CN111960597A - Method for refining high-salt high-organic wastewater byproduct salt - Google Patents
Method for refining high-salt high-organic wastewater byproduct salt Download PDFInfo
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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
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- C02F1/048—Purification of waste water by evaporation
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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Abstract
The invention discloses a method for refining a byproduct salt of high-salt high-organic wastewater, belonging to the technical field of wastewater recovery. According to the invention, the extracting agent is added into the MVR residual liquid, the solubility of the crystalline salt is reduced through the salt-like salting-out effect, the crystalline salt is separated out, the yield of the byproduct salt is improved, and the treatment capacity and cost of hazardous waste are reduced; meanwhile, the extraction agent is used for extracting organic matters on the surface of the crystalline salt, and the crystalline salt is refined and purified, so that the industrial byproduct salt recovery standard is reached, and the method has high environmental value and economic value.
Description
Technical Field
The invention belongs to the technical field of wastewater recovery, and particularly relates to a method for refining a byproduct salt of high-salt high-organic wastewater.
Background
With the acceleration of production development and industrialization process in China, the amount of sewage and wastewater generated in the production and life process is increased year by year, wherein the sewage and wastewater comprises a large amount of salt-containing wastewater. The high-salinity high-organic wastewater is one of the common industrial salt-containing wastewater, mainly comes from industrial production sewage, and refers to wastewater with the total salt content (based on NaCl content) of at least 1 percent, can inhibit the growth of microorganisms to a certain extent, also has a large amount of organic pollutants, and belongs to one of the wastewater difficult to treat.
At present, the zero discharge and resource recovery technology of high-salt and high-organic wastewater in China mainly adopts a mechanical vapor recompression evaporation technology (MVR), and the technology utilizes secondary vapor and energy thereof generated by an evaporation system, improves low-grade vapor into a high-grade vapor heat source through mechanical work of a compressor, circularly provides heat energy for the evaporation system, and reduces energy consumption. After the high-salt high-organic wastewater is subjected to the MVR process, one part of the high-salt high-organic wastewater is converted into condensate, and the other part of the high-salt high-organic wastewater is converted into MVR residual liquid containing high-boiling-point organic matters with higher salt content. A large amount of salt exists in residual liquid, the salt is miscellaneous salt with various inorganic salts and high-boiling point organic matters, and the miscellaneous salt can only be used as dangerous waste if not treated, so that on one hand, the waste of salt resources is caused, and on the other hand, the increase of the treatment cost of the dangerous waste also can cause the increase of the operation cost.
Through retrieval, the Chinese patent application with the application publication number CN109824194A and the application publication date 2019, 5 and 31 discloses a treatment method of high-salt and high-COD organic wastewater, which treats the high-salt and high-COD organic wastewater through ultrafiltration membrane filtration, COD remover oxidation treatment and multi-effect or MVR evaporation, wherein only flash evaporation desalination is mentioned in the step of the multi-effect or MVR evaporation treatment, but how to treat residual liquid generated after desalination is not mentioned.
In addition, the byproduct salt in the MVR residual liquid can carry partial organic matters in the mother liquor in the crystallization process, and the organic matters are the main reason for low purity of the crystallized salt. Generally, one approach to this phenomenon is: and putting the crystallized salt into a pyrolysis furnace to carbonize organic matters, dissolving, filtering and removing the organic matters, and then evaporating to obtain high-purity byproduct salt. However, this method requires treatment of the exhaust gas generated during pyrolysis and is relatively energy-intensive. The other treatment method comprises the following steps: preparing the crystalline salt into an aqueous solution, adding sodium hypochlorite to mineralize organic matters, adding polyaluminium chloride to flocculate and precipitate, filtering, and evaporating and crystallizing the filtrate to obtain the crystalline salt. The method needs to treat mineralized sludge sediment, thereby increasing the treatment cost; but also introduces impurity ions, which may cause the purity of the crystalline salt to be reduced.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems of low yield and purity of byproduct salt in wastewater treatment and high treatment cost of hazardous waste in the prior art, the invention provides a method for refining the byproduct salt in high-salt high-organic wastewater. According to the invention, the extracting agent is added into the MVR residual liquid, the solubility of the crystalline salt is reduced through the salt-like salting-out effect, the crystalline salt is separated out, the yield of the byproduct salt is improved, and the treatment capacity and cost of hazardous waste are reduced; meanwhile, the extraction agent is used for extracting organic matters on the surface of the crystalline salt, and the crystalline salt is refined and purified, so that the industrial byproduct salt recovery standard is reached, and the method has high environmental value and economic value.
2. Technical scheme
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention relates to a method for refining a byproduct salt of high-salt high-organic wastewater, which comprises the following steps:
s10, treating the high-salt and high-organic wastewater by a Mechanical Vapor Recompression (MVR) technology to obtain MVR crystallized salt and residual liquid A;
s20, adding an extracting agent into the residual liquid A, stirring, and separating out crystal salt to obtain a residual liquid B;
s30, mixing the MVR crystal salt obtained in the step S10 with the crystal salt separated out in the step S20, and adding an extracting agent for extraction to obtain refined salt and an extraction liquid;
s40, combining the raffinate B in the step S20 and the extract in the step S30, and carrying out rectification separation to obtain an extractant and a raffinate C.
Preferably, the type of the extracting agent is determined according to the type of the characteristic functional group of the organic matters in the raw wastewater, and the extracting agent meets the conditions that the boiling point is low (the boiling point is lower than 100 ℃) and the high-boiling-point organic matters in the raw wastewater can be extracted.
Preferably, in step S10, the crystalline salt includes, but is not limited to, one or two of sodium sulfate and sodium chloride.
Preferably, in step S20, the adding volume of the extracting agent is 5-30% of the volume of the raffinate a.
Preferably, in step S30, the volume ratio between the mixed crystalline salt and the added extractant is 1: (1-10).
Preferably, in step S30, the number of extraction times is 1 to 10.
Preferably, the extractant rectified in step S40 is recycled to step S20 and step S30.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the method for refining the byproduct salt of the high-salt high-organic wastewater, the extracting agent is added into the residual liquid of the high-salt high-organic wastewater after MVR treatment, the salt-like salting-out effect is utilized to reduce the solubility of the crystalline salt, increase the yield of the byproduct salt, and reduce the treatment capacity and cost of hazardous waste;
(2) according to the method for refining the byproduct salt from the high-salt high-organic wastewater, disclosed by the invention, the organic matter on the surface of the crystalline salt is extracted by using the extracting agent, and the crystalline salt is cleaned, refined and purified, so that the quality of the byproduct salt is improved and the byproduct salt reaches the recovery standard of industrial byproduct salt;
(3) according to the method for refining the byproduct salt of the high-salt and high-organic wastewater, the extracting agent can be separated from the extracting solution through rectification, the separated extracting agent can be returned to the front-end salting-out treatment and salt refining treatment step for recycling, and the operation cost is saved.
Drawings
FIG. 1 is a schematic flow chart of a method for refining a byproduct salt from high-salt and high-organic wastewater according to the present invention.
Detailed Description
The invention is further described with reference to specific examples.
As shown in figure 1, the method for refining the byproduct salt of the high-salt high-organic wastewater comprises the following steps:
s10, treating the high-salt and high-organic wastewater through an MVR technology to obtain high-salt and high-organic wastewater MVR crystallized salt, high-salt and high-organic wastewater MVR condensate and high-salt and high-organic wastewater MVR raffinate A, wherein the crystallized salt comprises one or two of sodium sulfate and sodium chloride, and the high-salt and high-organic wastewater MVR raffinate A is raffinate containing saturated salt;
s20, feeding the high-salt and high-organic wastewater MVR residual liquid A into a salting-out unit, adding an extracting agent into the residual liquid A, stirring for 5-30 minutes to reduce the salt solubility in the residual liquid A, separating out crystallized salt, and obtaining a residual liquid B; wherein the adding volume of the extracting agent is 5-30% of the volume of the residual liquid A; the type of the extractant is determined according to the type of the characteristic functional group of the organic matters in the raw wastewater, and the extractant meets the conditions that the boiling point is low (generally lower than 100 ℃) and the high-boiling-point organic matters in the raw wastewater can be extracted. Preferably, the extractant is low boiling point organic matter such as alcohols, ketones, ethers, benzene, etc. or a mixture thereof (if the organic matter in the wastewater contains carbonyl, the extractant is acetone, and if the organic matter in the wastewater contains hydroxyl, the extractant can be selected from methanol, ethanol, etc.).
S30, mixing the MVR crystallized salt in the step S10 and the crystallized salt precipitated in the step S20 in a salt refining unit, and adding an extracting agent into the salt refining unit for extraction, wherein the volume ratio of the mixed crystallized salt to the added extracting agent can be 1: (1-10), extracting to obtain refined salt and an extraction liquid; in the extraction process, the extractant serves as a cleaning agent to extract and clean organic matters on the surface of the crystalline salt, the crystalline salt is refined and purified to reach the industrial byproduct salt recovery standard, and the extraction frequency can be 1-10 times until the color of the cleaned extraction liquid is not obviously different from that of the extractant;
s40, combining the raffinate B in the step S20 and the extract liquor in the step S30, and carrying out rectification separation to obtain an extractant and a raffinate C containing high-boiling point organic matters; the recovered extractant can be respectively added into the salting-out unit in the step S20 and the salt refining unit in the step S30 for recycling of the extractant, and the residual liquid C is treated as hazardous waste. It should be noted that after the treatment by the method of the present invention, the yield of byproduct salt can be increased, the quality of byproduct salt can be improved, and the treatment amount and cost of hazardous waste can be reduced.
Example 1
The method for refining the byproduct salt of the high-salt and high-organic wastewater comprises the following steps:
s10, treating the high-salt high-organic pesticide wastewater containing sodium chloride and n-hexanol by adopting an MVR (mechanical vapor recompression) technology, wherein the treatment scale is 6m3And d, the MVR inlet water COD concentration is 80000-100000 mg/L, and the salt content is about 10%. MVR process control parameters: the reaction temperature is 80 ℃, the reaction pressure is 0.08-0.09 MPa, and the reaction time is 1.5h, so that MVR condensate, MVR residual liquid A and sodium chloride salt containing organic impurities are obtained;
s20, sending the high-salt high-organic wastewater MVR raffinate A into a salting-out unit, adding an extracting agent methanol into the raffinate A, wherein the volume ratio of the methanol addition to the raffinate is about 1: 20, continuously stirring for 5-30 minutes, separating out crystal salt, and filtering residual liquid to obtain crystal salt and MVR residual liquid B containing methanol;
s30, mixing the sodium chloride salt containing the organic impurities obtained in the step S10 and the crystalline salt obtained in the step S20 in a salt refining unit, and adding an extracting agent methanol into the mixture in three groups, wherein the volume ratio of the crystalline salt to the methanol is 1: 1. 1: 3 and 1: 10, stirring and shaking up to extract residual organic matters in the crystallized salt, and separating the extract from the crystallized salt through suction filtration. After more than 3 times of extraction and suction filtration processes are repeated, the colors of the methanol before and after extraction are not obviously different, and the crystallized salt is detected to have no organic residue, so that the sodium chloride byproduct salt with higher purity is obtained, and the industrial byproduct salt recovery standard is met;
s40, combining the MVR raffinate B containing the methanol in the step S20 and the extract liquid collected in the step S30, introducing the mixture into a rectifying tower for rectifying and separating, recovering the methanol, and returning the recovered methanol to the salting-out unit in the step S20 and the salt refining unit in the step S30 again to finish the recovery and utilization of the extractant methanol. And treating the residual liquid C separated by the rectifying tower as hazardous waste.
The recovery amount of the sodium chloride salt treated by the method of the embodiment is 324.8 kg/d; in the salt refining unit, the purity of the crystal salt obtained by three groups of different methanol adding amounts is 97.3 percent, 98.7 percent and 98.9 percent respectively.
From this, it is understood that although the purity of the crystalline salt slightly increases as the amount of methanol added increases, the ratio of the volume ratio of the crystalline salt to the methanol added is 1: the economic efficiency is highest when 3.
Example 2
The method for refining the byproduct salt of the high-salt and high-organic wastewater comprises the following steps:
s10, treating the high-salt and high-organic pesticide wastewater containing sodium sulfate and high-boiling-point carbonyl compounds by adopting MVR technology, wherein the treatment scale is 10m3And d, the MVR inlet water COD concentration is 60000-80000 mg/L, and the salt content is about 8%. MVR process control parameters: the reaction temperature is 80 ℃, the reaction pressure is 0.08-0.09 MPa, and the reaction time is 1.5h, so that MVR condensate, MVR residual liquid A and sodium sulfate containing organic impurities are obtained;
s20, feeding the high-salt and high-organic wastewater MVR raffinate A into a salting-out unit, adding an extracting agent acetone into the raffinate A, wherein the volume ratio of the added acetone to the MVR mother liquor is 1: 20. 1: 10 and 3: 10, continuously stirring for 5-30 minutes, separating out crystal salt, and filtering residual liquid to obtain crystal salt and MVR residual liquid B containing acetone;
s30, mixing the sodium sulfate containing the organic impurities obtained in the step S10 and the crystalline salt obtained in the step S20 in a salt refining unit, and adding acetone serving as an extracting agent, wherein the volume ratio of the crystalline salt to the acetone is 1: 3, stirring and shaking up to extract residual organic matters in the crystallized salt, and separating the extract from the crystallized salt through suction filtration. After more than 3 times of extraction and suction filtration processes are repeated, the color of acetone before and after extraction is not obviously different, and the crystallized salt is detected to have no organic residue, so that the sodium sulfate byproduct salt with higher purity is obtained, and the industrial byproduct salt recovery standard is met;
s40, combining the MVR raffinate B containing acetone in the step S20 and the extract collected in the step S30, introducing the mixture into a rectifying tower for rectifying and separating, recovering the acetone, and returning the recovered acetone to the salting-out unit in the step S20 and the salt refining unit in the step S30 again to finish the recovery and utilization of the extractant acetone. And treating the residual liquid C separated by the rectifying tower as hazardous waste.
The purity of the sodium sulfate salt obtained by the method of the embodiment can reach 98.5 percent.
Therefore, with the gradual increase of the acetone adding amount in the S20 salting-out link, the sodium sulfate recovery amounts of the three experiments are 270.4kg/d, 283.5kg/d and 288.1kg/d respectively. Although the recovery amount of the salt gradually increases with the addition amount of acetone, the rectification recovery cost also increases in consideration of the fact that the addition of acetone in an excessive amount increases the amount of waste liquid. Therefore, the volume ratio of the added acetone to the MVR mother solution is 1: the economic benefit is higher when 10 hours.
Comparative example 1
The basic contents of this comparative example are the same as example 1, except that: the method for refining the byproduct salt of the high-salt and high-organic wastewater in the comparative example comprises the following steps:
s10, mixingSodium chloride-containing high-salt high-organic pesticide wastewater is treated by adopting MVR technology, and the treatment scale is 6m3And d, the MVR inlet water COD concentration is 80000-100000 mg/L, and the salt content is about 10%. MVR process control parameters: the reaction temperature is 80 ℃, the reaction pressure is 0.08-0.09 MPa, and the reaction time is 1.5h, so that MVR condensate, MVR residual liquid and sodium chloride salt containing organic impurities are obtained;
s20, sending the sodium chloride salt containing the organic impurities obtained in the step S10 into a salt refining unit, adding an extracting agent methanol (the volume ratio of the crystal salt to the methanol is 1: 3), stirring and shaking uniformly to extract residual organic matters in the crystal salt, and separating the extract from the crystal salt through suction filtration. After more than 3 times of extraction and suction filtration processes are repeated, the colors of the methanol before and after extraction are not obviously different, and the crystallized salt is detected to have no organic residue, so that the sodium chloride byproduct salt with higher purity is obtained, and the industrial byproduct salt recovery standard is met;
s30, the extract liquid collected in the step S20 is guided into a rectifying tower to be rectified and separated, methanol is recovered, and the recovered methanol returns to the salt refining unit in the step S20 again, so that the recovery and the utilization of the extractant methanol are completed. And (4) treating the residual liquid separated by the rectifying tower and the MVR residual liquid obtained in the step S10 as hazardous wastes.
The sodium chloride salt obtained by the treatment of the method of the comparative example has the recovery amount of 249.8kg/d and the purity of 98.7 percent. The amount of hazardous waste to be disposed is increased by 70kg/d compared with the example 1.
Comparative example 2
The basic contents of this comparative example are the same as example 1, except that: the method for refining the byproduct salt of the high-salt and high-organic wastewater in the comparative example comprises the following steps:
s10, treating the sodium chloride-containing high-salinity high-organic pesticide wastewater by adopting an MVR (mechanical vapor recompression) technology, wherein the treatment scale is 6m3And d, the MVR inlet water COD concentration is 80000-100000 mg/L, and the salt content is about 10%. MVR process control parameters: the reaction temperature is 80 ℃, the reaction pressure is 0.08-0.09 MPa, and the reaction time is 1.5h, so that MVR condensate, MVR residual liquid A and sodium chloride salt containing organic impurities are obtained;
s20, sending the high-salt high-organic wastewater MVR raffinate A into a salting-out unit, adding an extracting agent methanol into the raffinate A, wherein the volume ratio of the methanol addition to the raffinate is about 1: 20, continuously stirring for 5-30 minutes, separating out crystal salt, and filtering residual liquid to obtain crystal salt and MVR residual liquid B containing methanol;
s30, mixing the sodium chloride salt containing the organic impurities obtained in the step S10 with the crystalline salt obtained in the step S20, putting the mixture into an oven for treatment for 4 hours, and taking out the mixture to obtain a byproduct salt;
s40, introducing the MVR residual liquid containing the methanol in the step S10 into a rectifying tower for rectifying separation, recovering the methanol, and returning the recovered methanol to the salting-out unit in the step S20 again to finish the recovery and utilization of the extractant methanol. And treating the residual liquid C separated by the rectifying tower as hazardous waste.
The sodium chloride salt obtained by the method of the comparative example has the recovery amount of 324.8kg/d, the purity of 72.1 percent and yellowish color, and cannot be recycled as industrial byproduct salt.
Claims (7)
1. A method for refining a byproduct salt of high-salt high-organic wastewater comprises the following steps:
s10, treating the high-salt and high-organic wastewater by an MVR technology to obtain MVR crystal salt and residual liquid A;
s20, adding an extracting agent into the residual liquid A, stirring, and separating out crystal salt to obtain a residual liquid B;
s30, mixing the MVR crystal salt obtained in the step S10 with the crystal salt separated out in the step S20, and adding an extracting agent for extraction to obtain refined salt and an extraction liquid;
s40, combining the raffinate B in the step S20 and the extract in the step S30, and carrying out rectification separation to obtain an extractant and a raffinate C.
2. The method for refining the byproduct salt of high-salinity high-organic wastewater according to claim 1, characterized in that: the extractant is low boiling point alcohol, ketone, ether, benzene or their mixture.
3. The method for refining the byproduct salt of high-salinity high-organic wastewater according to claim 1, characterized in that: in step S10, the crystalline salt includes one or both of sodium sulfate and sodium chloride.
4. The method for refining the byproduct salt of high-salinity high-organic wastewater according to claim 1, characterized in that: in step S20, the adding volume of the extracting agent is 5-30% of the volume of the residual liquid A.
5. The method for refining the byproduct salt of high-salinity high-organic wastewater according to claim 1, characterized in that: in step S30, the volume ratio of the mixed crystalline salt to the added extractant is 1: (1-10).
6. The method for refining the byproduct salt of high-salinity high-organic wastewater according to claim 1, characterized in that: in step S30, the number of extraction times is 1-10.
7. The method for refining the byproduct salt of high-salinity high-organic wastewater according to claim 1, characterized in that: recycling the extractant rectified in the step S40 to the step S20 and the step S30.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113501609A (en) * | 2021-07-08 | 2021-10-15 | 江苏瑞达环保科技有限公司 | Hazardous waste reduction process based on extraction crystallization technology |
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| CN109516625A (en) * | 2018-12-05 | 2019-03-26 | 北京环球中科水务科技有限公司 | A kind of processing method of high salt organic waste water |
| CN110054343A (en) * | 2019-05-29 | 2019-07-26 | 山东特保罗环保节能科技有限公司 | The rectifying pretreatment of high organic wastewater with high salt and salt processing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109502714A (en) * | 2017-09-15 | 2019-03-22 | 阜新达得利化工股份有限公司 | A kind of process for extracting high purity inorganic salt from wastewater from chemical industry with high salt using rectifying coupling dilution crystallization |
| CN109516625A (en) * | 2018-12-05 | 2019-03-26 | 北京环球中科水务科技有限公司 | A kind of processing method of high salt organic waste water |
| CN110054343A (en) * | 2019-05-29 | 2019-07-26 | 山东特保罗环保节能科技有限公司 | The rectifying pretreatment of high organic wastewater with high salt and salt processing method |
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| CN113501609A (en) * | 2021-07-08 | 2021-10-15 | 江苏瑞达环保科技有限公司 | Hazardous waste reduction process based on extraction crystallization technology |
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