CN109317089A - A kind of magnetic adsorptive material and its preparation and the method for handling waste water containing thallium - Google Patents
A kind of magnetic adsorptive material and its preparation and the method for handling waste water containing thallium Download PDFInfo
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- CN109317089A CN109317089A CN201811439179.5A CN201811439179A CN109317089A CN 109317089 A CN109317089 A CN 109317089A CN 201811439179 A CN201811439179 A CN 201811439179A CN 109317089 A CN109317089 A CN 109317089A
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- thallium
- adsorptive material
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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
- B01J20/28—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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Abstract
A kind of method the invention discloses magnetic adsorptive material and its preparation and for handling waste water containing thallium, the magnetic adsorptive material are manganese dioxide load Manganese Ferrite.Preparation method is that manganese acetate is dissolved in water, and citric acid dissolved dilution is added, and Manganese Ferrite is added, and is uniformly mixed, and can be obtained after dry, crushing, roasting.Method using magnetic adsorptive material processing waste water containing thallium is: manganese dioxide load Manganese Ferrite is added into industrial wastewater containing thallium for step 1, and magnetic adsorptive material adsorbs the thallium in industrial wastewater；The magnetic adsorptive material for being attached with thallium is sucked in step 2, externally-applied magnetic field；Step 3 is separated by solid-liquid separation, and supernatant is the processing water for removing thallium element；It is using magnetic adsorptive material recycling thallium element: nitre acid for adjusting pH value is added into the magnetic adsorptive material for be attached with thallium, externally-applied magnetic field attraction has been desorbed the magnetic adsorptive material finished, has been separated by solid-liquid separation, supernatant is exactly the enriching and recovering liquid for concentrating thallium element.
Description
Technical field
The invention belongs to environmental protection technical fields, and in particular to a kind of manganese dioxide (MnO2) load Manganese Ferrite
(MnFe2O4) magnetic adsorptive material and its preparation and application.
Background technique
Thallium (Tl) belongs to rare and scatter element, association in the metal sulfides such as Chang Tie, zinc, copper, also with organic matter knot in the earth's crust
Conjunction form is present in coalfield and petroleum.High-intensitive bio-toxicity is presented in thallium and its compound, to the toxicity of mammal
It is even stronger than heavy metals such as lead, mercury, it easily accumulates in vivo, excessively exposure can lead to nervous system, digestive system, skin to human body
The permanent poisoning injury such as skin, hair.
Currently, Mineral Resources in China demand increases, the low-temperature deposit exploitation scale for being associated with thallium constantly expands, and causes tight
The thallium pollution problem of weight.In recent years, a lot of thallium pollution events being affected occur for China.2010, Shaoguan Smelter was illegal
Waste water containing thallium is discharged, causes Guangdong Bei Jiang middle and upper reaches section thallium exceeded, influence is caused on the water supply in multiple cities.2013, extensively
Western He Jiang water body is by cadmium, thallium pollution, and exceeded 2.4 times of thallium.Water body thallium pollution problem increasingly attracts wide attention.U.S. environment is protected
Shield office (EPA) provides that thallium is no more than 0.14 mg/L in industrial discharge water, and thallium is no more than 2 μ g/L in Drinking Water, and China
" industrial wastewater thallium pollution object discharge standard " (DB 44/1989-2017) is, it is specified that the limit value of thallium concentration is 0.005mg/L, life
The content that thallium is defined in sanitary standard for drinking water is up to 0.12 μ g/L.
The administering method of water body containing thallium and soil has phytoremediation, ion-exchange, chemical precipitation method, solution extraction at present
It follows the example of, microbial technique method and absorption method etc..Wherein, absorption method processing thallium ion mainly utilizes porous structure material huge
Specific surface area and surface functional group abundant.Be compared with other methods, absorption method have selectivity it is good, at low cost, high-efficient,
The advantages that strong operability, therefore absorption method is the method for optimal processing waste water containing thallium.
But existing waste water removes thallium technology, does not have the enrichment, concentration and recycling function of thallium element, so that except thallium member
Cellulosic material becomes the higher hazardous waste of processing cost.In addition, existing waste water is high using reagent material input cost except thallium technology,
Except thallium effect is unstable.
Summary of the invention
For existing waste water except inherent technology defect existing for thallium technology, the technical problems to be solved by the invention are exactly to mention
For a kind of magnetic adsorptive material, its, separation of solid and liquid function admirable high to the absorption property of thallium, and recyclable regenerative are able to achieve useless
Water removes thallium and enriching and recovering thallium.The present invention also provides a kind of preparation methods of magnetic adsorptive material.The present invention provides one kind again
Use the method for magnetic adsorptive material processing waste water containing thallium.
For above-mentioned technical problem:
A kind of magnetic adsorptive material provided by the invention, the material be using manganese acetate as raw material, Manganese Ferrite particle be carrier, lemon
Acid is complexing agent, the manganese dioxide load Manganese Ferrite prepared using sol-gal process.
A kind of preparation method of above-mentioned magnetic adsorptive material provided by the invention: manganese acetate is dissolved in water, citric acid is added
Manganese Ferrite is added in dissolved dilution, is uniformly mixed, and after dry, crushing, roasting, obtains manganese dioxide load Manganese Ferrite.It was preparing
Cheng Zhong, citric acid are complexing agent, are complexed between citric acid group, and manganese ion can be chelated with citric acid, form gel network and include
Metal chelating it is fit；After heating, manganese citrate generates manganese dioxide.
A kind of method using above-mentioned magnetic adsorptive material processing waste water containing thallium provided by the invention, comprising the following steps:
Manganese dioxide load Manganese Ferrite is added into waste water containing thallium for step 1, and magnetic adsorptive material adsorbs the thallium in waste water；
The magnetic adsorptive material for being attached with thallium is sucked in step 2, externally-applied magnetic field；
Step 3 is separated by solid-liquid separation, and supernatant is the processing water for removing thallium element.
Further, thallium element is recycled using above-mentioned magnetic adsorptive material: the magnetic adsorptive material for being adsorbed with thallium is taken off
Attached, the thallium element of magnetic adsorptive material absorption is enriched with into desorption liquid.
The solution have the advantages that: the thallium ion in removal waste water can reach " the industrial wastewater thallium pollution object row of country
Put standard " standard of (DB 44/1989-2017), and thallium element can also be recycled.
Specific embodiment
Below with reference to embodiment, the invention will be further described:
Embodiment 1
Magnetic adsorptive material includes Manganese Ferrite and manganese dioxide, manganese dioxide (MnO2) and Manganese Ferrite (MnFe2O4) mass ratio be
1∶5。
The magnetic adsorptive material the preparation method comprises the following steps: by 12.10g(0.07mol) manganese acetate with 50ml distilled water dissolve, add
Enter 29.42g(0.14mol) lemon acid dissolution, be diluted with water 100ml, with ammonium hydroxide adjust solution pH value 5.0 ~ 6.0 it
Between, 30.45g Manganese Ferrite is added, stirs evenly, ultrasonic treatment 30min is uniformly mixed it, repaves and is put into baking oven in culture dish
Drying, through calcination process after grinding, obtains manganese dioxide load Manganese Ferrite, saves, spare, while performing the record of production.
Wastewater sample 1: selection thallium ion content is 950.0 μ g/L, the steel industry desulfurization wastewater of pH=6 ~ 7.
Preparatory work of experiment: it takes the magnetic adsorptive material of 10mg, 20mg, 30mg, 40mg and 50mg to be separately added into five and is equipped with
In the beaker of 100ml steel industry desulfurization wastewater, after standing 40min, the thallium ion content of five beakers clear liquid at the middle and upper levels is detected.
Testing result are as follows: the thallium ion content that gained supernatant liquor after 30mg and 40mg magnetic adsorptive material is handled is added is close, reaches
To 0.05 μ g/L hereinafter, and pH=7.0 ~ 8.5, then can determine added in every liter of steel industry desulfurization wastewater 350mg magnetism suction
Enclosure material is more suitable.
Using the method for the magnetic adsorptive material processing wastewater sample 1 of the present embodiment, according to the following steps:
The magnetic adsorptive material prepared is added in steel industry desulfurization wastewater and reacts by step 1, every liter of steel industry
The medical fluid added in desulfurization wastewater contains magnetic adsorptive material 350mg, reaction time 60min.
Step 2, after reaction, the magnetic adsorptive material for being attached with thallium is sucked in externally-applied magnetic field 0.2T；
Step 3 is separated by solid-liquid separation 30min, isolates the magnetic adsorptive material for being attached with thallium, the water that obtains that treated, removes additional
Magnetic field.
Water after detection processing, is detected by icp ms, and measuring thallium ion content is 0.039 μ
g/L 。
Further, thallium element is recycled to the above-mentioned magnetic adsorptive material for being attached with thallium: takes out the magnetic absorption for being attached with thallium
Material, nitre acid for adjusting pH is added into the magnetic adsorptive material for be attached with thallium to 1.5, desorption reaction 30min；Externally-applied magnetic field 0.2T
The magnetic adsorptive material finished has been desorbed in attraction, is separated by solid-liquid separation 30min, supernatant is exactly the enriching and recovering for concentrating thallium element
Liquid.
To the wastewater sample 1 of the present embodiment, enriching and recovering liquid thallium concentration is 47.31mg/L, and enriching and recovering rate is 99.6%.
Wastewater sample 2: certain southern untreated waste water of Xin Ye processing factory, waste water thallium content are 6.6mg/L.
Use the method for magnetic adsorptive material processing wastewater sample 3:
The magnetic adsorptive material prepared is added in the untreated waste water of Xin Ye processing factory and reacts by step 1, often
Rise added magnetic adsorptive material 3g, reaction time 60min in waste water.
Step 2, after reaction, the magnetic adsorptive material for being attached with thallium is sucked in externally-applied magnetic field 1.0T；
Step 3 is separated by solid-liquid separation 15min, isolates the magnetic adsorptive material for being attached with thallium, the water that obtains that treated, removes additional
Magnetic field.
Water after detection processing, measuring thallium ion content is 1.1 μ g/L.
Further, thallium element is recycled to the above-mentioned magnetic adsorptive material for being attached with thallium: takes out the magnetic absorption for being attached with thallium
Material, nitre acid for adjusting pH is added into the magnetic adsorptive material for be attached with thallium to 1.5, desorption reaction 30min；Externally-applied magnetic field 1.0T
The magnetic adsorptive material finished has been desorbed in attraction, is separated by solid-liquid separation 15min, supernatant is exactly the enriching and recovering for concentrating thallium element
Liquid.
To the wastewater sample 2 of the present embodiment, enriching and recovering liquid thallium concentration is 329.29mg/L, and enriching and recovering rate is 99.8%.
Wastewater sample 3: artificial modulation simulated wastewater containing thallium, thallium content are 10mg/L.
Use the method for magnetic adsorptive material processing wastewater sample 3:
The magnetic adsorptive material prepared is added in simulated wastewater and reacts by step 1, is added in every liter of simulated wastewater
Magnetic adsorptive material 150mg, reaction time 60min.
Step 2, after reaction, the magnetic adsorptive material for being attached with thallium is sucked in externally-applied magnetic field 2.0T；
Step 3 is separated by solid-liquid separation 10min, isolates the magnetic adsorptive material for being attached with thallium, the water that obtains that treated, removes additional
Magnetic field.
Water after detection processing, measuring thallium ion content is 1.2 μ g/L.
Further, thallium element is recycled to the above-mentioned magnetic adsorptive material for being attached with thallium: takes out the magnetic absorption for being attached with thallium
Material, nitre acid for adjusting pH is added into the magnetic adsorptive material for be attached with thallium to 1.5, desorption reaction 30min；Externally-applied magnetic field 2.0T
The magnetic adsorptive material finished has been desorbed in attraction, is separated by solid-liquid separation 10min, supernatant is exactly the enriching and recovering for concentrating thallium element
Liquid.
To the wastewater sample 3 of the present embodiment, enriching and recovering liquid thallium concentration is 498.94mg/L, and enriching and recovering rate is 99.8%.
Embodiment 2
Magnetic adsorptive material includes Manganese Ferrite and manganese dioxide, manganese dioxide (MnO2) and Manganese Ferrite (MnFe2O4) mass ratio be
1∶6。
The magnetic adsorptive material the preparation method comprises the following steps: by 12.10g(0.07mol) manganese acetate with 50ml distilled water dissolve, add
Enter 29.42g(0.14mol) lemon acid dissolution, be diluted with water 100ml, with ammonium hydroxide adjust solution pH value 5.0 ~ 6.0 it
Between, 36.54g Manganese Ferrite is added, stirs evenly, ultrasonic treatment 30min is uniformly mixed it, repaves and is put into baking oven in culture dish
Drying, through calcination process after grinding, obtains manganese dioxide load Manganese Ferrite, saves, spare, while performing the record of production.
To wastewater sample 1: same as Example 1 using magnetic adsorptive material processing wastewater sample 3.
Water after detection processing, measuring thallium ion content is 0.073 μ g/L.
To the wastewater sample 1 of the present embodiment, enriching and recovering liquid thallium concentration is 47.07mg/L, and enriching and recovering rate is 99.1%.
To wastewater sample 2: same as Example 1 using magnetic adsorptive material processing wastewater sample 3.
Water after detection processing, measuring thallium ion content is 1.5 μ g/L.
To the wastewater sample 2 of the present embodiment, enriching and recovering liquid thallium concentration is 327.94mg/L, and enriching and recovering rate is 99.4%.
To wastewater sample 3: same as Example 1 using magnetic adsorptive material processing wastewater sample 3.
Water after detection processing, measuring thallium ion content is 1.8 μ g/L.
To the wastewater sample 3 of the present embodiment, enriching and recovering liquid thallium concentration is 496.41mg/L, and enriching and recovering rate is 99.3%.
Claims (5)
1. a kind of magnetic adsorptive material, it is characterized in that: using manganese acetate as raw material, Manganese Ferrite particle be carrier, citric acid is complexing
Agent, the manganese dioxide load Manganese Ferrite prepared using sol-gal process.
2. magnetic adsorptive material according to claim 1, characterized in that titanium dioxide in the manganese dioxide load Manganese Ferrite
The mass values of manganese and Manganese Ferrite are 1: 5~6.
3. a kind of preparation method of magnetic adsorptive material as claimed in claim 1 or 2 is added it is characterized in that: manganese acetate is dissolved in water
Manganese Ferrite is added in citric acid dissolved dilution, is uniformly mixed, and after dry, crushing, roasting, obtains manganese dioxide load Manganese Ferrite.
4. a kind of method using as claimed in claim 1 or 22 magnetic adsorptive materials processing waste water containing thalliums, characterized in that including with
Lower step:
Manganese dioxide load Manganese Ferrite is added into waste water containing thallium for step 1, and magnetic adsorptive material adsorbs the thallium in waste water；
The magnetic adsorptive material for being attached with thallium is sucked in step 2, externally-applied magnetic field；
Step 3 is separated by solid-liquid separation, and supernatant is the processing water for removing thallium element.
5. the method for magnetic adsorptive material processing waste water containing thallium according to claim 4, it is characterized in that: to the magnetic for being attached with thallium
Property adsorbent material in be added acid for adjusting pH value, the magnetic adsorptive material finished has been desorbed in externally-applied magnetic field attraction, be separated by solid-liquid separation, on
Clear liquid is exactly the enriching and recovering liquid for concentrating thallium element.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124637A (en) * | 2019-05-30 | 2019-08-16 | 湖南省环境保护科学研究院 | A kind of waste water containing thallium adsorbent material and preparation method thereof |
| CN113083230A (en) * | 2021-04-02 | 2021-07-09 | 重庆大学 | Modified rice straw biochar adsorbing material, preparation method and application |
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| CN104150540A (en) * | 2014-07-14 | 2014-11-19 | 河南大学 | Heavy metal ion adsorbent ferrite hollow spheres MFe2O4 |
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| CN101186340A (en) * | 2007-11-28 | 2008-05-28 | 吴江市方霞企业信息咨询有限公司 | Method for preparing manganese dioxide by sol-gel |
| CN104150540A (en) * | 2014-07-14 | 2014-11-19 | 河南大学 | Heavy metal ion adsorbent ferrite hollow spheres MFe2O4 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124637A (en) * | 2019-05-30 | 2019-08-16 | 湖南省环境保护科学研究院 | A kind of waste water containing thallium adsorbent material and preparation method thereof |
| CN113083230A (en) * | 2021-04-02 | 2021-07-09 | 重庆大学 | Modified rice straw biochar adsorbing material, preparation method and application |
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