CN111547916A - Salt and nitrate separation method for nitrate-rich wastewater - Google Patents
Salt and nitrate separation method for nitrate-rich wastewater Download PDFInfo
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- CN111547916A CN111547916A CN202010269818.9A CN202010269818A CN111547916A CN 111547916 A CN111547916 A CN 111547916A CN 202010269818 A CN202010269818 A CN 202010269818A CN 111547916 A CN111547916 A CN 111547916A
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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
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/18—Dehydration
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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
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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
- C02F1/22—Treatment of water, waste water, or sewage by freezing
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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
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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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
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
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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
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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Abstract
The invention discloses a salt and nitrate salt separation method for nitrate-rich wastewater, which comprises the following steps: (1) introducing the nitrate-rich wastewater into an evaporator for evaporation treatment to obtain a concentrated solution; (2) sending the concentrated solution to a freezing and crystallizing device to separate out mirabilite from the concentrated solution at the temperature of-5-0 ℃; then carrying out solid-liquid separation on the crystal slurry to obtain mirabilite; (3) precooling the frozen mother liquor after solid-liquid separation, and then introducing the frozen mother liquor into a nanofiltration chamber, recovering the cold energy of the frozen mother liquor, and simultaneously adjusting the temperature of the mother liquor to be suitable for the use working condition of a nanofiltration membrane; sodium chloride in the freezing mother liquor can pass through a nanofiltration membrane arranged in the nanofiltration tank and is enriched on one side of the nanofiltration membrane; sodium sulfate can not pass through the nanofiltration membrane and is enriched on the other side of the nanofiltration membrane; (4) and (3) carrying out thermal salt separation on the sodium chloride-rich filtrate passing through the nanofiltration membrane to obtain sodium chloride. The salt and nitrate salt separation method for the nitrate-rich wastewater can effectively increase the recovery rate of target salt and reduce the rate of solid waste and miscellaneous salt.
Description
Technical Field
The invention relates to the technical field of wastewater recycling treatment, in particular to a salt and nitrate salt separation method for nitrate-rich wastewater.
Background
In the production process of a plurality of organic or inorganic chemical products, a large amount of high-salt wastewater is generated due to process requirements, wherein the content of sodium chloride and sodium sulfate is higher than 2%, the content of sodium chloride and sodium sulfate is more than 10%, and the content of sodium chloride and sodium sulfate is even more than 20%, and the high-salt wastewater is high-salt wastewater which is mostly subjected to evaporative crystallization or MVR evaporative crystallization in the currently mature treatment process; this produces a large amount of by-product miscellaneous salts (mixed salts of NaCl and sodium sulfate). The sodium chloride/sodium sulfate content of the salt is more than 95 percent, and simultaneously, the salt contains a large amount of organic or inorganic impurities, can not be directly used as industrial raw material salt, can not be used for food or medical use, and is stockpiled by most manufacturers. The long-term stacking of the mixed salt of sodium chloride and sodium sulfate not only occupies a large amount of fields, but also has great threat to the environment, salt and impurities are easy to lose, the surrounding soil is salinized, the surrounding vegetation is endangered, and meanwhile, the mixed salt causes pollution to surrounding rivers, water sources, rice fields and the like.
The yield of target salt in the conventional salt-nitrate separation of mine water, coal chemical industry and the like is about 80%, the yield of miscellaneous salt is between 15% and 20%, the yield of sodium chloride and sodium sulfate is to be further improved, the yield of miscellaneous salt can be reduced, and the cost of solid waste is reduced.
Disclosure of Invention
The invention aims to provide a salt and nitrate separating method for nitrate-rich wastewater, which can effectively increase the recovery rate of target salt and reduce the impurity salt rate of solid waste.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a salt and nitrate salt separation method for nitrate-rich wastewater, which comprises the following steps:
(1) introducing the nitrate-rich wastewater into an evaporator for evaporation treatment to obtain a concentrated solution;
(2) the concentrated solution is sent to a freezing and crystallizing device for freezing and crystallizing, so that mirabilite is separated out from the concentrated solution at the temperature of-5-0 ℃; then carrying out solid-liquid separation on the crystal slurry to obtain mirabilite;
(3) precooling the frozen mother liquor after solid-liquid separation, and then introducing the frozen mother liquor into a nanofiltration chamber, wherein sodium chloride in the frozen mother liquor can pass through a nanofiltration membrane arranged in the nanofiltration chamber and is enriched on one side of the nanofiltration membrane; the sodium sulfate in the freezing mother liquor can not pass through the nanofiltration membrane but is enriched on the other side of the nanofiltration membrane;
(4) and (3) carrying out thermal salt separation on the sodium chloride-rich filtrate passing through the nanofiltration membrane to obtain sodium chloride.
Further, in the step (1), the evaporator is a multi-effect evaporator or an MVR evaporator.
Further, in the step (2), sodium sulfate is obtained after evaporating and dehydrating the mirabilite.
Further, in the step (2), the solid-liquid separation specifically comprises: and (3) sending the frozen mother liquor into a centrifugal machine, carrying out centrifugal separation in the centrifugal machine, recovering solids to obtain mirabilite, and sending the liquid into a nano filter.
Further, in the step (3), after nanofiltration treatment, the nitrate-rich concentrated water in the nanofiltration tank is returned to the freezing crystallization device.
Further, in the step (4), the thermal salt separation specifically comprises: and (3) introducing the sodium chloride-rich filtrate into a multi-effect evaporator or MVR evaporator for evaporation, concentration and crystallization treatment, centrifuging the concentrated solution in a centrifugal machine, and collecting to obtain sodium chloride.
Further, in the step (4), the sodium chloride is purified by salt washing and dried to obtain a finished sodium chloride product.
The invention has the beneficial effects that:
1. the process of the invention takes cold method salt separation as a basic process, introduces a nanofiltration process section into an evaporation system, improves the purity and yield of inorganic salt, enables the inorganic salt to be reused, does not generate secondary waste which is difficult to treat in the production process, reduces the waste of resources, reduces the damage of waste water to the environment, and has good economic and social benefits.
2. The process flow of the invention has high automation degree and mature process, is suitable for industrial utilization, and can be used for treating high-salinity wastewater in industries such as mine water, coal chemical industry, steel making and the like.
Drawings
FIG. 1 is a process flow diagram of the salt-nitrate salt separation method of the nitrate-rich wastewater of the invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental methods used in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used therein are commercially available without otherwise specified.
As described in the background art, the yield of target salt in the conventional salt-nitrate separation of mine water, coal chemical industry and the like in the prior art is about 80%, the impurity salt rate is between 15% and 20%, and the yield of sodium chloride and sodium sulfate is required to be further improved.
In order to solve the technical problem, the invention provides a salt and nitrate salt separation method for nitrate-rich wastewater. As shown in fig. 1, the method comprises the following steps:
(1) introducing the nitrate-rich wastewater into an evaporator for evaporation treatment to obtain a concentrated solution;
(2) the concentrated solution is sent to a freezing and crystallizing device for freezing and crystallizing, so that mirabilite is separated out from the concentrated solution at the temperature of-5-0 ℃; then carrying out solid-liquid separation on the crystal slurry to obtain mirabilite;
(3) precooling the frozen mother liquor after solid-liquid separation, and then introducing the frozen mother liquor into a nanofiltration chamber, wherein sodium chloride in the frozen mother liquor can pass through a nanofiltration membrane arranged in the nanofiltration chamber and is enriched on one side of the nanofiltration membrane; the sodium sulfate in the freezing mother liquor can not pass through the nanofiltration membrane but is enriched on the other side of the nanofiltration membrane;
(4) and (3) carrying out thermal salt separation on the sodium chloride-rich filtrate passing through the nanofiltration membrane to obtain sodium chloride.
In step (1) of the present invention, the nitrate-rich wastewater is preferably pretreated to remove impurities in the wastewater before being subjected to evaporation treatment. The evaporation treatment can use a multi-effect evaporator or an MVR evaporator, and the concentration of the salts in the wastewater is gradually increased through evaporation.
Because the solubility of the sodium sulfate is greatly changed along with the temperature, in the step (2), the concentrated solution is sent to a freezing and crystallizing device for freezing and crystallizing, so that the mirabilite is separated out from the waste water, and the primary salt separation is realized. After freezing treatment, the crystal slurry is subjected to solid-liquid separation to obtain mirabilite. The crystallization separation can be carried out in various ways, such as filtration, centrifugation, and the like. Preferably, the crystal is separated by centrifugation, specifically: and (4) feeding the crystal slurry into a centrifugal machine, carrying out centrifugal separation in the centrifugal machine, and recovering solids to obtain mirabilite. And evaporating and dehydrating mirabilite to obtain a finished sodium sulfate product.
After freezing crystallization and solid-liquid separation, the main salt in the liquid is sodium chloride accompanied by a small amount of sodium sulfate. No matter the existing salt separation technology such as hot salt separation, cold salt separation or mixed salt separation is adopted, sodium chloride and sodium sulfate cannot be separated, so that the salt impurity rate is high. In the invention, the problem is successfully solved by introducing a nanofiltration process into the salt-nitrate separation process.
Nanofiltration, also known as low pressure reverse osmosis, is an emerging field of membrane separation technology, and has separation performance between reverse osmosis and ultrafiltration, allowing some inorganic salts and some solvents to permeate through the membrane, thereby achieving separation effect. The aperture range of the nanofiltration membrane used in the nanofiltration process is only about a few nanometers, and the nanofiltration membrane can intercept organic matters with molecular weight more than 100 and multivalent ions, and allow small molecular organic matters and monovalent ions to permeate through, so that substances with relatively small molecular weight, such as inorganic salt or small molecular organic matters such as glucose, sucrose and the like, can be separated from a solvent.
In the step (3), the frozen mother liquor after solid-liquid separation is precooled and then introduced into the nanofiltration chamber, so that the cold quantity of the frozen mother liquor is recovered, and the temperature of the mother liquor is adjusted to be suitable for the use condition of the nanofiltration membrane. The sodium chloride in the liquid can pass through a nanofiltration membrane and is enriched in the filtered liquid due to the small molecular weight of the sodium chloride in the liquid; and the sodium sulfate has larger molecular weight and can not pass through the nanofiltration membrane, so that the sodium sulfate is enriched on the other side of the nanofiltration membrane, and the separation of sodium chloride and sodium sulfate is realized. Furthermore, the nitrate-rich concentrated water in the nano filter can be returned to the freezing and crystallizing device, so that the full utilization of sodium sulfate is realized.
Because the filtrate is sodium chloride solution with higher concentration, the sodium chloride crystal can be obtained by adopting the traditional thermal method to separate salt. Therefore, in the step (4), after nanofiltration treatment, the sodium chloride-rich filtrate is introduced into a multi-effect evaporator or an MVR evaporator for evaporation, concentration and crystallization treatment, and the concentrated solution enters a centrifuge for centrifugation and collection to obtain sodium chloride. And (3) collecting the obtained sodium chloride, and performing salt washing, purification and drying to obtain a sodium chloride finished product with higher purity.
The salt and nitrate separation process for the nitrate-rich wastewater can effectively increase the recovery rate of target salt, reduce the rate of solid waste and miscellaneous salt, avoid secondary waste which is difficult to treat in the production process, reduce the waste of resources, reduce the damage of the wastewater to the environment and have good economic and social benefits.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (7)
1. A salt and nitrate separation method for nitrate-rich wastewater is characterized by comprising the following steps:
(1) introducing the nitrate-rich wastewater into an evaporator for evaporation treatment to obtain a concentrated solution;
(2) the concentrated solution is sent to a freezing and crystallizing device for freezing and crystallizing, so that mirabilite is separated out from the concentrated solution at the temperature of-5-0 ℃; then carrying out solid-liquid separation on the crystal slurry to obtain mirabilite;
(3) precooling the frozen mother liquor after solid-liquid separation, and then introducing the frozen mother liquor into a nanofiltration chamber, wherein sodium chloride in the frozen mother liquor can pass through a nanofiltration membrane arranged in the nanofiltration chamber and is enriched on one side of the nanofiltration membrane; the sodium sulfate in the freezing mother liquor can not pass through the nanofiltration membrane but is enriched on the other side of the nanofiltration membrane;
(4) and (3) carrying out thermal salt separation on the sodium chloride-rich filtrate passing through the nanofiltration membrane to obtain sodium chloride.
2. The method for separating salt and nitrate from nitrate-rich wastewater as claimed in claim 1, wherein in the step (1), the evaporator is a multi-effect evaporator or an MVR evaporator.
3. The method for separating salt and nitrate from nitrate-rich wastewater according to claim 1, wherein in the step (2), sodium sulfate is obtained after the mirabilite is evaporated and dehydrated.
4. The method for separating salt and nitrate from nitrate-rich wastewater according to claim 1, wherein in the step (2), the solid-liquid separation specifically comprises: and (3) sending the frozen mother liquor into a centrifugal machine, carrying out centrifugal separation in the centrifugal machine, recovering solids to obtain mirabilite, and sending the liquid into a nano filter.
5. The method for separating salt and nitrate from nitrate-rich wastewater according to claim 1, wherein in the step (3), after the nanofiltration treatment, the nitrate-rich concentrated water in the nanofiltration tank is returned to the freezing and crystallizing device.
6. The method for separating salt and nitrate from nitrate-rich wastewater according to claim 1, wherein in the step (4), the thermal separation salt is specifically: and (3) introducing the sodium chloride-rich filtrate into a multi-effect evaporator or MVR evaporator for evaporation, concentration and crystallization treatment, centrifuging the concentrated solution in a centrifugal machine, and collecting to obtain sodium chloride.
7. The method for separating salt and nitrate from nitrate-rich wastewater according to claim 1, wherein in the step (4), the sodium chloride is subjected to salt washing, purification and drying to obtain a finished product of sodium chloride.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112794344A (en) * | 2020-12-14 | 2021-05-14 | 伊犁川宁生物技术股份有限公司 | Method for purifying sodium sulfate from antibiotic wastewater |
CN114671554A (en) * | 2020-12-24 | 2022-06-28 | 大连波美科技有限公司 | Zero-discharge sewage system containing guanidine salt and application method |
CN115465995A (en) * | 2022-09-22 | 2022-12-13 | 倍杰特集团股份有限公司 | Membrane separation salt and nitrate-based salt-containing wastewater recycling treatment system and method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US5587083A (en) * | 1995-04-17 | 1996-12-24 | Chemetics International Company Ltd. | Nanofiltration of concentrated aqueous salt solutions |
CN108947064A (en) * | 2018-07-02 | 2018-12-07 | 广州汉泰环境技术有限公司 | A kind of the sub-prime crystallization processes and its system of brine waste |
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2020
- 2020-04-08 CN CN202010269818.9A patent/CN111547916A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5587083A (en) * | 1995-04-17 | 1996-12-24 | Chemetics International Company Ltd. | Nanofiltration of concentrated aqueous salt solutions |
CN108947064A (en) * | 2018-07-02 | 2018-12-07 | 广州汉泰环境技术有限公司 | A kind of the sub-prime crystallization processes and its system of brine waste |
Non-Patent Citations (1)
Title |
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朱洪法: "《精细化工 产品、技术与配方》", 31 August 1998, 中国石化出版社 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112794344A (en) * | 2020-12-14 | 2021-05-14 | 伊犁川宁生物技术股份有限公司 | Method for purifying sodium sulfate from antibiotic wastewater |
CN114671554A (en) * | 2020-12-24 | 2022-06-28 | 大连波美科技有限公司 | Zero-discharge sewage system containing guanidine salt and application method |
CN115465995A (en) * | 2022-09-22 | 2022-12-13 | 倍杰特集团股份有限公司 | Membrane separation salt and nitrate-based salt-containing wastewater recycling treatment system and method |
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