CN106311186A - Preparation method of magnetic mercury removal adsorbent - Google Patents
Preparation method of magnetic mercury removal adsorbent Download PDFInfo
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- CN106311186A CN106311186A CN201610785011.4A CN201610785011A CN106311186A CN 106311186 A CN106311186 A CN 106311186A CN 201610785011 A CN201610785011 A CN 201610785011A CN 106311186 A CN106311186 A CN 106311186A
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- demercuration adsorbent
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a preparation method of a magnetic mercury removal adsorbent. The magnetic mercury removal adsorbent adopts magnetic Mn ferrite nanoparticles, carriers are added to the magnetic nanoparticles to improve the performance, and then the magnetic nanoparticles are subjected to amino-functionalization through modification and addition of a specific solution. According to the preparation method, corresponding salt is dissolved with ionized water, a strong base solution is added, stirred and heated, a reaction product is separated by means of an external magnetic field, stirred, heated and dried, and the amino-functionalized magnetic adsorbent prepared through modification is obtained and can acquire good mercury removal performance. Two modification processes are combined, and removal of mercury ions in a solution by the adsorbent can be improved effectively.
Description
Technical field
The invention belongs to industrial wastewater demercuration field, relate to a kind of by making it easier at activated carbon surface load magnetic source
Separate, magnetic source is increased amino group and improves the new adsorbent of mercury removal performance in solution, and preparation method thereof.
Background technology
Modern industry result in serious water resources crisis to the pollution of water, and the important component part that water pollutes is heavy metal
Pollute.Wherein hydrargyrum has higher volatility, will not be trapped by cleaner unit in flue gas, because the harm of especially severe is famous.Hydrargyrum has
Stronger toxicity, persistency, volatility, can form the mercury compound of other forms with long time sedimentation in water body, can pass through food
Chain enters human body, is enriched with in human body, and harm is very big, and it is relatively low and be difficult to control to compare other pollutant levels, it has also become state
Inside and outside the priority pollutants paid close attention to very much.
The common method processed heavy metal pollution in water at present has the sedimentation method, electrochemical process, biological restoration and absorption
Method (physical absorption/chemisorbed) etc..The process of the heavy metal containing sewage relatively low to concentration, absorption method can with adsorbent species very
Many, operation is simple and feasible, non-secondary pollution, and operating cost is low, therefore should be potential wide.The pass of hydrargyrum in absorption method removing solution
Key is the selection of adsorbent.Magnetic material has magnetic characteristic and corresponding Targeting Performance, and advantage is the most prominent.The work of outside magnetic field
Can be easily separated under with, and specific surface area is big, be to remove the good selection of mercury ion in sewage.
The present invention selects to use amino group and magnetic adsorptive material to combine, and expands specific surface area further and makes adsorbent
Internal diffusional resistance declines, it is possible to heavy metal ion in removing solution efficiently.
Summary of the invention
Technical problem: the present invention is directed to existing adsorbent to showing that metal mercury ions removing performance in water is not adequate
Shape, it is provided that a kind of utilize common Powdered Activated Carbon as carrier loaded magnetic ferrimanganic oxysome, modified increases ammonia by simple
High-efficiency mercury removal performance is obtained after base group.
Technical scheme: the preparation method of a kind of magnetic demercuration adsorbent of the present invention comprises the following steps:
1) with deionized water dissolving according to 1: the manganous salt of the elemental mole ratios example mixing of (2~2.5) and trivalent iron salt,
Or iron salt and trivalent iron salt, it is slowly added dropwise strong base solution, adds adsorbing agent carrier and jointly participate in reaction, control reaction temperature well,
Stirring mixed solution makes reaction carry out;
2) described mixed solution applying external magnetic field isolates wherein precipitate, cleans this precipitate with deionized water, afterwards
It is then added in ethanol solution;Disperseing the particle in ethanol solution with ultrasonic, add silane crosslinker, stirring mixing makes
Reaction uniformly, controls reaction temperature well;
3) utilize magnetic field separation to go out magnetic material, after cleaning-drying, i.e. make this demercuration adsorbent.
Wherein:
Step 1) described in highly basic be potassium hydroxide or sodium hydroxide, concentration 0.6~0.8mol/L, and strong base solution need
To be prepared by deionized water.Described adsorbing agent carrier is active carbon powder.Described reaction temperature needs to control in temperature 70
~90 DEG C, stir speed (S.S.) 420~480r/min, time needs 50~70 minutes.
Step 2) described in silane crosslinker can be selected for aminopropyl trimethoxysilane APTMS or aminopropyl-triethoxy
Silane APTES etc..Described reaction temperature needs to control at room temperature, stir speed (S.S.) 420~480r/min, the response time
5~7 hours.
Step 3) described in cleaning process use ethanol and deionized water that obtained magnetisable material is cleaned multiple times, exist afterwards
60~80 DEG C are dried 16~20 hours.
The mechanism of the present invention is to utilize the good magnetic characteristic of magnetic Nano material and corresponding Targeting Performance, ensures to inhale
Attached dose is easily isolated.But the magnetic of exposed nanoparticle and other physicochemical properties are vulnerable to destroy or oxidation, stability of material
Not ideal enough, so being carried on carbon based surfaces, then build selective absorption system by introducing specific function component, so
Both can promote adsorbent demercuration ability further, it can be made again easily separated.
Beneficial effect: the present invention compares with prior art, has the following advantages:
(1) the adsorbent demercuration efficiency that prepared by the present invention is high, and magnetic adsorbent particle has the advantage being easily isolated, has very
Good application prospect.
(2) present invention uses amino functional modified and strengthens the adsorbent self adsorption effect to mercury ion, and
Adsorption is not susceptible to the impact of other metal ions in solution, and modified scheme has preference to the removing of hydrargyrum.
(3) magnetic material prepared by inexpensively has prospect, good dispersion in water, preparation process simple possible.
Detailed description of the invention
The preparation method of a kind of modified magnetic solution demercuration adsorbent of the present invention comprises the following steps:
1) manganous salt mixed according to the elemental mole ratios example of 1: 2~2.5 with deionized water dissolving and trivalent iron salt, or
Iron salt and trivalent iron salt, be slowly added dropwise strong base solution, adds adsorbing agent carrier and jointly participates in reaction, controls reaction temperature well, stirs
Mixing mixed solution makes reaction carry out;
2) described mixed solution applying external magnetic field isolates wherein precipitate, cleans this precipitate with deionized water, afterwards
It is then added in ethanol solution;Disperseing the particle in ethanol solution with ultrasonic, add silane crosslinker, stirring mixing makes
Reaction uniformly, controls reaction condition well;
3) utilize magnetic field separation to go out magnetic material, after cleaning-drying, i.e. make this demercuration adsorbent.
In the preparation method of the present invention, highly basic available hydrogen potassium oxide or sodium hydroxide etc., concentration 0.6~0.8mol/L.For
Adsorbent distribution carrier can be Powdered Activated Carbon etc..The reaction generating magnetisable material needs the condition controlled: temperature needs control
Making temperature 70~90 DEG C, stir speed (S.S.) 420~480r/min, the time needs 50~70 minutes.Amino functional medicine is optional
With aminopropyl trimethoxysilane (APTMS), or the similar silane crosslinker such as aminopropyl triethoxysilane (APTES) is equal
Can.Modified-reaction at room temperature, stir speed (S.S.) 420~480r/min, response time 5~7 hours.Use ethanol and go from
Sub-water is cleaned multiple times obtained magnetisable material, is dried 16~20 hours at 60~80 DEG C afterwards.
Following case study on implementation is provided to more clearly express the purpose of the present invention, technical scheme and advantage.Should be appreciated that
Specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
Case study on implementation 1
Weigh 4g FeCl2·4H2O and 11g FeCl3·H2O, the concentrated hydrochloric acid 2ml adding 12mol/L are dissolved in 450ml
In deionized water, being then added drop-wise in the 0.75mol/L potassium hydroxide solution of 450ml by above solution, reaction temperature controls
80 DEG C, reaction stirred.Adding NACF, along with the carrying out of reaction, the black precipitate produced in reactant liquor is adsorbed
To activated carbon surface.The activated carbon having loaded nanoparticle is separated from reaction medium by recycling externally-applied magnetic field, spends
Ionized water cleans 3 times, and ethanol purge 2 times joins gains about 50ml in ethanol and deionized water mixed liquor, is diluted to
300ml.Add 1ml aminopropyl trimethoxysilane (APTMS), stir mixing under room temperature and make reaction uniform, after 6 hours.
Being separated from solution by adsorbent with centrifuge, ethanol and deionized water are cleaned multiple times, and the magnetic i.e. making modification after drying is molten
Loss of thick fluid mercury absorbent.
Case study on implementation 2
Use coprecipitation, ferrous sulfate and the iron chloride that molar ratio is 1: 2 is mixed, uses a certain amount of deionized water
Dissolved, be added thereto to active carbon powder afterwards.Control reaction temperature 80 DEG C, stir speed (S.S.) 500r/min, react 40min
After, externally-applied magnetic field separates, and after using deionized water to clean to neutral state, dries at 60 DEG C.Particle in dispersion soln, adds
Amino functional medicine, stirring mixing makes reaction uniform, controls reaction condition well.Utilize magnetic field separation to go out magnetic material, use second
Alcohol and deionized water are cleaned multiple times, and be dried 18 hours, i.e. make this demercuration adsorbent at 70 DEG C.
Embodiment 3:
After applicant selects manganese chloride prepared in embodiment 1 and iron chloride mixing, activated carbon is selected to do ferrum oxide
The carrier of particle, with the modified adsorbent of aminopropyl triethoxysilane, uses the mercuric chloride equipped with 0.1mg/L in the lab
The Adsorption of Mercury ion energy of the coupon inspection adsorbent of solution.The mercury solution made is placed in 12 coupons stand-by, point
Become 2 groups.First group of label marks 5min, 10min, 15min, 20min, 25min and 25min-blank, and wherein 25min-is blank
As blank group, weigh 10mg adsorbent 6 parts, for adding, first group removes the hydrargyrum/cadmium ion in solution;Second group of weighing
Adsorbent 5 parts, quality is 5mg, 10mg, 15mg, 20mg, 25mg, adds 0g/L and does not add blank group of adsorbent, dosage
The group response time is 10min.
The adsorbent weighed is added in each group of solution, according to the label time as the response time;After reaction in coupon
Adsorbent is disposed, and the solution stayed is for remaining hydrargyrum measurement of concetration.Permanent magnet is used to be taken out from test solution by magnetic adsorbent.
Use in HydraAA mercury analyzer detection solution not to be adsorbed fall the concentration value of hydrargyrum.Assist to measure with hydrargyrum mark liquid during measurement.Logical
Cross mark liquid curve and record deionized water and blank mercury solution concentration, accurately measure solution hydrargyrum after preparing more accurate mark liquid curve and contain
Amount.
After testing 25 minutes, adsorbent can remove the hydrargyrum of 80-90% in solution.When dosage reaches 0.5g/L, amino is repaiied
Decorations adsorbent just can remove the mercury ion of 60% in solution.When adsorbent dosage reaches 2.5g/L, two kinds of equal energy of adsorbent
Remove the metal ion of 90%.
Embodiment 4:
Optional embodiment 1,2 or this kind of demercuration adsorbent of other preparation, according to the experimental technique of embodiment 3, carried out
Solution demercuration is verified, can produce preferable removal effect.
Claims (7)
1. the preparation method of a magnetic demercuration adsorbent, it is characterised in that the method comprises the following steps:
1) with deionized water dissolving according to 1: the manganous salt of the elemental mole ratios example mixing of (2~2.5) and trivalent iron salt, or ferrum
Salt and trivalent iron salt, be slowly added dropwise strong base solution, adds adsorbing agent carrier and jointly participates in reaction, controls reaction temperature well, stirring
Mixed solution makes reaction carry out;
2) described mixed solution applying external magnetic field isolates wherein precipitate, cleans this precipitate with deionized water, adds
Enter in ethanol solution;Disperseing the particle in ethanol solution with ultrasonic, add silane crosslinker, stirring mixing makes reaction
Uniformly, reaction temperature is controlled well;
3) utilize magnetic field separation to go out magnetic material, after cleaning-drying, i.e. make this demercuration adsorbent.
The preparation method of a kind of magnetic demercuration adsorbent the most according to claim 1, it is characterised in that step 1) described in
Highly basic be potassium hydroxide or sodium hydroxide, concentration 0.6~0.8mol/L, and strong base solution need prepared by deionized water.
The preparation method of a kind of magnetic demercuration adsorbent the most according to claim 1, it is characterised in that step 1) described in
Adsorbing agent carrier be active carbon powder.
The preparation method of a kind of magnetic demercuration adsorbent the most according to claim 1, it is characterised in that step 1) described in
Reaction temperature needs to control temperature 70~90 DEG C, stir speed (S.S.) 420~480r/min, and the time needs 50~70 minutes.
The preparation method of a kind of magnetic demercuration adsorbent the most according to claim 1, it is characterised in that step 2) described in
Silane crosslinker can be selected for aminopropyl trimethoxysilane APTMS or aminopropyl triethoxysilane APTES.
The preparation method of a kind of magnetic demercuration adsorbent the most according to claim 1, it is characterised in that step 2) described in
Reaction temperature needs to control at room temperature, stir speed (S.S.) 420~480r/min, response time 5~7 hours.
The preparation method of a kind of magnetic demercuration adsorbent the most according to claim 1, it is characterised in that step 3) described in
Cleaning process uses ethanol and deionized water that obtained magnetisable material is cleaned multiple times, and is dried 16~20 at 60~80 DEG C afterwards little
Time.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106943998A (en) * | 2017-04-14 | 2017-07-14 | 成都信息工程大学 | A kind of preparation method for being used to remove to remove water the magnetic active carbon of Methylene Blue |
CN108940183A (en) * | 2018-08-07 | 2018-12-07 | 东北师范大学 | A method of magnetic adsorbent is prepared using water factory's ferrimanganic sludge as raw material |
CN109647336A (en) * | 2019-01-15 | 2019-04-19 | 合肥工业大学 | It is a kind of for efficiently removing the compound adsorbent and preparation method thereof of heavy metal ions in wastewater |
CN110538630A (en) * | 2019-08-27 | 2019-12-06 | 华南农业大学 | Acid-resistant camellia oleifera shell-based magnetic activated carbon and preparation method thereof |
CN114014642A (en) * | 2021-10-09 | 2022-02-08 | 国家能源集团科学技术研究院有限公司 | Manganese-cobalt ferrite nano material and preparation method and application thereof |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106943998A (en) * | 2017-04-14 | 2017-07-14 | 成都信息工程大学 | A kind of preparation method for being used to remove to remove water the magnetic active carbon of Methylene Blue |
CN108940183A (en) * | 2018-08-07 | 2018-12-07 | 东北师范大学 | A method of magnetic adsorbent is prepared using water factory's ferrimanganic sludge as raw material |
CN108940183B (en) * | 2018-08-07 | 2020-12-22 | 东北师范大学 | Method for preparing magnetic adsorbent by using waterworks ferro-manganese sludge as raw material |
CN109647336A (en) * | 2019-01-15 | 2019-04-19 | 合肥工业大学 | It is a kind of for efficiently removing the compound adsorbent and preparation method thereof of heavy metal ions in wastewater |
CN109647336B (en) * | 2019-01-15 | 2021-10-26 | 合肥工业大学 | Composite adsorbent for efficiently removing heavy metal ions in wastewater and preparation method thereof |
CN110538630A (en) * | 2019-08-27 | 2019-12-06 | 华南农业大学 | Acid-resistant camellia oleifera shell-based magnetic activated carbon and preparation method thereof |
CN114014642A (en) * | 2021-10-09 | 2022-02-08 | 国家能源集团科学技术研究院有限公司 | Manganese-cobalt ferrite nano material and preparation method and application thereof |
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