WO2021232391A1 - Procédé de récupération de produit et dispositif utilisé dans la préparation et processus d'utilisation d'un agent de traitement des eaux usées - Google Patents

Procédé de récupération de produit et dispositif utilisé dans la préparation et processus d'utilisation d'un agent de traitement des eaux usées Download PDF

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WO2021232391A1
WO2021232391A1 PCT/CN2020/091714 CN2020091714W WO2021232391A1 WO 2021232391 A1 WO2021232391 A1 WO 2021232391A1 CN 2020091714 W CN2020091714 W CN 2020091714W WO 2021232391 A1 WO2021232391 A1 WO 2021232391A1
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Prior art keywords
reaction
treatment agent
product
wastewater treatment
magnesium
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PCT/CN2020/091714
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English (en)
Chinese (zh)
Inventor
姚鹤
丁宏铃
李建仓
曾能
唐丽梅
雍红团华
侯晓刚
杨耀华
张福晏
朱竑卫
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兰州兰石中科纳米科技有限公司
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Priority to PCT/CN2020/091714 priority Critical patent/WO2021232391A1/fr
Priority to CN202080099993.6A priority patent/CN115443185A/zh
Publication of WO2021232391A1 publication Critical patent/WO2021232391A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • 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
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
    • 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
    • C02F2101/20—Heavy metals or heavy metal compounds

Definitions

  • This application relates to the field of wastewater treatment, and in particular to a product recovery method and device used in the preparation and use of wastewater treatment agents.
  • One of the embodiments of the present application provides a method for product recovery during the preparation and use of wastewater treatment agents.
  • the method includes: obtaining a wastewater treatment agent through a first reaction process; passing the wastewater treatment agent into the wastewater produced by preparing heavy metals, and obtaining a second reaction product through a second reaction process, wherein the second reaction product The reaction product at least includes the product after the wastewater treatment agent undergoes adsorption; through the third reaction process, the second reaction product is processed to obtain a third reaction product, wherein the third reaction product includes at least the first part And a second part; performing a first recovery process on the first part to obtain a reactant for preparing the wastewater treatment agent; and performing a second recovery process on the second part to obtain a heavy metal Reactant.
  • the obtaining the wastewater treatment agent through the first reaction process includes: passing the magnesium salt solution, the precipitation agent, and the coating agent into the reaction device at a preset flow rate; and performing the reaction under the first reaction condition; And after the first separation process, the product salt solution and the wastewater treatment agent are obtained.
  • the magnesium salt solution includes a magnesium sulfate solution or a magnesium chloride solution.
  • the precipitating agent includes sodium hydroxide solution, ammonia water, and calcium hydroxide solution.
  • the coating agent includes ammonium oleate, sodium oleate, ammonium stearate, sodium stearate, ammonium hydrogenated dimerate, sodium hydrogenated dimerate, ammonium dimerate, dimer acid Sodium or potassium stearyl phosphate.
  • the preset flow rate is 200 mL/min to 20 L/min.
  • the first reaction conditions include a first reaction temperature of 20°C to 50°C.
  • the product salt solution includes a sodium sulfate solution; and, the method further includes: crystallizing the sodium sulfate solution to generate Glauber's salt.
  • said passing the waste water treatment agent into the waste water produced by the preparation of heavy metals, and obtaining the second reaction product through the second reaction process includes: the waste water treatment agent adsorbs all the waste water under the second reaction conditions. The heavy metals in the waste water; and the second separation process is performed on the waste water after adsorption to obtain the product of the waste water treatment agent after adsorption.
  • the second reaction conditions include a second reaction temperature of 20°C to 50°C.
  • the second reaction conditions include a pH value of 5-11.
  • the wastewater produced by the preparation of heavy metals includes at least one of nickel, copper, cobalt, arsenic, cadmium, and lead.
  • the processing of the second reaction product through the third reaction process to obtain the third reaction product includes: passing carbon dioxide gas into the product after adsorption of the wastewater treatment agent, and Performing a desorption reaction under the third reaction condition to obtain a third reaction product; and performing a third separation process on the third reaction product to obtain the first part and the second part.
  • the third reaction condition includes the pressure of the desorption reaction from 0.3 MPa to 0.5 MPa.
  • the first part includes magnesium bicarbonate solution; and the second part includes heavy metal carbonate precipitation.
  • the performing the first recovery treatment on the first part includes: heating the magnesium bicarbonate solution to obtain a magnesium carbonate precipitate; and calcining the magnesium carbonate precipitate to obtain a product carbon dioxide gas And magnesium oxide solid, the product carbon dioxide gas is recycled for the reactant of the third reaction process; and the magnesium oxide solid is subjected to a flue gas desulfurization reaction to obtain a magnesium sulfate solution, and the magnesium sulfate solution is used to prepare the The reactant of the wastewater treatment agent.
  • One of the embodiments of the present application provides a device for product recovery during the preparation and use of a wastewater treatment agent.
  • the device includes: a first device for obtaining a wastewater treatment agent through a first reaction process; a second device for passing the wastewater treatment agent into the wastewater produced by the preparation of heavy metals through a second reaction process, Obtain a second reaction product, where the second reaction product at least includes the product after the wastewater treatment agent undergoes adsorption; a third device is used to process the second reaction product through a third reaction process, A third reaction product is obtained, wherein the third reaction product includes at least a first part and a second part; a first recovery device for performing a first recovery treatment on the first part to obtain the waste water treatment agent And a second recovery device for performing a second recovery process on the second part to obtain a reactant for preparing the heavy metal.
  • Figure 1 is a flowchart of an exemplary product recovery method used in the preparation and use of wastewater treatment agents according to some embodiments of the present application;
  • Figure 2 is a schematic diagram of an exemplary product recovery device used in the preparation and use of wastewater treatment agents according to some embodiments of the present application.
  • Fig. 3 is a schematic diagram of an exemplary product recovery method used in the preparation and use of wastewater treatment agents according to some embodiments of the present application.
  • system is a method for distinguishing different components, elements, parts, parts, or assemblies of different levels.
  • the words can be replaced by other expressions.
  • the waste water treatment agent can adsorb heavy metal ions in the waste water produced by the preparation of heavy metals, and obtain the product of the waste water treatment agent after the adsorption and the waste water after the adsorption. After the adsorption, the content of heavy metal ions in the wastewater is reduced and can meet the discharge standard, so it can be directly discharged without harm to the ecological environment.
  • the product after the adsorption of the wastewater treatment agent can be processed and separated, and further processed for recycling, to obtain the reactant for the preparation of the wastewater treatment agent and the reactant for the preparation of heavy metals, which can be recycled, which not only protects the environment, but also And save resources.
  • Fig. 1 is an exemplary flow chart of a product recovery method used in the preparation and use of a wastewater treatment agent according to some embodiments of the present application.
  • the process 100 may be automatically performed by the control system.
  • the process 100 may be implemented through control instructions, and the control system controls various devices to complete the operations of the process 100 based on the control instructions.
  • the process 100 may be performed semi-automatically.
  • one or more operations of process 100 may be performed manually by an operator.
  • one or more additional operations not described may be added, and/or one or more operations discussed herein may be deleted.
  • the order of operations shown in FIG. 1 is not restrictive.
  • step 110 a wastewater treatment agent is obtained through the first reaction process.
  • the first reaction process can be realized by the first device.
  • the wastewater treatment agent may be a nano water treatment agent.
  • the wastewater treatment agent may be nano-magnesium hydroxide.
  • the reactants for preparing the wastewater treatment agent may include a magnesium salt solution, a precipitation agent, and a coating agent.
  • the magnesium salt solution, the precipitating agent, and the coating agent may be respectively introduced into the first reaction device at a preset flow rate, and the reaction is carried out under the first reaction conditions, and then the product salt solution is obtained through the first separation process.
  • wastewater treatment agent may be a bubble liquid film reactor, which includes at least a reaction cylinder and a stirring device.
  • the magnesium salt solution may include magnesium sulfate solution, magnesium chloride solution, magnesium nitrate solution, and the like.
  • the concentration of the magnesium salt solution may be 0.5 mol/L to 3 mol/L.
  • the concentration of the magnesium salt solution may be 0.7 mol/L to 2.8 mol/L.
  • the concentration of the magnesium salt solution may be 0.9 mol/L to 2.6 mol/L.
  • the concentration of the magnesium salt solution may be 1.1 mol/L to 2.4 mol/L.
  • the concentration of the magnesium salt solution may be 1.3 mol/L to 2.2 mol/L.
  • the concentration of the magnesium salt solution may be 1.5 mol/L to 2.0 mol/L.
  • the concentration of the magnesium salt solution may be 1.7 mol/L to 1.8 mol/L.
  • the precipitating agent may be used to precipitate the magnesium salt solution.
  • the precipitating agent may include sodium hydroxide solution, ammonia water, calcium hydroxide solution, and the like.
  • the precipitation agent may also include ammonia gas and the like.
  • the concentration of the precipitating agent can be determined according to the concentration of the magnesium salt solution and the flow rate of the magnesium salt solution and the precipitating agent passing into the first reaction device, so that the stoichiometric ratio of the magnesium salt and the precipitating agent participating in the reaction is 1:2.
  • the concentration of the magnesium sulfate solution can be 1.1 mol/L ⁇ 2.4 mol/L
  • the concentration of the corresponding precipitation agent sodium hydroxide solution can be 2.2 mol /L ⁇ 4.8mol/L
  • the concentration of the magnesium chloride solution can be 1.1mol/L ⁇ 2.4mol/L
  • the concentration of the corresponding precipitation agent sodium hydroxide solution can be 2.2mol/L ⁇ 4.8mol/L.
  • the concentration of the magnesium chloride solution can be 1.1 mol/L to 2.4 mol/L, and the concentration of the corresponding precipitation agent sodium hydroxide solution can be It is 1.1mol/L ⁇ 2.4mol/L.
  • gas can also be used in the process of preparing the wastewater treatment agent, which is used to mix the reactants uniformly and enhance the mass and heat transfer between phases.
  • the gas can separate the reactant into a bubble liquid film, the bubble is the dispersed phase, and the liquid film is the continuous phase, forming a nano-reaction environment.
  • the magnesium salt solution and the precipitating agent can react in the liquid film to generate nanoparticles.
  • the gas may be an inert gas, such as nitrogen, helium, and the like.
  • the coating agent may include fatty acid, polyunsaturated fatty acid, sulfonate, sulfate, phosphate, titanate, silicon Acid esters and so on.
  • the coating agent may include ammonium oleate, sodium oleate, ammonium stearate, sodium stearate, ammonium hydrogenated dimerate, sodium hydrogenated dimerate, ammonium dimerate, sodium dimerate , Potassium octadecyl phosphate, etc.
  • the non-polar part of the coating can extend to the inside of the bubble, and the polar part can extend to the liquid film.
  • the coating agent can be combined with the surface of the newly generated nanoparticles at the interface between the bubbles and the liquid film to form a coating layer to generate nanocapsule particles (ie, nano wastewater treatment agent).
  • the concentration of the coating agent may be 0.005 mol/L to 0.02 mol/L. In some embodiments, the concentration of the coating agent may be 0.006 mol/L to 0.019 mol/L. In some embodiments, the concentration of the coating agent may be 0.007 mol/L to 0.018 mol/L. In some embodiments, the concentration of the coating agent may be 0.008 mol/L to 0.017 mol/L.
  • the concentration of the coating agent may be 0.009 mol/L to 0.016 mol/L. In some embodiments, the concentration of the coating agent may be 0.01 mol/L to 0.015 mol/L. In some embodiments, the concentration of the coating agent may be 0.011 mol/L to 0.014 mol/L. In some embodiments, the concentration of the coating agent may be 0.012 mol/L to 0.013 mol/L.
  • the predetermined flow rate at which the magnesium salt solution, the precipitation agent, and the coating agent are respectively introduced into the first reaction device may be 200 mL/min to 20000 mL/min. In some embodiments, the preset flow rate may be 210 mL/min to 15000 mL/min. In some embodiments, the preset flow rate may be 220 mL/min to 10000 mL/min. In some embodiments, the preset flow rate may be 230 mL/min to 6000 mL/min. In some embodiments, the preset flow rate may be 240 mL/min to 2000 mL/min. In some embodiments, the preset flow rate may be 250 mL/min to 800 mL/min.
  • the preset flow rate may be 260 mL/min to 600 mL/min. In some embodiments, the preset flow rate may be 270 mL/min to 400 mL/min. In some embodiments, the preset flow rate may be 280 mL/min to 360 mL/min. In some embodiments, the preset flow rate may be 290 mL/min to 320 mL/min. In some embodiments, the preset flow rate may be 300 mL/min.
  • the first reaction conditions may include a first reaction temperature.
  • the first reaction temperature may be 20°C-50°C.
  • the first reaction temperature may be 21°C to 45°C.
  • the first reaction temperature may be 22°C-40°C.
  • the first reaction temperature may be 23°C to 35°C.
  • the first reaction temperature may be 24°C to 30°C.
  • the first reaction temperature may be 25°C-28°C.
  • the first reaction temperature may be 26°C-27°C.
  • the first reaction condition may include the stirring speed of the bubble liquid film reactor.
  • the stirring speed may be 1000 r/min to 6000 r/m.
  • the stirring speed may be 1500r/min to 5500r/m.
  • the stirring speed may be 2000 r/min to 5000 r/m.
  • the stirring speed may be 2500r/min to 4500r/m.
  • the stirring speed may be 3000 r/min to 4000 r/m.
  • the stirring speed may be 3200 r/min to 3800 r/m.
  • the stirring speed may be 3400r/min to 3600r/m.
  • the stirring speed may be 3500 r/m.
  • the reaction product after performing the reaction under the first reaction conditions may be a foamy reaction product.
  • the first separation process may include filtering, washing, drying, etc., the reaction product (for example, a foamy reaction product).
  • the first separation process can be implemented by a first separation device.
  • the product salt solution and the wastewater treatment agent can be obtained.
  • the product salt solution may include sodium sulfate solution, sodium chloride solution, sodium nitrate solution, ammonium sulfate solution, ammonium chloride solution, ammonium nitrate solution, calcium sulfate solution, calcium chloride solution, calcium nitrate solution, etc. .
  • the product salt solution is a sodium sulfate solution
  • the sodium sulfate solution can also be crystallized to generate Glauber's salt (sodium sulfate decahydrate).
  • the crystallization temperature of the crystallization treatment may be -4°C to -10°C.
  • the crystallization temperature of the crystallization treatment may be -4.2°C to -9.5°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -4.4°C to -9°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -4.6°C to -8.5°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -4.8°C to -8°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -5°C to -7.5°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -5.2°C to -7°C.
  • the crystallization temperature of the crystallization treatment may be -5.4°C to -6.8°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -5.6°C to -6.6°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -5.8°C to -6.4°C. In some embodiments, the crystallization temperature of the crystallization treatment may be -6°C to -6.2°C.
  • step 120 the wastewater treatment agent is passed into the wastewater produced by the preparation of heavy metals, and a second reaction product is obtained through a second reaction process.
  • the second reaction process can be realized by a second device.
  • the waste water produced by the preparation of heavy metals may be produced by a heavy metal smelting device (or a heavy metal smelting production line).
  • the wastewater produced by the preparation of heavy metals may include at least one of nickel, copper, cobalt, arsenic, cadmium, and lead.
  • the content of nickel may be 20 mg/L to 40 mg/L.
  • the content of copper may be 3 mg/L to 6 mg/L.
  • the content of cobalt may be 0.2 mg/L to 1.0 mg/L.
  • the content of arsenic may be 2 mg/L to 6 mg/L.
  • the content of cadmium may be 0.02 mg/L to 0.06 mg/L.
  • the content of lead may be 1 mg/L to 3 mg/L.
  • the wastewater treatment agent can adsorb heavy metals in the wastewater under the second reaction conditions; then, the wastewater after the adsorption can be subjected to a second separation process to obtain the product of the wastewater treatment agent after the adsorption.
  • the adsorption process can be realized by a second reaction device.
  • the second reaction device may be an adsorption reactor.
  • the wastewater treatment agent and wastewater can be metered into the second reaction device according to the saturated adsorption capacity of various heavy metal ions by the wastewater treatment agent.
  • the saturated adsorption capacity of the nano-magnesium hydroxide wastewater treatment agent for heavy metal ions in the wastewater is 74.07 mg/g, that is, 1 g of the nano-magnesium hydroxide wastewater treatment agent can adsorb 74.07 mg of heavy metal ions.
  • the second reaction conditions may include a second reaction temperature.
  • the second reaction temperature may be 20°C-50°C. In some embodiments, the second reaction temperature may be 21°C to 45°C. In some embodiments, the second reaction temperature may be 22°C-40°C. In some embodiments, the second reaction temperature may be 23°C to 35°C. In some embodiments, the second reaction temperature may be 24°C to 30°C. In some embodiments, the second reaction temperature may be 25°C-28°C. In some embodiments, the second reaction temperature may be 26°C-27°C.
  • the second reaction conditions may include pH.
  • the pH value may be 5-11. In some embodiments, the pH value may be 5.5-10.5. In some embodiments, the pH value may be 6-10. In some embodiments, the pH value may be 6.5 to 9.5. In some embodiments, the pH value may be 7-9. In some embodiments, the pH value may be 7.5 to 8.5. In some embodiments, the pH value may be 8.
  • the second reaction conditions may also include stirring time.
  • the mixing time will affect the adsorption speed of the wastewater treatment agent to the heavy metal ions in the wastewater.
  • the stirring time may be 10 minutes to 60 minutes. In some embodiments, the stirring time may be 15 minutes to 55 minutes. In some embodiments, the stirring time may be 20 minutes to 50 minutes. In some embodiments, the stirring time may be 25 minutes to 45 minutes. In some embodiments, the stirring time may be 30 minutes to 40 minutes. In some embodiments, the stirring time may be 32 minutes to 38 minutes. In some embodiments, the stirring time may be 34 minutes to 36 minutes. In some embodiments, the stirring time may be 35 minutes.
  • the second separation process may include filtering the wastewater after adsorption (including the product of the wastewater treatment agent after adsorption, that is, the solid matter that adsorbs heavy metal ions). After filtration, the second reaction product can be obtained. The second reaction product at least includes the product after the wastewater treatment agent undergoes adsorption. In some embodiments, the second separation process can be implemented by a second separation device. In some embodiments, after filtering the second reaction product, the content of heavy metal ions in the wastewater after adsorption is: total nickel 1.0 mg/L, total cobalt 1.0 mg/L, total copper 0.5 mg/L, Total cadmium is 0.1mg/L, total arsenic is 0.5mg/L. Therefore, after the wastewater treatment agent adsorbs the wastewater produced by the preparation of heavy metals, the obtained wastewater after adsorption can meet the discharge standard, and therefore can be directly discharged.
  • step 130 the second reaction product is processed through the third reaction process to obtain the third reaction product.
  • the third reaction process can be realized by a third device.
  • carbon dioxide gas may be passed into the second reaction product, and the desorption reaction is performed under the third reaction conditions to obtain the third reaction product.
  • the third reaction product may include at least a first part and a second part. Further, the third reaction product can be subjected to a third separation process to obtain the first part and the second part.
  • the desorption reaction can be realized by a third reaction device.
  • the third reaction device may be a desorption reactor.
  • the second reaction product that is, the product after the wastewater treatment agent has undergone adsorption
  • the second reaction product can be mixed with soft water, and stirred to disperse the second reaction product (the product after the wastewater treatment agent has undergone adsorption). Further, the dispersed second reaction product is passed into the desorption reactor through a mud pump for desorption reaction.
  • the third reaction condition may include the pressure of the desorption reaction, that is, the pressure of the gas in the third reaction device where the third reaction product is located.
  • the pressure of the desorption reaction may include 0.3 MPa to 0.5 MPa.
  • the pressure of the desorption reaction may include 0.31 MPa to 0.49 MPa.
  • the pressure of the desorption reaction may include 0.32 MPa to 0.48 MPa.
  • the pressure of the desorption reaction may include 0.33 MPa to 0.47 MPa.
  • the pressure of the desorption reaction may include 0.34 MPa to 0.46 MPa.
  • the pressure of the desorption reaction may include 0.35 MPa to 0.45 MPa.
  • the pressure of the desorption reaction may include 0.36 MPa to 0.44 MPa. In some embodiments, the pressure of the desorption reaction may include 0.37 MPa to 0.43 MPa. In some embodiments, the pressure of the desorption reaction may include 0.38 MPa to 0.42 MPa. In some embodiments, the pressure of the desorption reaction may include 0.39 MPa to 0.41 MPa. In some embodiments, the pressure of the desorption reaction may include 0.4 MPa.
  • the third reaction condition may include the pressure maintenance time of the desorption reaction.
  • the pressure maintenance time may include 1 h to 6 h. In some embodiments, the pressure maintaining time may include 1.5h to 5.5h. In some embodiments, the pressure maintaining time may include 2h to 5h. In some embodiments, the pressure maintaining time may include 2.5h to 4.5h. In some embodiments, the pressure maintenance time may include 2.7h to 4.3h. In some embodiments, the pressure maintaining time may include 2.9h to 4.1h. In some embodiments, the pressure maintaining time may include 3.1h to 3.9h. In some embodiments, the pressure maintaining time may include 3.3h to 3.7h. In some embodiments, the pressure maintaining time may include 3.4h to 3.6h. In some embodiments, the pressure maintenance time may include 3.5 hours.
  • the third reaction condition may include the temperature of the desorption reaction.
  • the temperature of the desorption reaction may include 20°C to 50°C. In some embodiments, the temperature of the desorption reaction may include 22°C to 48°C. In some embodiments, the temperature of the desorption reaction may include 24°C to 46°C. In some embodiments, the temperature of the desorption reaction may include 26°C to 44°C. In some embodiments, the temperature of the desorption reaction may include 28°C to 42°C. In some embodiments, the temperature of the desorption reaction may include 30°C to 40°C. In some embodiments, the temperature of the desorption reaction may include 31°C to 39°C.
  • the temperature of the desorption reaction may include 32°C to 38°C. In some embodiments, the temperature of the desorption reaction may include 33°C to 37°C. In some embodiments, the temperature of the desorption reaction may include 34°C to 36°C. In some embodiments, the temperature of the desorption reaction may include 35°C.
  • the first part of the third reaction product may include magnesium bicarbonate solution, and the second part may include heavy metal carbonate precipitation.
  • the third separation process may include filtration.
  • the third reaction product is filtered to obtain the above-mentioned first part and second part.
  • the third separation process can be implemented by a third separation device.
  • Step 140 Perform a first recovery treatment on the first part to obtain a reactant for preparing a wastewater treatment agent.
  • the first recovery process can be implemented by a first recovery device.
  • the first part may include a magnesium bicarbonate solution.
  • the magnesium bicarbonate solution can be heated to obtain a basic magnesium carbonate precipitate.
  • the heating temperature may be 50°C to 80°C.
  • the magnesium carbonate precipitate can be calcined to obtain product carbon dioxide gas and magnesium oxide solid, wherein the product carbon dioxide gas is circulated for the reactant in the above-mentioned third reaction process.
  • the temperature of the calcination treatment may be 600°C to 700°C.
  • the magnesium oxide solid can be subjected to a flue gas desulfurization reaction to obtain a magnesium sulfate solution.
  • magnesium oxide solids can be mixed with water to form a magnesium oxide slurry, and then the flue gas (for example, it can include at least one of sulfur dioxide and sulfur trioxide) and the magnesium oxide slurry are contacted in counter-current flow to make it fully react to produce Magnesium sulfite solution.
  • the flue gas may be contacted with the magnesium oxide slurry for multiple times (for example, two or three times) in counter-current flow, so that the sulfur dioxide and/or sulfur trioxide gas in the flue gas is fully absorbed, so that the treated The flue gas reaches the emission standard and can be discharged directly.
  • the content of particulate matter in the treated flue gas is 19 mg/m 3
  • the content of sulfur dioxide is 48 mg/m 3
  • the content of nitrogen oxides is 190 mg/m 3
  • the smoke blackness is 1 mg/m 3
  • the magnesium sulfite solution can undergo an oxidation reaction (for example, react with oxygen or air) to generate a magnesium sulfate solution.
  • Magnesium sulfate solution can be used as a reactant (ie, magnesium salt solution) for preparing the wastewater treatment agent.
  • the magnesium sulfate solution after the oxidation reaction may be subjected to solid-liquid separation, and the clear liquid obtained after filtration is used to prepare the reactant of the wastewater treatment agent.
  • Step 150 Perform a second recovery process on the second part to obtain a reactant for preparing heavy metals.
  • the second recovery process can be implemented by a second recovery device.
  • the second part may include heavy metal carbonate precipitation.
  • heavy metal carbonate precipitation can be recovered and smelted to complete the recovery and utilization of heavy metals.
  • Figure 2 is a schematic diagram of an exemplary product recovery device used in the preparation and use of wastewater treatment agents according to some embodiments of the present application.
  • the product recovery device used in the preparation and use of the wastewater treatment agent may include a first device, a second device, a third device, a first recovery device, and a second recovery device.
  • the first device can be used to obtain a wastewater treatment agent through the first reaction process.
  • the first device may include at least a first reaction device (for example, a bubble liquid film reactor) and a first separation device (for example, a filter).
  • the magnesium salt solution, the precipitant, and the coating agent can be separately introduced (for example, added by a metering pump) into the first reaction device at a preset flow rate, and the reaction is carried out under the first reaction conditions, and then the first reaction device is reacted under the first reaction condition.
  • the product salt solution and waste water treatment agent are obtained.
  • the inert gas is introduced into the first reaction device while the reactant is passed in.
  • the gas is dispersed into a stream of polygonal polyhedral bubbles.
  • the reactant is separated into a liquid film by the bubbles.
  • the bubbles are the dispersed phase and the liquid film is the continuous phase.
  • the reactants react in the liquid film to generate nano-capsule particles (ie, nano-wastewater treatment agent). Then it passes through the first separation device to obtain the product salt solution and the wastewater treatment agent. More descriptions of the first reaction process can be found elsewhere in this application, such as Figure 1 and its description.
  • the second device can be used to pass the wastewater treatment agent into the wastewater produced by the preparation of heavy metals, and obtain a second reaction product through the second reaction process, wherein the second reaction product at least includes the product after the wastewater treatment agent undergoes adsorption.
  • the second device may include at least a second reaction device (for example, an adsorption reactor) and a second separation device (for example, a filter).
  • the wastewater treatment agent for example, nano-magnesium hydroxide
  • the wastewater treatment agent can be passed into the wastewater generated by heavy metal smelting, and the wastewater treatment agent adsorbs heavy metal ions such as nickel, copper, cobalt, arsenic, cadmium, and lead in the wastewater.
  • the wastewater after adsorption (including the product after the adsorption of the wastewater treatment agent) is subjected to a second separation process to obtain the product after the adsorption of the wastewater treatment agent. More descriptions about the second reaction process can be found elsewhere in this application, such as Figure 1 and its description.
  • the third device can be used to process the second reaction product through a third reaction process to obtain a third reaction product, wherein the third reaction product at least includes a first part and a second part.
  • the third device may include at least a third reaction device (for example, a desorption reactor) and a third separation device (for example, a filter).
  • carbon dioxide gas can be introduced into the product of the wastewater treatment agent (for example, nano-magnesium hydroxide) after adsorption, and the desorption reaction can be carried out under the third reaction condition to obtain the third reaction product (including the first part and The second part, for example, magnesium bicarbonate solution and heavy metal carbonate precipitation).
  • the third reaction product is subjected to a third separation process through the third separation device to obtain the first part and the second part. More descriptions about the third reaction process can be found elsewhere in this application, such as Figure 1 and its description.
  • the first recovery device may be used to perform a first recovery treatment on the first part to obtain a reactant for preparing the wastewater treatment agent.
  • the first part may include a magnesium bicarbonate solution.
  • the first recovery device may include at least a first heating device (for example, a heating furnace), a calcining device (for example, a calcining furnace), and a flue gas desulfurization device.
  • the magnesium bicarbonate solution can be heated by the first heating device to obtain basic magnesium carbonate precipitation.
  • the basic magnesium carbonate precipitate is calcined by a calcining device to obtain product carbon dioxide gas and magnesium oxide solid, wherein the product carbon dioxide gas can be recycled for the reactant of the third reaction process.
  • the second recovery device can be used to perform a second recovery process on the second part to obtain a reactant for preparing heavy metals.
  • the second part may include heavy metal carbonate precipitation.
  • the second recovery device may include a smelting recovery device for recovering and smelting heavy metal carbonate precipitation to complete the recovery and utilization of heavy metals.
  • Fig. 3 is a schematic diagram of an exemplary product recovery method used in the preparation and use of wastewater treatment agents according to some embodiments of the present application.
  • the following description takes the nano-magnesium hydroxide wastewater treatment agent prepared from magnesium sulfate salt solution, sodium hydroxide solution and sodium oleate aqueous solution as an example, and is not intended to limit the protection scope of the present application.
  • Step 1 Take the magnesium sulfate salt solution with a concentration of 1mol/L, the sodium hydroxide solution with a concentration of 2mol/L and the sodium oleate solution with a concentration of 0.01mol/L at a temperature of 20 ⁇ 50°C, respectively with a metering pump
  • the first filter device F301 After filtering by the first filter device F301, 17.4g (ie, 17.4g/min) of nano-magnesium hydroxide wastewater treatment agent and 900mL (ie, 900mL/min) of sodium sulfate solution (wherein, the output of sodium sulfate is 42.6g/min).
  • the sodium sulfate solution can also be passed into the crystallization device R304 for low-temperature crystallization to obtain Glauber's salt.
  • Step 2 Pass 2L of heavy metal wastewater into the adsorption reactor R302.
  • the content of heavy metal in the heavy metal wastewater is respectively: Ni is 100mg/L, Co is 0mg/L, and Cu is 50mg/L.
  • the nano-magnesium hydroxide wastewater treatment agent that is, the product of the wastewater treatment agent after the adsorption action
  • 2L of the wastewater after the adsorption action are obtained.
  • the content of heavy metals in the wastewater after adsorption is as follows: Ni is 0.01 mg/L, Co is 0.01 mg/L, and Cu is 0.01 mg/L, which meets the standard for direct discharge and can be discharged directly.
  • Step 3 Mix 5.8g of the nano-magnesium hydroxide wastewater treatment agent after heavy metal adsorption with 0.2L of soft water, stir for 10min-60min to completely disperse the solids, and then pass the slurry pump into the desorption reactor R303. Introduce CO 2 gas, maintain the internal pressure of the desorption reactor R303 at 0.3 MPa to 0.5 MPa, hold for 1 h to 6 h, and carry out the pressure desorption reaction at a temperature of 20° C. to 50° C. Then, after filtering through the third filtering device F303, 0.2L of magnesium bicarbonate solution (wherein, containing 13.59g of magnesium bicarbonate) and 0.798g of heavy metal carbonate precipitate were obtained.
  • Step 4 Smelting and recovering 0.798 g of heavy metal carbonate precipitation through the smelting recovery device R305.
  • Step 5 Heat the magnesium bicarbonate solution to obtain 6-10 g of basic magnesium carbonate precipitate.
  • 6-10 g of basic magnesium carbonate precipitates are calcined in a calciner T301 to obtain product carbon dioxide gas and 3.75 g of magnesium oxide solid.
  • the product carbon dioxide gas can be stored in the collection tank F304 and can be used as the desorption gas in the desorption reactor R303.
  • Step 6 Mix 3.75g of magnesium oxide solid soft water to form a magnesium oxide slurry, pass the magnesium oxide slurry and flue gas into the flue gas desulfurization device T302, and make the flue gas and the magnesium oxide slurry perform multiple counter-flow contact to make the flue gas
  • the sulphur dioxide and/or sulphur trioxide gas in the gas is fully absorbed to produce magnesium sulfite solution.
  • the content of sulfur dioxide and sulfur trioxide in the treated flue gas reaches the emission standard and can be directly discharged.
  • the magnesium sulfite solution reacts with oxygen or air, and the magnesium sulfate solution can be used as the reactant magnesium sulfate salt solution for preparing the nano-magnesium hydroxide wastewater treatment agent.
  • Wastewater treatment agent can be prepared to adsorb heavy metal ions in the waste water produced by the preparation of heavy metals, so that it can meet the emission standards and protect the environment; (2) The product after the adsorption of the wastewater treatment agent can be recycled and treated to obtain the reactant for preparing the wastewater treatment agent, so that part of the product of the wastewater treatment agent can be recycled and save resources; (3) The wastewater treatment agent can be recycled The product after adsorption is recovered and processed to obtain a reactant for preparing heavy metals, so that the heavy metal ions in the wastewater can be recycled, protect the environment, and save resources.
  • the possible beneficial effects may be any one or a combination of the above, or any other beneficial effects that may be obtained.
  • this application uses specific words to describe the embodiments of the application.
  • “one embodiment”, “an embodiment”, and/or “some embodiments” mean a certain feature, structure, or characteristic related to at least one embodiment of the present application. Therefore, it should be emphasized and noted that “one embodiment” or “one embodiment” or “an alternative embodiment” mentioned twice or more in different positions in this specification does not necessarily refer to the same embodiment. .
  • some features, structures, or characteristics in one or more embodiments of the present application can be appropriately combined.
  • numbers describing the number of ingredients and attributes are used. It should be understood that such numbers used in the description of the embodiments use the modifiers "approximately”, “approximately” or “substantially” in some examples. Retouch. Unless otherwise stated, “approximately”, “approximately” or “substantially” indicates that the number is allowed to vary by ⁇ 20%.
  • the numerical parameters used in the specification and claims are approximate values, and the approximate values can be changed according to the required characteristics of individual embodiments. In some embodiments, the numerical parameter should consider the prescribed effective digits and adopt the method of general digit retention. Although the numerical ranges and parameters used to confirm the breadth of the range in some embodiments of the present application are approximate values, in specific embodiments, the setting of such numerical values is as accurate as possible within the feasible range.

Abstract

La présente invention concerne un procédé et un dispositif de récupération de produit utilisés dans la préparation et l'utilisation de processus d'un agent de traitement des eaux usées. Le procédé comprend les étapes consistant à : obtenir un agent de traitement des eaux usées au moyen d'un premier procédé de réaction ; introduire l'agent de traitement des eaux usées dans les eaux usées produites par la préparation d'un métal lourd, et obtenir un second produit de réaction au moyen d'un second procédé de réaction ; effectuer un traitement sur le deuxième produit de réaction au moyen d'un troisième processus de réaction pour obtenir un troisième produit de réaction, le troisième produit de réaction comprenant au moins une première partie et une deuxième partie ; effectuer un premier traitement de récupération sur la première partie pour obtenir un réactif pour préparer l'agent de traitement des eaux usées ; et réaliser un second traitement de récupération sur la seconde partie pour obtenir un réactif pour la préparation du métal lourd.
PCT/CN2020/091714 2020-05-22 2020-05-22 Procédé de récupération de produit et dispositif utilisé dans la préparation et processus d'utilisation d'un agent de traitement des eaux usées WO2021232391A1 (fr)

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CN202080099993.6A CN115443185A (zh) 2020-05-22 2020-05-22 一种用于废水处理剂制备和使用过程中的产物回收方法和装置

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