quickly reduce the ammonia nitrogen concentration in the wet desulphurization wastewater, and avoid the problems of high energy consumption and operation cost of the technologies such as gaseous membrane method deamination nitrogen, stripping deamination nitrogen and the like.
Description
Technical Field
The invention relates to a method for improving purity of a wet desulphurization wastewater byproduct, in particular to a method for improving purity of a wet desulphurization wastewater byproduct by using an ammonium ferrous sulfite method, and belongs to the technical field of wet desulphurization wastewater treatment.
Background
The water quality components of the desulfurization wastewater contain various pollutants such as suspended matters, supersaturated sulfite, ammonia nitrogen, heavy metals and the like, wherein the concentration content of the suspended matters is high, the suspended matters and the solid wastes such as the heavy metals and the like form harmful sludge, and the harmful sludge needs to be subjected to centralized treatment by a solid waste treatment factory, so that the treatment cost is high. The main component of the insoluble suspended matter is gypsum which can be recycled for preparing green building material products such as mortar and the like.
However, the content of chloride ions in the recycled gypsum is high, the coordination capacity of the chloride ions is very strong, when the concentration of the chloride ions is high, the chloride ions and magnesium ions and ammonium ions in wastewater can generate chemical reaction to generate water-soluble chloride salt, the chloride salt is wrapped in the gypsum, the quality of the gypsum can be reduced, and the performance and the quality of the gypsum and products thereof can be greatly limited, for example, when high-chlorine-content desulfurized gypsum is adopted to prepare gypsum mortar, the phenomena of moisture regain and yellowing of the gypsum mortar in the using process can be caused. And can also generate electrochemical reaction with reinforcing steel bars and the like to cause the corrosion of the reinforcing steel bars and cause serious safety problems. Therefore, the reduction of the content of the chloride salt in the gypsum and the improvement of the quality of the chlorine-containing gypsum are very important for the treatment and resource utilization of the gypsum.
Under the current technical conditions, an effective method for reducing the content of chloride salt in the desulfurized gypsum is to wash and filter a gypsum filter cake by using a large amount of washing water. The gypsum is washed by a large amount of washing water, the content of chloride ions can be effectively reduced, but the quality of the gypsum is also influenced, and the problems of high energy consumption, high washing water consumption, complex operation, high cost and the like exist. Therefore, the research of the method for controlling the purity of the byproduct in the wet desulphurization wastewater has important practical significance.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention aims to provide a method for improving the purity of a wet desulphurization waste water byproduct, which can effectively improve the quality of the wet desulphurization waste water byproduct gypsum, replaces the traditional filtering method of a disc vacuum filter, greatly simplifies the operation, and reduces the energy consumption and water consumption; but also can quickly reduce the ammonia nitrogen concentration in the wet desulphurization wastewater, and avoid the problems of high energy consumption and operation cost of the technologies such as gaseous membrane method deamination nitrogen, stripping deamination nitrogen and the like.
In order to achieve the technical purpose, the invention provides a method for improving the purity of a byproduct of wet desulphurization wastewater, which comprises the steps of adjusting the pH value of the wet desulphurization wastewater to 6-9, and then mixing the wet desulphurization wastewater with ferrous salt for reaction to obtain a mixed solution; and (3) concentrating and carrying out solid-liquid separation on the mixed solution to obtain low-chlorine calcium sulfate and ferrous ammonium sulfite products as solids and high-chlorine concentrated brine as liquid.
Mainly contain sulfate radical, sulfite radical, calcium ion, ammonium ion and chloride ion etc. in the wet flue gas desulfurization waste water, prior art mainly is through concentrating the wet flue gas desulfurization waste water and obtaining gypsum product, but can make ammonia nitrogen concentration improve to 10 ~ 20g/L in the concentration process of wet flue gas desulfurization waste water, high concentration ammonia nitrogen will combine with chloride ion and a small amount of impurity magnesium ion in the waste water and form magnesium ammonium chloride crystal salt, mix in calcium sulfate product with the form of coprecipitation, thereby can increase chloride ion content in the gypsum product, influence the gypsum quality. The key point of the technical scheme of the invention is that ammonia nitrogen in the wet desulphurization wastewater is preferably converted into a relatively stable ferrous ammonium sulfite product together with sulfite and ferrous ions by strictly controlling the pH condition of the wet desulphurization wastewater and using ferrous salt in a matching way under a proper condition, so that the formation of magnesium ammonium chloride can be effectively inhibited, chloride ions are still enriched in an aqueous solution as soluble salt, and the chlorine content of a gypsum product is greatly reduced.
Preferably, the wet desulphurization wastewater contains 2100-3200 mg/L sulfate radical, 800-2000 mg/L sulfite radical, 2000-3100 mg/L calcium ion, 1000-2500 mg/L ammonium ion and 15000-20000 mg/L chloride ion. The technical scheme of the invention utilizes the characteristic that the wet desulphurization wastewater is rich in sulfite and ammonium ions, and only a proper amount of ferrous ions are needed to be introduced to convert ammonia nitrogen into stable ferrous ammonium sulfite, thereby effectively preventing the ammonia nitrogen from being separated out in the form of magnesium ammonium chloride.
In a preferred embodiment, the ferrous salt is at least one of ferrous sulfate heptahydrate, ferrous chloride tetrahydrate and ferrous nitrate. The technical scheme of the invention mainly utilizes ferrous ions to convert ammonia nitrogen and sulfite ions, and theoretically common water-soluble iron salts meet the requirements of the technical scheme of the invention.
As a preferable scheme, the adding concentration of the ferrous salt in the wet desulphurization wastewater is 0.3 to 0.8 times, more preferably 0.4 to 0.6 times, and most preferably 0.5 times of the molar concentration of the sulfite in the wet desulphurization wastewater. The preferable adding concentration of the ferrous salt can ensure the full reaction with ammonia nitrogen and sulfite, and the ammonia nitrogen concentration is reduced to avoid the precipitation of magnesium ammonium chloride.
As a preferred solution, the concentration is achieved by a step evaporation concentration device.
As a preferable scheme, the concentration process adopts 3-stage concentration treatment, and the concentration multiple is more than or equal to 14.
As a preferable scheme, the high-chlorine concentrated brine is diluted by steam condensate water generated in the evaporation process to obtain dilute-salt low-ammonia water to replace part of industrial water for recycling.
As an optimal scheme, the wet desulphurization wastewater is acidic, the pH value of the wet desulphurization wastewater can be further reduced after concentration, and in order to ensure that ferrous salt, sulfite and ammonia nitrogen are converted into ammonium ferrous sulfite with high selectivity, the pH value of the wet desulphurization wastewater needs to be strictly controlled within a range of 6-9, so that the pH value of the concentrated wet desulphurization wastewater is ensured to be 5-8, and the optimal pH range of the ferrous salt for precipitating the ammonia nitrogen is ensured. The alkaline substance used for adjusting the pH is at least one of sodium hydroxide, potassium hydroxide and calcium hydroxide.
The mixing mode of the invention is mechanical stirring, magnetic stirring or shaking table oscillation.
The technical scheme of the invention also tries to realize the conversion of ammonia nitrogen in the high-humidity desulfurization wastewater by a magnesium ammonium phosphate method, the magnesium ammonium phosphate method is adopted, the pH of the wastewater solution is required to be ensured to be between 8 and 10 during concentration, and meanwhile, phosphate radical is added to ensure that ammonia nitrogen and magnesium ions in the wastewater react with the externally added phosphate radical to form magnesium ammonium phosphate, so that the formation of magnesium ammonium chloride can be prevented from being effectively inhibited. However, the method has obvious defects that the pH condition for generating magnesium ammonium phosphate is strict, ammonia nitrogen is easily converted into free ammonia to enter the atmosphere to cause pollution under the high pH condition, and meanwhile, the introduction of phosphate radical introduced from the outside easily causes the water quality to exceed the standard, so that subsequent high-chlorine concentrated brine is difficult to recycle. Therefore, the technical scheme of the invention adopts the ferrous ammonium sulfite method under milder conditions, does not introduce external ions, and has good inhibition effect on formation of magnesium ammonium chloride.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
1. the technical scheme of the invention can effectively inhibit the formation of magnesium ammonium chloride and effectively reduce the content of chloride ions in the recovered gypsum.
2. The invention needs less chemical drugs, only needs alkaline substances and ferrous salt, has simple process and equipment and low energy consumption.
3. The invention can also simply, conveniently and rapidly reduce the ammonia nitrogen concentration in the wet desulphurization wastewater, and avoids the problems of high energy consumption and operation cost of the traditional treatment process. Belongs to the technical field of wet desulphurization wastewater treatment.
Drawings
FIG. 1 is a process flow diagram of a method of increasing the purity of a wet-desulfurization waste water byproduct of the present invention.
Detailed Description
The following examples are intended to further illustrate the present invention and are not intended to limit the scope of the claims.
The wet desulfurization waste water in the following examples and comparative examples mainly contained 2794mg/L, 1828mg/L sulfite, 2338mg/L calcium ion, 1450mg/L ammonium ion, and 19600mg/L chloride ion.
Example 1
The method for controlling the purity of the wet desulphurization wastewater byproduct comprises the following steps:
(1) taking 5L of wet desulphurization wastewater, and adding sodium hydroxide to adjust the pH of the wastewater solution to 6.4;
(2) adding 15.06g of ferrous sulfate into the wet desulphurization wastewater after the pH value is adjusted in the step (1), and uniformly stirring by a mechanical arm;
(3) introducing steam into the steam side of the 3-stage evaporation and concentration device;
(4) introducing the wet desulphurization wastewater in the step (2) into the water side of the step evaporation concentration device;
(5) the wastewater in the step (4) is concentrated by 3 grades to obtain high suspended matter wastewater;
(6) introducing the high-suspended matter wastewater obtained in the step (5) into a plate-and-frame filter press for solid-liquid separation, wherein the solid is low-chlorine calcium sulfate and ferrous ammonium sulfite, and the liquid is high-salt water;
(7) drying the low-chlorine calcium sulfate and ferrous ammonium sulfite solids obtained in the step (6) at 80 ℃ to constant weight, and recycling;
(8) and (4) condensing the steam in the step (3) by 3 stages to generate condensed water, recycling the condensed water, introducing the condensed water into the high-salinity water in the step (6), and diluting to obtain dilute-salt low-ammonia water to replace part of industrial water for recycling.
In example 1, the chlorine content of the obtained low-chlorine calcium sulfate and ammonium ferrous sulfite was 4.88%, and the weight was 25.60 g; the high-salt water contains 10920mg/L sulfate radical, 5250mg/L sulfite radical, 7338mg/L calcium ion, 3565mg/L ammonium ion, 239540mg/L chloride ion, etc.
Example 2
The method for controlling the purity of the wet desulphurization wastewater byproduct comprises the following steps:
(1) taking 5L of wet desulphurization wastewater, and adding sodium hydroxide to adjust the pH of the wastewater solution to 7.8;
(2) adding 18.56g of ferrous sulfate into the wet desulphurization wastewater after the pH value is adjusted in the step (1), and uniformly stirring by a mechanical arm;
(3) introducing steam into the steam side of the 3-stage evaporation and concentration device;
(4) introducing the wet desulphurization wastewater in the step (2) into the water side of the step evaporation concentration device;
(5) the wastewater in the step (4) is concentrated by 3 grades to obtain high suspended matter wastewater;
(6) introducing the high-suspended matter wastewater obtained in the step (5) into a plate-and-frame filter press for solid-liquid separation, wherein the solid is low-chlorine calcium sulfate and ferrous ammonium sulfite, and the liquid is high-salt water;
(7) drying the low-chlorine calcium sulfate and ferrous ammonium sulfite solids obtained in the step (6) at 80 ℃ to constant weight, and recycling;
(8) and (4) condensing the steam in the step (3) by 3 stages to generate condensed water, recycling the condensed water, introducing the condensed water into the high-salinity water in the step (6), and diluting to obtain dilute-salt low-ammonia water to replace part of industrial water for recycling.
In example 2, the chlorine content of the obtained low-chlorine calcium sulfate and ammonium ferrous sulfite was 4.31%, and the weight thereof was 28.50 g; the high-salt water contains 10876mg/L sulfate radical, 5350mg/L sulfite radical, 7340mg/L calcium ion, 3321mg/L ammonium ion, 24239 mg/L chloride ion and the like.
Example 3
The method for controlling the purity of the wet desulphurization wastewater byproduct comprises the following steps:
(1) taking 5L of wet desulphurization wastewater, and adding sodium hydroxide to adjust the pH of the wastewater solution to 9.0;
(2) adding 26.00g of ferrous sulfate into the wet desulphurization wastewater after the pH value is adjusted in the step (1), and uniformly stirring by a mechanical arm;
(3) introducing steam into the steam side of the 3-stage evaporation and concentration device;
(4) introducing the wet desulphurization wastewater in the step (2) into the water side of the step evaporation concentration device;
(5) the wastewater in the step (4) is concentrated by 3 grades to obtain high suspended matter wastewater;
(6) introducing the high-suspended matter wastewater obtained in the step (5) into a plate-and-frame filter press for solid-liquid separation, wherein the solid is low-chlorine calcium sulfate and ferrous ammonium sulfite, and the liquid is high-salt water;
(7) drying the low-chlorine calcium sulfate and ferrous ammonium sulfite solids obtained in the step (6) at 80 ℃ to constant weight, and recycling;
(8) and (4) condensing the steam in the step (3) by 3 stages to generate condensed water, recycling the condensed water, introducing the condensed water into the high-salinity water in the step (6), and diluting to obtain dilute-salt low-ammonia water to replace part of industrial water for recycling.
In example 3, the obtained low-chlorine calcium sulfate and ammonium ferrous sulfite had a chlorine content of 4.37%, a weight of 27.71g, and a chlorine content of 4.37%; the high-salt water contains 10997mg/L sulfate, 5298mg/L sulfite, 7471mg/L calcium ion, 3875mg/L ammonium ion, 242356mg/L chloride, etc.
Comparative example 1
The method for controlling the purity of the wet desulphurization wastewater byproduct comprises the following steps:
(1) taking 5L of wet desulphurization wastewater, and adding sodium hydroxide to adjust the pH of the wastewater solution to 3.0;
(2) adding 32.00g of ferrous sulfate into the wet desulphurization wastewater after the pH value is adjusted in the step (1), and uniformly stirring by a mechanical arm;
(3) introducing steam into the steam side of the 3-stage evaporation and concentration device;
(4) introducing the wet desulphurization wastewater in the step (2) into the water side of the step evaporation concentration device;
(5) the wastewater in the step (4) is concentrated by 3 grades to obtain high suspended matter wastewater;
(6) introducing the high-suspended matter wastewater obtained in the step (5) into a plate-and-frame filter press for solid-liquid separation, wherein the solid is low-chlorine calcium sulfate and ferrous ammonium sulfite, and the liquid is high-salt water;
(7) drying the low-chlorine calcium sulfate and ferrous ammonium sulfite solids obtained in the step (6) at 80 ℃ to constant weight, and recycling;
(8) and (4) condensing the steam in the step (3) by 3 stages to generate condensed water, recycling the condensed water, introducing the condensed water into the high-salinity water in the step (6), and diluting to obtain dilute-salt low-ammonia water to replace part of industrial water for recycling.
In comparative example 1, the chlorine content of the obtained low-chlorine calcium sulfate and ammonium ferrous sulfite was 31.73%, and the weight was 11.77 g; the high-salt water contains 10857mg/L sulfate, 9558mg/L sulfite, 7290mg/L calcium ion, 12834mg/L ammonium ion, 178470mg/L chloride ion and the like.
Comparative example 2
The method for controlling the purity of the wet desulphurization wastewater byproduct comprises the following steps:
(1) taking 5L of wet desulphurization wastewater, and adding sodium hydroxide to adjust the pH of the wastewater solution to 10.0;
(2) adding 7.50g of ferrous sulfate into the wet desulphurization wastewater after the pH value is adjusted in the step (1), and uniformly stirring by a mechanical arm;
(3) introducing steam into the steam side of the 3-stage evaporation and concentration device;
(4) introducing the wet desulphurization wastewater in the step (2) into the water side of the step evaporation concentration device;
(5) the wastewater in the step (4) is concentrated by 3 grades to obtain high suspended matter wastewater;
(6) introducing the high-suspended matter wastewater obtained in the step (5) into a plate-and-frame filter press for solid-liquid separation, wherein the solid is low-chlorine calcium sulfate and ferrous ammonium sulfite, and the liquid is high-salt water;
(7) drying the low-chlorine calcium sulfate and ferrous ammonium sulfite solids obtained in the step (6) at 80 ℃ to constant weight, and recycling;
(8) and (4) condensing the steam in the step (3) by 3 stages to generate condensed water, recycling the condensed water, introducing the condensed water into the high-salinity water in the step (6), and diluting to obtain dilute-salt low-ammonia water to replace part of industrial water for recycling.
In comparative example 2, the chlorine content of the obtained low-chlorine calcium sulfate and ferrous ammonium sulfite was 26.31%, and the weight was 13.41 g; the high-salt water contains 10387mg/L sulfate radical, 10922mg/L sulfite radical, 7261mg/L calcium ion, 9934mg/L ammonium ion and 191640mg/L chloride ion.
Claims (6)
1. A method for improving the purity of a wet desulphurization wastewater byproduct is characterized by comprising the following steps: adjusting the pH value of the wet desulphurization wastewater to 6-9, and then mixing the wet desulphurization wastewater with ferrous salt for reaction to obtain a mixed solution; and (3) concentrating and carrying out solid-liquid separation on the mixed solution to obtain low-chlorine calcium sulfate and ferrous ammonium sulfite products as solids and high-chlorine concentrated brine as liquid.
2. The method for improving the purity of the wet desulphurization waste water byproduct according to claim 1, wherein: the wet desulphurization wastewater contains 2100-3200 mg/L sulfate radical, 800-2000 mg/L sulfite radical, 2000-3100 mg/L calcium ion, 1000-2500 mg/L ammonium ion and 15000-20000 mg/L chloride ion.
3. The method for improving the purity of the wet desulfurization waste water byproduct as claimed in claim 1, wherein: the ferrous salt is at least one of ferrous sulfate heptahydrate, ferrous chloride tetrahydrate and ferrous nitrate.
4. A method for increasing the purity of a wet flue gas desulfurization waste water byproduct as set forth in claim 1 or 3, wherein: the adding concentration of the ferrous salt in the wet desulphurization wastewater is 0.3-0.8 time of the molar concentration of the sulfite in the wet desulphurization wastewater.
5. The method for improving the purity of the wet desulfurization waste water byproduct as claimed in claim 1, wherein: the concentration is realized by a step evaporation concentration device.
6. The method for improving purity of a wet desulfurization waste water byproduct of claim 5, wherein: the concentration process adopts 3-level concentration treatment, and the concentration multiple is more than or equal to 14.
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| JPS51126990A (en) * | 1975-04-30 | 1976-11-05 | Idemitsu Kosan Co Ltd | Process for removing nitrogen oxides |
| KR100798417B1 (en) * | 2007-07-26 | 2008-01-28 | 한국지질자원연구원 | Preparation method of magnesium chloride anhydrate from magnesium chloride aqueous solution with ammonium chloride |
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| CN109354248A (en) * | 2018-11-12 | 2019-02-19 | 湘潭大学 | A kind of processing method of wet desulphurization waste water |
| CN111268753A (en) * | 2020-02-14 | 2020-06-12 | 北京光耀环境工程有限公司 | Desulfurization wastewater treatment system and method |
| CN111847701A (en) * | 2019-04-29 | 2020-10-30 | 中冶长天国际工程有限责任公司 | Pretreatment method of ultrahigh-concentration ammonia nitrogen wastewater |
| CN112299491A (en) * | 2019-07-30 | 2021-02-02 | 中冶长天国际工程有限责任公司 | Method for synthesizing ferrous ammonium sulfite |
-
2021
- 2021-11-03 CN CN202111293158.9A patent/CN114212930B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51126990A (en) * | 1975-04-30 | 1976-11-05 | Idemitsu Kosan Co Ltd | Process for removing nitrogen oxides |
| KR100798417B1 (en) * | 2007-07-26 | 2008-01-28 | 한국지질자원연구원 | Preparation method of magnesium chloride anhydrate from magnesium chloride aqueous solution with ammonium chloride |
| CN107098372A (en) * | 2017-04-19 | 2017-08-29 | 湖北三宁化工股份有限公司 | A kind of method that hydrochloric acid decomposes phosphorus mine tailing extracting sulfuric acid calcium pyroborate and magnesium hydroxide |
| CN109354248A (en) * | 2018-11-12 | 2019-02-19 | 湘潭大学 | A kind of processing method of wet desulphurization waste water |
| CN111847701A (en) * | 2019-04-29 | 2020-10-30 | 中冶长天国际工程有限责任公司 | Pretreatment method of ultrahigh-concentration ammonia nitrogen wastewater |
| CN112299491A (en) * | 2019-07-30 | 2021-02-02 | 中冶长天国际工程有限责任公司 | Method for synthesizing ferrous ammonium sulfite |
| CN111268753A (en) * | 2020-02-14 | 2020-06-12 | 北京光耀环境工程有限公司 | Desulfurization wastewater treatment system and method |
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