CN103623772A - Absorbent for removing and recovering liquid-phase mercury as well as preparation method and using method thereof - Google Patents
Absorbent for removing and recovering liquid-phase mercury as well as preparation method and using method thereof Download PDFInfo
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- CN103623772A CN103623772A CN201310633361.5A CN201310633361A CN103623772A CN 103623772 A CN103623772 A CN 103623772A CN 201310633361 A CN201310633361 A CN 201310633361A CN 103623772 A CN103623772 A CN 103623772A
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Abstract
The invention relates to an absorbent for removing and recovering liquid-phase mercury as well as a preparation method and using method thereof. According to the method, a material with high specific surface area and large pore volume is used as a carrier, and a sulfide or selenide nano absorbent is loaded on the carrier, so as to prepare an ion exchange nano mercury-removing absorbent with high adsorption capacity; a filter layer is prepared by adopting the nano mercury-removing absorbent to perform filtering processing on mercury ion contained waste liquid; the mercury ions in the liquid phase are absorbed to the absorbent by exchanging metal ions and mercury ions on the material, so as to achieve the purpose of removing liquid-phase mercury. The absorbent has the characteristics of high adsorption capacity and quick adsorption rate, and is suitable for waste water mercury-removing processing for coal-fired flue gas, non-ferrous metal metallurgical off-gas and other mercury related industry.
Description
Technical field
The invention belongs to a kind of waste water removal of mercury technology of field of environment protection, mainly by the exchange of the metal ion on adsorbent and mercury ion, the mercury ion in liquid phase is adsorbed onto on adsorbent, reach the object of the liquid phase removal of mercury.
Background technology
Owing to having the features such as persistence, easy animal migration, bioaccumulation and high toxicity, mercury pollution has caused the extensive concern of international community.In January, 2013 the United Nations's government-to-government talks committee has passed through the international control of a legally binding < < mercury pollution pact > >, will control in the world and reduce mercury emissions.China, because mercury emission is larger, will be faced with the severe pressure of honouring an agreement.Coal-fired flue-gas and non-ferrous metal metallurgy flue gas are considered to the anthropogenic discharge source of topmost two mercury.Therefore, the mercury control technology of these two industries receives much concern.In coal-fired flue-gas mercury control process, utilize oxidation means that the nonvalent mercury in flue gas is converted into divalence mercury, and then technology divalence mercury being absorbed by wet desulfurizing process is the technology that current research is the most popular.Although this technology can effectively reduce the Mercury In Coal Combustion Flue Gas concentration that is discharged into atmosphere, will certainly increase the mercury concentration in doctor solution, mercury pollution is transferred to water body from atmosphere.And in non-ferrous metal metallurgy flue gas purifying technique, generally all can have the technique of wet sprinkling to reduce flue-gas temperature.In wet sprinkling process, inevitably the divalence mercury in flue gas can be transferred in cleaning solution, be caused the mercury Enrichment in scrub raffinate.Also have other to relate to mercury industry, more or less all can produce some mercurous waste liquids.These mercurous waste liquids generally all can pass through some necessary treatment process before discharge, to remove heavy metal Hg wherein, also had much relevant research for this reason.As disclosing, patent CN201110042926.3 a kind ofly adds vulcanizing agent and composite assistant makes Hg in waste water
2+change the method for HgS particle precipitation into; The active carbon that patent CN96108886.9 discloses a kind of carrying alkali metal or alkaline earth sulfide is removed the method for the mercury and mercuric compounds in liquid hydrocarbon.But the method major part that in current waste liquid, mercury is removed is to utilize active carbon by mercury Adsorption, or utilizing sulfide to generate HgS with reacting of mercury precipitates to remove the mercury in liquid phase.But the adsorption capacity of adsorbent is generally smaller, if a large amount of use can cause operating cost high; And the method for utilizing sulfide to generate HgS is difficult to make mercury and sulfur cycle utilization; If mishandling, these methods may cause secondary pollution.
Summary of the invention
Object of the present invention is exactly in order to overcome the defect that above-mentioned prior art exists, to provide a kind of for removing and reclaim adsorbent and preparation method thereof and the using method of liquid phase mercury.
Object of the present invention can be achieved through the following technical solutions: a kind of for removing and reclaim the adsorbent of liquid phase mercury, it is characterized in that, this adsorbent is the nano adsorber loading on adsorbing agent carrier, the load capacity 1～50wt% of described nano adsorber on adsorbing agent carrier.
Described nano adsorber is metal sulfide or metal selenide nano adsorber.
Described adsorbing agent carrier is to have large specific area and the material of pore volume, comprises aluminium oxide, diatomite, molecular sieve, attapulgite, zeolite or active carbon.
For removing and reclaim a preparation method for the adsorbent of liquid phase mercury, it is characterized in that, comprise the following steps:
The first step, choose adsorbing agent carrier;
The nano adsorption agent solution of second step, configuration high concentration;
The 3rd step, adsorbing agent carrier be impregnated in the nano adsorption agent solution of high concentration, and by stirring nano adsorption agent solution, it is fully contacted with adsorbing agent carrier, utilize electrostatic attraction or chemical attachment attract a large amount of nano adsorbers to enter in the duct of adsorbing agent carrier and are carried on its surface;
The 4th step, until adsorbing agent carrier, with after nano adsorption agent solution mixing 1-3h, is separated adsorbing agent carrier by filtering, and is dried under room temperature from nano adsorption agent solution, obtains adsorbent.
The nano adsorption agent solution of described high concentration refers to the nano adsorption agent solution that one or more metal sulfides in zinc, iron, aluminium, titanium, manganese, calcium or selenides are configured to, and its concentration range is 0.1-10.0mol/L.
The speed of the stirring described in the 3rd step is 60 revs/min-300 revs/min.
The described dry temperature of step (4) is 15～30 ℃, by calcining 0.1-2.0h at dried adsorbing agent carrier 100-250 ℃, forms stable nanometer mercury-removing adsorbent.
A kind of for removing and reclaim the using method of the adsorbent of liquid phase mercury, it is characterized in that, comprise the following steps: a. is made into filter course by the nanometer mercury-removing adsorbent preparing the waste liquid containing mercury ion is carried out to filtration treatment, utilize metal ion on material and the exchange of mercury ion, mercury ion in liquid phase is adsorbed onto on adsorbent, reaches the object of the liquid phase removal of mercury; B. in the waste liquid after filtering, mercury content reaches certain value, nanometer mercury-removing adsorbent filter course is changed, and by special processing means, the mercury being adsorbed on adsorbent is carried out to desorb and recovery.
The described waste liquid containing mercury ion is with the flow velocity of 0.05-0.5m/s by the filter course of being made by nanometer mercury-removing adsorbent, and the time of staying of waste liquid in filter course is 10-120s; In waste liquid after filtering, mercury content reaches the 80-95% of relevant emission standards limit value, need nanometer mercury-removing adsorbent filter course to change, change the nanometer mercury-removing adsorbent of enriched mercury at 500-800 ℃ of temperature lower calcination, the mercuric sulphide of generation is desorbed, and the mercuryvapour desorbing condensation at subzero 20-50 ℃ temperature is reclaimed.
It is carrier that the inventive method be take the material of high-specific surface area and large pore volume, and sulfur loaded compound or selenides nano adsorber, make the ion-exchange nanometer mercury-removing adsorbent with high-adsorption-capacity thereon.During use, adsorbent is directly immersed and is rich in the solution of mercury ion, utilize metal ion on adsorbent and the exchange of mercury ion, the mercury ion in liquid phase is adsorbed onto on adsorbent, reach the object of the liquid phase removal of mercury.This adsorbent has the advantages that adsorption capacity is large, the rate of adsorption is fast, is suitable for coal-fired flue-gas, non-ferrous metal metallurgy flue gas and other waste water removal of mercury that relates to mercury industry and administers.
Compared with prior art, the present invention has following advantages:
1, the present invention utilizes the sources such as aluminium oxide to enrich low-cost material as carrier, and loaded metal sulfide nano adsorber is prepared the adsorbent of high-adsorption-capacity and speed, and price is very cheap;
2, by enrichment the adsorbent of high concentration mercury can focus on, by the method for desorption under high temperature and cryogenic condensation, realize the recovery resource of mercury.
3, the metal ion itself entering in liquid phase by ion-exchange in use procedure of the present invention is nontoxic, can not cause secondary pollution;
4, using method of the present invention is very convenient, only needs that nanometer mercury-removing adsorbent is made to filter course mercurous waste liquid is carried out to filtration treatment, gets final product the ionic mercury in efficient adsorption liquid phase.
5, the present invention is applicable to coal-fired flue-gas, non-ferrous metal metallurgy flue gas and other mercurous waste liquids that relates to mercury industry are removed and recycling.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Below embodiments of the invention are elaborated: the present embodiment is implemented under with technical solution of the present invention prerequisite, have provided detailed embodiment and specific operation process, but protection scope of the present invention is not limited to following embodiment.In the present invention program in implementation process, emphasis take that to realize divalence mercury efficient adsorption be target.
Embodiment 1
Taking 10g particle diameter is that 0.25mm activated alumina is standby as adsorbing agent carrier, configuration 100ml zinc sulfide nano sorbent reactions precursor solution (zinc chloride 0.5mol/L, thiocarbamide 2mol/L, mercaptopropionic acid 1.5mol/L).10g activated alumina is immersed in nano adsorber reacting precursor solution, was at 95 ℃ in temperature, with the rotating speeds of 100 revs/min, stirring reaction 1 hour.Load is had to the activated alumina of zinc sulphide by isolated by filtration out, under 25 degree room temperatures, be dried 5 hours, make zinc sulfide nano mercury-removing adsorbent.Through detecting, on activated alumina, the load capacity of nano adsorber is about 32%.Mercury-removing adsorbent specific area is about 367m
2/ g.
Embodiment 2
The molecular sieve that takes 10g particle diameter and be 0.25mm is standby as adsorbing agent carrier, configuration 100ml ferrous sulfide nano adsorber precursor solution (frerrous chloride 1mol/L, oleic acid 3mol/L, sulphur simple substance 3mol/L, octadecylene 100ml).10g molecular sieve is immersed in 100ml ferrous sulfide nano adsorber precursor solution, when temperature is 250 ℃, with the rotating speed stirring reactions of 500 revs/min 1 hour.There is the molecular sieve of iron sulfide to separate by filtration washing load, under 25 ℃ of room temperatures, be dried 5 hours, make ferrous sulfide mercury-removing adsorbent.Through detecting, on molecular sieve, the load capacity of nano adsorber is about 45%.Mercury-removing adsorbent specific area is 483m
2/ g.
Embodiment 3
The zinc sulfide nano adsorbent of embodiment 1 preparation is got to 0.1g and place in the mercuric chloride solution that 50mL concentration is 200mg/L, and stir with the speed of 400 revs/min.After 5 minutes, solution, by filtration treatment, is detected filtrate, result shows that in solution, the removal efficiency of mercury is greater than 99.9%, remaining ion concentration of mercury is less than 1 μ g/L.
Embodiment 4
For removing and reclaim preparation method and the using method of the adsorbent of liquid phase mercury, comprise the following steps:
The first step, choose there is large specific area and pore volume diatomite as adsorbing agent carrier;
The nano adsorption agent solution of second step, configuration high concentration: concentration is 0.1mol/L aluminum selenide solution.
The 3rd step, adsorbing agent carrier be impregnated in the reaction precursor liquid solution of metal selenide nano adsorber, and by stirring nano adsorption agent solution, it is fully contacted with adsorbing agent carrier, 60 revs/min of mixing speeds, utilize electrostatic attraction or chemical attachment attract a large amount of nano adsorbers to enter in the duct of adsorbing agent carrier and are carried on its surface;
The 4th step, by filtering, adsorbing agent carrier separated from reaction precursor liquid solution, and to be positioned under 15 ℃ of room temperatures dryly, to obtain nanometer mercury-removing adsorbent.The load capacity 1wt% of described nano adsorber on adsorbing agent carrier;
The 5th step, dried adsorbing agent carrier is calcined to 2.0h under 100 ℃ of conditions, form stable nanometer mercury-removing adsorbent;
The 6th step, the nanometer mercury-removing adsorbent preparing is made into filter course to carrying out filtration treatment containing the waste liquid of mercury ion, containing the waste liquid of mercury ion with the flow velocity of 0.1m/s by the filter course of being made by nanometer mercury-removing adsorbent, the time of staying of waste liquid in filter course is 30s; Utilize metal ion on material and the exchange of mercury ion, the mercury ion in liquid phase is adsorbed onto on adsorbent, reach the object of the liquid phase removal of mercury;
In the 7th step, the waste liquid after filtering, mercury content reaches the 80-95% of relevant emission standards limit value, need nanometer mercury-removing adsorbent filter course to change, change the adsorbent of enriched mercury at 500-800 ℃ of temperature lower calcination, the mercuric sulphide of generation is desorbed, and the mercuryvapour desorbing condensation at subzero 20-50 ℃ temperature is reclaimed.
Embodiment 5
For removing and reclaim preparation method and the using method of the adsorbent of liquid phase mercury, comprise the following steps:
The first step, choose there is large specific area and pore volume diatomite as adsorbing agent carrier;
The nano adsorption agent solution of second step, configuration high concentration: concentration is 10.0mol/L calcium selenide solution.
The 3rd step, adsorbing agent carrier be impregnated in the reaction precursor liquid solution of metal selenide nano adsorber, and by stirring nano adsorption agent solution, it is fully contacted with adsorbing agent carrier, 300 revs/min of mixing speeds, utilize electrostatic attraction or chemical attachment attract a large amount of nano adsorbers to enter in the duct of adsorbing agent carrier and are carried on its surface;
The 4th step, by filtering, adsorbing agent carrier separated from reaction precursor liquid solution, and to be positioned under 30 ℃ of room temperatures dryly, to obtain nanometer mercury-removing adsorbent.The load capacity 50wt% of described nano adsorber on adsorbing agent carrier;
The 5th step, dried adsorbing agent carrier is calcined to 0.1h under 250 ℃ of conditions, form stable nanometer mercury-removing adsorbent;
The 6th step, the nanometer mercury-removing adsorbent preparing is made into filter course to carrying out filtration treatment containing the waste liquid of mercury ion, containing the waste liquid of mercury ion with the flow velocity of 0.05m/s by the filter course of being made by nanometer mercury-removing adsorbent, the time of staying of waste liquid in filter course is 120s; Utilize metal ion on material and the exchange of mercury ion, the mercury ion in liquid phase is adsorbed onto on adsorbent, reach the object of the liquid phase removal of mercury;
In the 7th step, the waste liquid after filtering, mercury content reaches the 80-95% of relevant emission standards limit value, need nanometer mercury-removing adsorbent filter course to change, change the adsorbent of enriched mercury at 500-800 ℃ of temperature lower calcination, the mercuric sulphide of generation is desorbed, and the mercuryvapour desorbing condensation at subzero 20-50 ℃ temperature is reclaimed.
Claims (9)
1. for removing and reclaim an adsorbent for liquid phase mercury, it is characterized in that, this adsorbent is the nano adsorber loading on adsorbing agent carrier, the load capacity 1～50wt% of described nano adsorber on adsorbing agent carrier.
2. according to claim 1 a kind ofly it is characterized in that for removing and reclaim the adsorbent of liquid phase mercury, described nano adsorber is metal sulfide or metal selenide nano adsorber.
3. according to claim 1 a kind of for removing and reclaim the adsorbent of liquid phase mercury, it is characterized in that, described adsorbing agent carrier is to have large specific area and the material of pore volume, comprises aluminium oxide, diatomite, molecular sieve, attapulgite, zeolite or active carbon etc.
4. as claimed in claim 1ly for removing and reclaim a preparation method for the adsorbent of liquid phase mercury, it is characterized in that, comprise the following steps:
The first step, choose adsorbing agent carrier;
The nano adsorption agent solution of second step, configuration high concentration;
The 3rd step, adsorbing agent carrier be impregnated in the nano adsorption agent solution of high concentration, and by stirring nano adsorption agent solution, it is fully contacted with adsorbing agent carrier, utilize electrostatic attraction or chemical attachment attract a large amount of nano adsorbers to enter in the duct of adsorbing agent carrier and are carried on its surface;
The 4th step, until adsorbing agent carrier, with after nano adsorption agent solution mixing 1-3h, is separated adsorbing agent carrier by filtering, and is dried under room temperature from nano adsorption agent solution, obtains adsorbent.
5. according to claim 4 a kind of for removing and reclaim the preparation method of the adsorbent of liquid phase mercury, it is characterized in that, the nano adsorption agent solution of described high concentration refers to the nano adsorption agent solution that one or more metal sulfides in the harmless metals such as zinc, iron, aluminium, titanium, manganese, calcium or selenides are configured to, and its concentration range is 0.1-10.0mol/L.
6. according to claim 4 a kind ofly it is characterized in that for removing and reclaim the preparation method of the adsorbent of liquid phase mercury, the speed of the stirring described in the 3rd step is 60 revs/min-300 revs/min.
7. according to claim 4 a kind of for removing and reclaim the preparation method of the adsorbent of liquid phase mercury, it is characterized in that, the described dry temperature of step (4) is 15～30 ℃, by calcining 0.1-2.0h at dried adsorbing agent carrier 100-250 ℃, form stable nanometer mercury-removing adsorbent.
One kind as claimed in claim 1 for removing and reclaim the using method of the adsorbent of liquid phase mercury, it is characterized in that, comprise the following steps: a. is made into filter course by the nanometer mercury-removing adsorbent preparing the waste liquid containing mercury ion is carried out to filtration treatment, utilize metal ion on material and the exchange of mercury ion, mercury ion in liquid phase is adsorbed onto on adsorbent, reaches the object of the liquid phase removal of mercury; B. in the waste liquid after filtering, mercury content reaches certain value, nanometer mercury-removing adsorbent filter course is changed, and by special processing means, the mercury being adsorbed on adsorbent is carried out to desorb and recovery.
9. according to claim 8 a kind of for removing and reclaim the using method of the adsorbent of liquid phase mercury, it is characterized in that, the described waste liquid containing mercury ion is with the flow velocity of 0.05-0.5m/s by the filter course of being made by nanometer mercury-removing adsorbent, and the time of staying of waste liquid in filter course is 10-120s; In waste liquid after filtering, mercury content reaches the 80-95% of relevant emission standards limit value, need nanometer mercury-removing adsorbent filter course to change, change the nanometer mercury-removing adsorbent of enriched mercury at 500-800 ℃ of temperature lower calcination, the mercuric sulphide of generation is desorbed, and the mercuryvapour desorbing condensation at subzero 20-50 ℃ temperature is reclaimed.
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Cited By (12)
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| CN105854812A (en) * | 2016-04-20 | 2016-08-17 | 中建中环工程有限公司 | Liquid-phase mercury adsorbent and preparation method and application thereof |
| CN105950155A (en) * | 2016-06-27 | 2016-09-21 | 安徽金联地矿科技有限公司 | Soil conditioner with heavy metal polluted soil remediation function |
| CN109603410A (en) * | 2019-02-11 | 2019-04-12 | 中南大学 | A kind of method of Elemental Mercury in efficient removal flue gas |
| CN109762566A (en) * | 2018-12-29 | 2019-05-17 | 贵州大学 | A kind of mercury contaminated soil selenizing renovation agent and preparation method thereof |
| CN110170302A (en) * | 2019-05-31 | 2019-08-27 | 贵州重力科技环保有限公司 | The preparation method and material of grade nanometer selenium charcoal base demercuration sorbing material in situ and application |
| CN110302743A (en) * | 2019-06-24 | 2019-10-08 | 上海交通大学 | The preparation method of Adsorption of Radioactive nucleic and the concave convex rod bead of heavy metal ion |
| CN110756157A (en) * | 2019-11-08 | 2020-02-07 | 浙江大学 | Preparation and demercuration method of supported iron-based mercury adsorbent |
| CN110841590A (en) * | 2019-11-19 | 2020-02-28 | 江南大学 | Adsorbent for emergency treatment of indoor mercury leakage and preparation method thereof |
| CN112808228A (en) * | 2020-12-30 | 2021-05-18 | 华北电力大学（保定） | WSe2/halloysite nanotube demercuration adsorbent and preparation method and application thereof |
| CN113521979A (en) * | 2021-08-12 | 2021-10-22 | 上海交通大学 | Method for trapping mercury from sulfur-containing mercury-containing flue gas through chlorine selenium mercury deposition |
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| CN114259839A (en) * | 2021-12-24 | 2022-04-01 | 西安交通大学 | Coal-fired flue gas mercury recycling system and method utilizing selenium-containing adsorbent |
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| CN105854812A (en) * | 2016-04-20 | 2016-08-17 | 中建中环工程有限公司 | Liquid-phase mercury adsorbent and preparation method and application thereof |
| CN105950155A (en) * | 2016-06-27 | 2016-09-21 | 安徽金联地矿科技有限公司 | Soil conditioner with heavy metal polluted soil remediation function |
| CN109762566A (en) * | 2018-12-29 | 2019-05-17 | 贵州大学 | A kind of mercury contaminated soil selenizing renovation agent and preparation method thereof |
| CN109603410A (en) * | 2019-02-11 | 2019-04-12 | 中南大学 | A kind of method of Elemental Mercury in efficient removal flue gas |
| CN110170302A (en) * | 2019-05-31 | 2019-08-27 | 贵州重力科技环保有限公司 | The preparation method and material of grade nanometer selenium charcoal base demercuration sorbing material in situ and application |
| CN110302743A (en) * | 2019-06-24 | 2019-10-08 | 上海交通大学 | The preparation method of Adsorption of Radioactive nucleic and the concave convex rod bead of heavy metal ion |
| CN110756157A (en) * | 2019-11-08 | 2020-02-07 | 浙江大学 | Preparation and demercuration method of supported iron-based mercury adsorbent |
| CN110841590A (en) * | 2019-11-19 | 2020-02-28 | 江南大学 | Adsorbent for emergency treatment of indoor mercury leakage and preparation method thereof |
| CN112808228A (en) * | 2020-12-30 | 2021-05-18 | 华北电力大学（保定） | WSe2/halloysite nanotube demercuration adsorbent and preparation method and application thereof |
| CN113521979A (en) * | 2021-08-12 | 2021-10-22 | 上海交通大学 | Method for trapping mercury from sulfur-containing mercury-containing flue gas through chlorine selenium mercury deposition |
| CN113521979B (en) * | 2021-08-12 | 2024-01-12 | 上海交通大学 | Method for trapping mercury from sulfur-containing mercury-containing flue gas through chlorselenomel deposition |
| CN114045173A (en) * | 2021-11-10 | 2022-02-15 | 贵州大学 | Mercury-contaminated soil remediation agent and preparation method thereof |
| CN114259839A (en) * | 2021-12-24 | 2022-04-01 | 西安交通大学 | Coal-fired flue gas mercury recycling system and method utilizing selenium-containing adsorbent |
| CN114259839B (en) * | 2021-12-24 | 2023-02-07 | 西安交通大学 | Coal-fired flue gas mercury recycling system and method utilizing selenium-containing adsorbent |
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