CN111020236A - Method for recovering waste mercury iodide reagent - Google Patents
Method for recovering waste mercury iodide reagent Download PDFInfo
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- CN111020236A CN111020236A CN201911206069.9A CN201911206069A CN111020236A CN 111020236 A CN111020236 A CN 111020236A CN 201911206069 A CN201911206069 A CN 201911206069A CN 111020236 A CN111020236 A CN 111020236A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B43/00—Obtaining mercury
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/37—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by reduction, e.g. hydrogenation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The technical key point of the method for recovering the waste mercury iodide reagent is that the method comprises the following steps: step 1, adding gelatin and hot water solution of waste mercury iodide into a reaction container, and stirring until the gelatin is completely dissolved; continuously adding formaldehyde and sodium hydroxide solution into the reaction container, and fully stirring; step 2, reacting for 2-3 h at 70-90 ℃, and naturally cooling to room temperature; step 3, sequentially filtering and recovering precipitated sodium formate crystals and separating reduced elemental mercury; and 4, condensing and adsorbing the mercury-containing waste gas to reach the standard, and then discharging the mercury-containing waste gas into the atmosphere. The problems of complex process, high cost and the like of the existing demercuration method are fundamentally solved.
Description
Technical Field
The invention relates to a demercuration method for reducing valence mercury by chemical change in waste mercury reagent, in particular to a recovery method of waste mercury iodide reagent, which is mainly suitable for wet regeneration of mercury, and the IPC classification number mainly related to the recovery method is A62D3/00 or A62D 3/37.
Background
In recent years, the national emphasis on the prevention and control of heavy metal pollution is increasing, and people pay more and more attention to the prevention and control of mercury pollution due to the effective notice of 'water guarantee about mercury' issued by the country in 8 months in 2017, and the pressure on the prevention and control of mercury pollution in the mercury-related industry is increasing. Particularly, the mercury smelting industry is strictly regulated by related national departments, and the industry faces huge environmental protection pressure.
Most of the existing wet mercury removal methods are oxidation methods, for example, as disclosed in application publication No. CN107569811A, "a method for removing mercury from dangerous waste residue containing mercury by full wet method with high efficiency", the method comprises oxidizing organic mercury and monovalent mercury into bivalent mercury by oxidizing agent, and then removing mercury by subsequent treatment. Namely, at least two steps of reaction are needed to reduce the mercury in the valence state into the mercury simple substance, the process is relatively complex, and the treatment cost is high.
Disclosure of Invention
The invention aims to provide a method for recovering a waste mercury iodide reagent, which fundamentally solves the problems of complex process, high cost and the like of the existing demercuration method.
In order to achieve the purpose, the invention provides the following technical scheme: the method for recovering the waste mercury iodide reagent comprises the following steps:
step 3, sequentially filtering and recovering precipitated sodium formate crystals and separating reduced elemental mercury;
and 4, condensing and adsorbing the mercury-containing waste gas to reach the standard, and then discharging the mercury-containing waste gas into the atmosphere.
Further, the molar ratio of the mercuric iodide to the formaldehyde solution to the sodium hydroxide solute is 1: 3.02-4.55: 6.82-9.10.
The invention also provides a system for recovering the waste mercury iodide reagent, which is characterized in that: comprises a reaction kettle component, a filtering device, a condenser and an active carbon adsorption device, wherein the condenser is connected with the active carbon adsorption device; the reaction kettle (1) assembly comprises a reaction kettle (1) with a water jacket (11), a cooling kettle (2) matched with the reaction kettle (1), and a water pump and a filter which are arranged on a water inlet pipe (23) of the reaction kettle (1), wherein the cooling kettle (2) comprises a kettle body with a concave middle part and an exhaust assembly (22) limited on the kettle body; a bearing seat (27) is arranged in the cooling kettle (2), the exhaust assembly (22) comprises an exhaust hood (224) which is limited at the top of the cooling kettle (2) and is provided with an exhaust port at the side part, a rotating shaft (223) which is limited through the exhaust hood (224) and the bearing seat (27), a plurality of hydraulic blades (222) which are arranged at the bottom of the rotating shaft (223), and helical blades (221) which are limited in the exhaust hood (224), and the outline of the hydraulic blades is matched with the shape of the inner wall of the cooling kettle (2); the upper end and the lower end of the cooling kettle (2) are respectively provided with a water inlet pipe (23) and a water outlet pipe (25) which are matched with the reaction kettle (1) along the tangential direction of the kettle body, and the other side of the bottom of the kettle body is provided with an emptying pipe (21).
The invention has the beneficial effects that: in the process, in the feeding sequence, only the deionized water solution of gelatin and mercury iodide, the formaldehyde solution and the sodium hydroxide solution are sequentially fed, and the feeding speed is not required to be controlled; in the feed ratio, only the relative feed ratio of formaldehyde, sodium hydroxide and mercury iodide needs to be controlled; in terms of reaction parameters, the whole reaction process can be completely controlled only by controlling the temperature and the time. Therefore, compared with other wet methods for recovering heavy metals, the process flow of the invention is simpler.
In the process, all the raw materials participating in the reaction belong to common substances sold in the market, the price is low, and the raw materials can be directly used without special pretreatment. Therefore, the processing cost of the invention is lower.
The reaction products of the invention can be recycled, for example, sodium formate (harmless to human body and having stimulation to eyes, respiratory system and skin) can be recycled after crystallization, separation and filtration, condensed mercury vapor is gathered to the bottom of the container, simple substance mercury at the bottom of the container can be separated and recycled after being directly discharged through a bottom pipeline, and waste gas is discharged after being adsorbed by activated carbon. The whole process has no three wastes discharge, thereby having good environmental affinity. Meanwhile, the waste of each substance is changed into valuable, and the treatment cost can be further reduced.
In conclusion, the method has the advantages of simple process flow, low treatment cost, high environmental affinity and the like, and can almost completely recover the mercury (the average recovery rate is more than 99%).
Drawings
FIG. 1 is a flow chart of a method for recovering a waste mercuric iodide reagent according to the present invention.
FIG. 2 is a schematic top view of a reactor according to the present invention.
FIG. 3 is a schematic diagram of a front view structure of a reaction kettle of the present invention.
Detailed Description
The following describes the present invention in detail with reference to the embodiments with reference to fig. 1 to 3. The method for recovering the waste mercury iodide reagent utilizes the process that the mercury iodide chemically reacts with formaldehyde and sodium hydroxide solution under the action of catalyst gelatin to obtain liquid elemental mercury, and the liquid elemental mercury is separated and extracted. And simultaneously, the generated mercury-containing waste gas is condensed and adsorbed to reach the emission standard.
It mainly involves the following reactions:
the addition amount of formaldehyde is 0.08-0.3 kg/kg HgI2The optimum range is 0.2 to 0.3kg/kgHgI2。
The addition amount of NaOH is 0.4-0.8 kg/kg HgI2The optimum range is 0.6 to 0.8kg/kgHgI2。
The reaction temperature is 50-90 ℃, and the optimal range is 70-80 ℃.
The reaction time is 0.5-3 h, and the optimal range is more than 2.5 h.
The gelatin is one of industrial gelatin, animal gelatin, etc., and has a protein content of above 82%.
The recovery method specifically comprises the following steps:
in the mixed solution, the molar ratio of mercury iodide, formaldehyde solution and sodium hydroxide solute is 1: 1.20-4.55: 4.55-9.10; the gelatin is selected from more than one of industrial gelatin with protein content of more than 82% or animal gelatin;
the input amount of the gelatin is 0.14-0.15 wt% of the total amount of the mixed solution;
step 3, sequentially filtering and recovering precipitated sodium formate crystals and separating reduced elemental mercury;
and 4, condensing and adsorbing the mercury-containing waste gas to reach the standard, and then discharging the mercury-containing waste gas into the atmosphere.
The method is preferably carried out in a system, wherein the waste mercury iodide reagent recovery system mainly comprises a reaction kettle assembly, a filtering device, a condenser and an active carbon adsorption device, and the condenser is connected with the active carbon adsorption device.
In the reaction kettle component, mercuric iodide, formaldehyde and sodium hydroxide are subjected to chemical reaction under the action of catalyst gelatin to generate metallic mercury, sodium formate, sodium iodide and the like. And naturally cooling and precipitating the mixture, passing the mixture through a filter to obtain crystallized sodium formate crystals and liquid metal mercury, and further purifying and recovering the sodium formate. The waste gas generated in the process enters a condenser to be cooled to further separate the metallic mercury, and finally the waste gas is subjected to activated carbon adsorption treatment and then is discharged after reaching the standard.
As shown in FIGS. 2 to 3, a cooling kettle is connected to the side of the reaction kettle 1 to improve the reaction efficiency, effectively save resources and reduce energy consumption. The reaction kettle 1 assembly comprises a reaction kettle 1 with a water jacket 11 and a stirring motor 12, a cooling kettle 2 matched with the reaction kettle 1, a water pump and a filter (not shown in the figure) arranged on a water inlet pipe 23 of the reaction kettle 1, and the cooling kettle 2 comprises a kettle body with an inwards concave middle part and an exhaust assembly 22 limited on the kettle body. The water pump sets up on outlet pipe 25 for let in the water jacket of reation kettle 1 with the cooling water in the cooling kettle, the filter setting is in the end of intaking of water pump, avoids impurity such as incrustation scale to get into the water pump.
The cooling kettle 2 is internally provided with a bearing seat 27, the exhaust assembly 22 comprises an exhaust hood 224 which is limited at the top of the cooling kettle 2 and is provided with an exhaust port at the side part, a rotating shaft 223 limited by the exhaust hood 224 and the bearing seat 27, a plurality of hydraulic blades 222 which are arranged at the bottom of the rotating shaft 223 and a helical blade 221 limited in the exhaust hood 224, and the outline of the hydraulic blades 222 is matched with the shape of the inner wall of the cooling kettle 2. To reduce weight, reduce drag, and reduce manufacturing costs, the water blade 222 and the helical blades are preferably non-metallic components, such as PVC, which is common. The cooling kettle is designed to be in a shape with a concave middle part and a blade structure with a wide upper part and a narrow lower part, and the reduction of water resistance at the bottom end of the blade is facilitated. Simultaneously, match blade outside profile and cauldron internal wall, help the maximize blade area, reach the biggest atress area under the prerequisite of limited impulsive force.
The upper end and the lower end of the cooling kettle 2 are respectively provided with a water inlet pipe 23 and a water outlet pipe 25 which are matched with the reaction kettle 1 along the tangential direction of the kettle body, and the other side of the bottom of the kettle body is provided with an emptying pipe 21. When the cross section of the kettle body is circular, the water inlet pipe and the water outlet pipe are communicated with the kettle body of the cooling kettle or the kettle body of the reaction kettle along a circular tangential direction, so that cooling water enters the water jacket of the reaction kettle 1 along the tangential water inlet pipe (not marked in the figure) through the water pump, water current rises to the water outlet pipe (not marked in the figure) of the reaction kettle 1 in a vortex manner, and finally, the water inlet pipe 23 of the cooling kettle sprays to the hydraulic blades 222 along the tangential direction of the kettle body, so that the rotating shaft 223 is driven, the spiral blades 221 are driven to rotate, and hot gas in the kettle body is led out. Utilize the cooling cauldron effectively to promote the heat radiating area of circulating water to cooperation exhaust assembly gets rid of evaporation state's cooling water fast, utilizes the liquid level in the level gauge 26 real time monitoring cooling cauldron, guarantees neither can show the increase blade resistance, can not influence the normal flow of circulating water yet. And meanwhile, by matching with pipeline components such as a liquid level sensor, an electric valve and the like, the automatic supply of cooling water through the water replenishing pipe 24 can be realized.
Above, through the conversion of the potential energy and the kinetic energy of circulating water self, effectively utilized the kinetic energy of circulating water, the operation of drive "unpowered" exhaust subassembly improves the radiating rate of cooling water, and then usable single-cycle pump lasts the use recirculated cooling water, has effectively practiced thrift cooling water quantity and electric energy.
In addition, on the basis of the technical scheme, the number of the reaction kettles can be further increased, namely a plurality of reaction kettles share the same cooling kettle, and if the diameter of the cooling kettle is larger, a plurality of water inlet pipes and water outlet pipes can be arranged in the circumferential direction; if the cooling kettle is small in size, a plurality of tee structures can be arranged on the water inlet pipe or the water outlet pipe to achieve the same function.
Application example 1
Adding 10g of waste mercuric iodide reagent (0.022 mol) and 1.5g of gelatin into 1L of deionized water at 50-90 ℃, stirring and dissolving, transferring into a 2L reaction kettle (a mercury release valve is arranged at the bottom of the reaction kettle), adding 2.7g of 37% industrial formaldehyde (solute is about 0.999g and 0.0333 mol) and 4g of NaOH (0.1 mol) into the mixture, fully stirring, and leaching at the temperature of 70 ℃ for reaction for 1 hour.
Naturally cooling to room temperature, precipitating sodium formate crystals, filtering to recover sodium formate, discharging mercury liquid precipitated at the lower part of the reaction kettle, and filtering to obtain metallic mercury with purity of 99.05%.
Application example 2
Adding 10g of waste mercuric iodide reagent (0.022 mol) and 1.5g of gelatin into 1L of deionized water at 50-90 ℃, stirring and dissolving, transferring into a 2L reaction kettle (a mercury release valve is arranged at the bottom of the reaction kettle), adding 5.4g of 37% industrial formaldehyde (solute is about 1.998g and 0.0666 mol) and 6g of NaOH (0.15 mol) into the mixture, fully stirring, and leaching at the temperature of 80 ℃ for reaction for 2.5 hours.
Naturally cooling to room temperature, precipitating sodium formate crystals, filtering to recover sodium formate, discharging mercury liquid at the lower part of the reaction kettle, and filtering to obtain metallic mercury with purity of 99.68%.
Application example 3
Adding 10g of waste mercuric iodide reagent (0.022 mol) and 1.5g of gelatin into 1L of deionized water at 50-90 ℃, stirring and dissolving, transferring into a 2L reaction kettle (a mercury release valve is arranged at the bottom of the reaction kettle), adding 8.1g of 37% industrial formaldehyde (solute about 2.997g and 0.0999 mol) and 8g of NaOH (0.2 mol) into the mixture, fully stirring, and leaching at 90 ℃ for reaction for 3 hours.
Naturally cooling to room temperature, precipitating sodium formate crystals, filtering to recover sodium formate, discharging mercury liquid at the lower part of the reaction kettle, and filtering to obtain metallic mercury with purity of 99.66%.
Physicochemical properties of the main compounds referred to herein:
mercury iodide under another name: mercuric iodide, mercuric diiodide, molecular formula: HgI2Appearance and properties: yellow crystals or powder, molecular weight: 454.40, melting point: 259 ℃, boiling point: 354 ℃, solubility: insoluble in water and acid, slightly soluble in absolute ethyl alcohol, easily soluble in solution of iodized alkali metal and sodium thiosulfate, and has the following density: relative density (water =1)6.09, CAS number: 7774-29-0.
Description of reference numerals:
1 reaction kettle
11 water jacket
12 stirring motor
2 Cooling kettle
21 evacuation pipe
22 exhaust assembly
221 helical blade
222 hydraulic blade
223 rotating shaft
224 exhaust hood
23 water inlet pipe
24 water supply pipe
25 water outlet pipe
26 liquid level meter
27 bearing seat.
Claims (3)
1. A method for recovering a waste mercury iodide reagent is characterized by comprising the following steps:
step 1, adding gelatin and hot water solution of waste mercury iodide into a reaction container, and stirring until the gelatin is completely dissolved; continuously adding formaldehyde and sodium hydroxide solution into the reaction container, and fully stirring; in the mixed solution, the molar ratio of mercury iodide, formaldehyde solution and sodium hydroxide solute is 1: 1.20-4.55: 4.55-9.10; the gelatin is selected from more than one of industrial gelatin with protein content of more than 82% or animal gelatin; the input amount of the gelatin is 0.14-0.15 wt% of the total amount of the mixed solution;
step 2, reacting for 2-3 h at 70-90 ℃, and naturally cooling to room temperature;
step 3, sequentially filtering and recovering precipitated sodium formate crystals and separating reduced elemental mercury;
and 4, condensing and adsorbing the mercury-containing waste gas to reach the standard, and then discharging the mercury-containing waste gas into the atmosphere.
2. The method for recovering a spent mercuric iodide reagent according to claim 1, wherein: the mol ratio of the mercuric iodide to the formaldehyde solution to the sodium hydroxide solute is 1: 3.02-4.55: 6.82-9.10.
3. The utility model provides a useless mercuric iodide reagent recovery system which characterized in that: comprises a reaction kettle component, a filtering device, a condenser and an active carbon adsorption device, wherein the condenser is connected with the active carbon adsorption device; the reaction kettle (1) assembly comprises a reaction kettle (1) with a water jacket (11), a cooling kettle (2) matched with the reaction kettle (1), and a water pump and a filter which are arranged on a water inlet pipe (23) of the reaction kettle (1), wherein the cooling kettle (2) comprises a kettle body with a concave middle part and an exhaust assembly (22) limited on the kettle body; a bearing seat (27) is arranged in the cooling kettle (2), the exhaust assembly (22) comprises an exhaust hood (224) which is limited at the top of the cooling kettle (2) and is provided with an exhaust port at the side part, a rotating shaft (223) which is limited through the exhaust hood (224) and the bearing seat (27), a plurality of hydraulic blades (222) which are arranged at the bottom of the rotating shaft (223), and helical blades (221) which are limited in the exhaust hood (224), and the outline of the hydraulic blades is matched with the shape of the inner wall of the cooling kettle (2); the upper end and the lower end of the cooling kettle (2) are respectively provided with a water inlet pipe (23) and a water outlet pipe (25) which are matched with the reaction kettle (1) along the tangential direction of the kettle body, and the other side of the bottom of the kettle body is provided with an emptying pipe (21).
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| CN201911206069.9A CN111020236A (en) | 2019-11-30 | 2019-11-30 | Method for recovering waste mercury iodide reagent |
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| CN201911206069.9A CN111020236A (en) | 2019-11-30 | 2019-11-30 | Method for recovering waste mercury iodide reagent |
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Citations (6)
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| CN203075937U (en) * | 2013-02-05 | 2013-07-24 | 浙江美诺华药物化学有限公司 | Cooling water circulating device of reaction kettle |
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2019
- 2019-11-30 CN CN201911206069.9A patent/CN111020236A/en active Pending
Patent Citations (6)
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| CN203075937U (en) * | 2013-02-05 | 2013-07-24 | 浙江美诺华药物化学有限公司 | Cooling water circulating device of reaction kettle |
| CN204638187U (en) * | 2015-01-23 | 2015-09-16 | 宁波大学 | A kind of with waste gas purification and the chemical reaction still reclaiming integrated apparatus |
| CN205392372U (en) * | 2016-02-15 | 2016-07-27 | 四川金江建材科技有限公司 | Reation kettle water circulating system |
| CN107741165A (en) * | 2017-11-15 | 2018-02-27 | 华北电力大学（保定） | One kind energy-conservation demisting dry and wet combination cooling tower |
| CN207970848U (en) * | 2018-01-11 | 2018-10-16 | 连云港三诺化工有限公司 | A kind of chemical products fine work cooling reactor |
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