CN107952420A - A kind of preparation method and application for removing the sorbing material of anion in water removal - Google Patents
A kind of preparation method and application for removing the sorbing material of anion in water removal Download PDFInfo
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- CN107952420A CN107952420A CN201711212493.5A CN201711212493A CN107952420A CN 107952420 A CN107952420 A CN 107952420A CN 201711212493 A CN201711212493 A CN 201711212493A CN 107952420 A CN107952420 A CN 107952420A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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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
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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
- C02F2101/101—Sulfur compounds
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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
- C02F2101/12—Halogens or halogen-containing compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a kind of preparation method and application for removing the sorbing material of anion in water removal, belong to dirty water decontamination handles technical field in environmental protection.Using chitosan acetic acid solution as material, atoleine obtains crosslinked chitosan microsphere as crosslinking agent as organic dispersion medium, glutaraldehyde by lotion cross-linking method.The crosslinked chitosan microsphere adsorbent being prepared using this method has iodide ion good absorption property and recycles performance.Meanwhile the adsorbent also other adsorbable halide ions and oxygen-containing acid ion, and there is larger adsorption capacity.The present invention provides new technology reference for the removal of anion in waste water, and with good recycling and recycles effect.Raw material Nantural non-toxic needed for the present invention, and it is common be easy to get, cheap, preparation process is simple, and treatment effeciency is high, and the cycle is short, and regeneration treatment is convenient, is a kind of fertile absorber for handling anion in waste water.
Description
Technical field
Remove anion in water removal the invention discloses one kind, including the sorbing material of halide ion and oxygen-containing acid ion and
Its preparation method, belongs to dirty water decontamination handles technical field in environmental protection.
Background technology
The process that chemical products are produced and utilized can produce a variety of problem of environmental pollutions, such as discharge of wastewater.Industrial wastewater
Complicated component, common such as copper heavy metal ion, halogen and oxygen-containing acid group anionoid etc..Existing waste water is mainly with contained by processing
Based on cation, the research to anion is less.Removing chloride, fluorine, iodine and bromine are halogens common in waste water, such as directly
Discharge, not only pollutes environment and causes the wasting of resources.Iodine and its iodine radioisotope -131 have essentially from nuclear energy waste water
The shortcomings of specific activity is big, fission yield is high, half-life period is longer, ray energy is high.Such as cannot efficient process Spent Radioactive in time
Water, it will serious and long-term side effect is brought to environment.
At present, mainly there are ion-exchange-resin process, blowout method and absorption method to the processing method of anion in water, wherein from
Sub-exchange resin is to utilize one of main path of halide ion in ion exchange extraction natural water.Ion-exchange-resin process
Suitable for being extracted from the material liquid of low concentration, selectivity is preferable, but ion exchange process is relatively complicated, and sorbing material is easy
It is subject to other impurities in material liquid to disturb, resin regeneration process is complicated.Blowout method yield is higher, easy to operate, but to ion
Content requirement is stringenter, and cost of equipment is high, and energy source and power consumption is big, therefore is only suitable for mass producing.Absorption method technique
Process is relatively easy, and adsorbent is renewable to realize recycling, such as silver-based material, copper-based material, all multiple types of activated carbon class.
Although these adsorbents can remove anion in water body, with the rate of adsorption is fast, adsorption capacity is big, high selectivity and trace are handled
The features such as ability is strong, but there are it is expensive, cost input is big, and preparation process is complicated, the problems such as process cycle is longer.For
The problems such as waste water treatment process containing anion is complicated, costly, urgent need is a kind of easy to operate, environmental-friendly, of low cost
Processing contains such as method of iodide ion halogen and oxygen-containing acid radical anion waste water.
The method of the chitosan crosslinked microballoon processing anion waste water obtained using emulsification and cross linked the present invention provides a kind of,
And for being adsorbed in water containing Iodide Ion.It is close according to isotopic element ionic nature, present invention selection iodo- 127
Tested instead of radioactivity iodine -131, harm reduction.The invention avoids mentioned above as silver-based adsorbent is expensive, system
The shortcomings that standby complex process, while the adsorbent can also be used for adsorbing other halide ions and oxygen-containing acid ion, be in waste water
The processing of anion provides skill art reference.
The content of the invention
The shortcomings of present invention is directed to current silver-based, copper-based sorbing material cost is big, preparation process is complicated, there is provided one kind is gone
Anion in water removal, including chitosan microball sorbing material of halide anion and oxygen-containing acid ion and preparation method thereof.This
Invention is with the prices of raw materials are cheap, adsorption efficiency is high, the cycle is short, technique is simple, easy to control, absorption cost is controllable and can advise greatly
Mould is applied to the features such as production.
Technical scheme：
A kind of preparation method for removing the sorbing material of anion in water removal, step are as follows：
(1) at room temperature, add chitosan into acetic acid solution, stirring makes chitosan be stood overnight after fully dissolving；Its
In, the mass ratio of chitosan and acetic acid is 1-2, and the mass percent concentration of chitosan is 1-5%；
(2) add Span-80 into liquid paraffin, add the solution obtained by step (1), in 4000-8000 turn/
The homogeneous dispersion machine divided stirs 5-10 minutes；Wherein, Span-80 volumes are the 3-6% of paraffin volume, control paraffin volume and shell
Glycan liquor capacity ratio is 1-4；
(3) step (2) gains are warming up to 30-50 DEG C in water-bath, the glutaraldehyde that volume fraction is 50% is added dropwise, stirs
Mix reaction 4-6 it is small when；Wherein, it is 1-3 to control the molar ratio of glutaraldehyde and chitosan；
(4) by step (3) gains add EtOH Sonicate demulsification 0.5~1 it is small when, control ethanol and step (3) gains
Volume ratio is 1-3；
(5) washed respectively 2~3 times with ethanol and deionized water after step (4) gains are filtered；
(6) step (5) gains are dried in vacuo 12-24 hours to constant weight in 30-60 DEG C, it is micro- obtains a diameter of 0.9-1.5
The crosslinked chitosan microsphere of rice, is sorbing material.
Ethanol described in step (4) and step (5) is absolute ethyl alcohol.
Solvent used is deionized water in step (1).
Halide ion or oxygen-containing acid ion are adsorbed using crosslinked chitosan microsphere, step is as follows：
(1) adsorption process：
Crosslinked chitosan microsphere is added in the aqueous solution containing halide ion or oxygen-containing acid ion, in constant temperature oscillator
In, adsorption operations are carried out, remaining anion concentration is until balance in the water phase of measure analysis at regular intervals；
Adsorbance Qe is calculated using following formula：
In formula：The adsorbance of crosslinked chitosan microsphere, mgg when Qe is balance-1；Co and Ce is respectively anion in water phase
Initial concentration, mgL-1With concentration during balance, mgL-1；M be added crosslinked chitosan microsphere quality, g；V is liquid phase body
Product, L；
(2) crosslinked chitosan microsphere regenerative process
Crosslinked chitosan microsphere after adsorption equilibrium is washed repeatedly repeatedly with deionized water, surface moisture is blotted with filter paper
Dry afterwards to constant weight, used crosslinked chitosan microsphere is then added into the NaCl aqueous solutions that concentration is 0.5-2mol/L and is desorbed
In agent, keep crosslinked chitosan microsphere with desorb agent solution mass ratio be more than 200, constant temperature oscillation to measure solution in the moon from
The concentration of son no longer changes.
Beneficial effects of the present invention：The present invention proposes one kind and contains anion using crosslinked chitosan microsphere adsorption treatment
Waste water method, this method uses emulsification and cross linked means, selects glutaraldehyde as cross linker, obtain the shell with high-specific surface area
Glycan microballoon is used to adsorb.Compared with conventional anion adsorption method, the chitosan that the present invention chooses derives from a wealth of sources, and safe nothing
Poison；Chitosan microball preparation process is simple, and size is controllable, easily operated；Chitosan microball adsorbent has higher ratio table
Area and more uniform size, form ammonium ion in acidic aqueous solution using amino of chitosan and produce electric charge with anion
Between the characteristics of acting on, there is high-adsorption-capacity to halogen and oxygen-containing acid radical anion, and regenerative process is easy.
Brief description of the drawings
Fig. 1 is crosslinked chitosan microsphere SEM figures.
Fig. 2 is the repeat performance design sketch of adsorbent.
Embodiment
Illustrate the present invention with reference to instantiation, however, it should be understood that these examples are merely to illustrate the present invention without structure
Into limitation of the scope of the invention.
A kind of crosslinked chitosan microsphere sorbing material preparation method is as follows：
(1) chitosan powdered 2g is added in the acetic acid solution that 100mL mass concentrations are 1%, stirring makes chitosan
Fully dissolving；
(2) liquid paraffin 60mL is taken, 2mL Span-80 is first added, adds 20mL steps (1) gains, in
6300 revs/min of high speed dispersion homogenizer 8 minutes；
(3) step (2) gains are warming up to 50 DEG C in water-bath, the glutaraldehyde that 0.3mL volume fractions are 50% are added dropwise,
When stirring reaction 4 is small；
(4) product of step (3) reaction gained is demulsified, filtering, respectively with 300mL ethanol and 400mL deionization moisture
Chong Xi not be 2 times, until the pH value of cleaning solution reaches neutral.
(5) by step (4) gains, drying is no less than 12h in 50 DEG C of vacuum desiccators, obtains crosslinked chitosan microsphere.
With 4 specific experiments, the present invention will be described in detail below：
(1) the accurate crosslinked chitosan microsphere for weighing the above-mentioned preparations of 0.1g, it is 0.1mmol/ to add 100mL iodide ion concentrations
Vibrated in L aqueous solutions, at 20 DEG C 4 it is small when, 6000 revs/min centrifuge 10 minutes, survey its supernatant iodide ion concentration, in utilization
It is 12.5mg/g to state formula and calculate adsorbance, and removal effect reaches more than 95%, and processed waste water reaches surface water environment matter
Measure secondary standard.
(2) the accurate chitosan microball for weighing the above-mentioned preparations of 0.1g, it is 0.2mmol/L water to add 100mL bromide ion concentrations
In solution, when vibration 4 is small at 20 DEG C, 6000 revs/min centrifuge 10 minutes, survey its supernatant bromide ion concentration, utilization is above-mentioned
It is 14.4mg/g that formula, which calculates adsorbance, and removal effect reaches more than 90%, and processed waste water reaches surface water environment quality
Secondary standard.
(3) the accurate chitosan microball for weighing the above-mentioned preparations of 0.1g, adds 100mLSO4 2-Concentration is water-soluble for 0.1mmol/L
In liquid, its supernatant SO is surveyed4 2-Ion concentration, it is 9.2mg/g to calculate adsorbance using above-mentioned formula, and removal effect reaches 95%
More than, and processed waste water reaches surface water environment quality secondary standard.
(4) the accurate chitosan microball for weighing the above-mentioned preparations of 0.1g, adds 100mL iodide ions, sulfate radical, bromide ion, fluorine
Ion concentration is respectively in the mixed solution of 0.1mmol/L, surveys each ion concentration of its supernatant, and absorption is calculated using above-mentioned formula
Measure and be:38.1mg/g、13.5mg/g、6.7mg/g、2.5mg/g.
Claims (4)
1. a kind of preparation method for removing the sorbing material of anion in water removal, it is characterised in that step is as follows：
(1) at room temperature, add chitosan into acetic acid solution, stirring makes chitosan be stood overnight after fully dissolving；Wherein, shell
The mass ratio of glycan and acetic acid is 1-2, and the mass percent concentration of chitosan is 1-5%；
(2) Span-80 is added into liquid paraffin, the solution obtained by step (1) is added, in 4000-8000 revs/min
Homogeneous dispersion machine stirs 5-10 minutes；Wherein, Span-80 volumes are the 3-6% of paraffin volume, control paraffin volume and chitosan
Liquor capacity ratio is 1-4；
(3) step (2) gains are warming up to 30-50 DEG C in water-bath, the glutaraldehyde that volume fraction is 50% is added dropwise, stirring is anti-
When answering 4-6 small；Wherein, it is 1-3 to control the molar ratio of glutaraldehyde and chitosan；
(4) by step (3) gains add EtOH Sonicate demulsification 0.5~1 it is small when, control ethanol and step (3) gains volume
Than for 1-3；
(5) washed respectively 2~3 times with ethanol and deionized water after step (4) gains are filtered；
(6) step (5) gains are dried in vacuo 12-24 hours to constant weight in 30-60 DEG C, obtained 0.9-1.5 microns a diameter of
Crosslinked chitosan microsphere, is sorbing material.
2. preparation method according to claim 1, it is characterised in that the ethanol described in step (4) and step (5) is
Absolute ethyl alcohol.
3. preparation method according to claim 1 or 2, it is characterised in that solvent used is deionization in step (1)
Water.
4. the application for the sorbing material that any preparation methods of claim 1-3 obtain, it is characterised in that using crosslinking shell
Glycan microballoon adsorbs halide ion or oxygen-containing acid ion, and step is as follows：
(1) adsorption process：
Crosslinked chitosan microsphere is added in the aqueous solution containing halide ion or oxygen-containing acid ion, in constant temperature oscillator,
Adsorption operations are carried out, remaining anion concentration is until balance in the water phase of measure analysis at regular intervals；
Adsorbance Qe is calculated using following formula：
<mrow>
<mi>Q</mi>
<mi>e</mi>
<mo>=</mo>
<mfrac>
<mrow>
<mo>(</mo>
<mi>C</mi>
<mi>o</mi>
<mo>-</mo>
<mi>C</mi>
<mi>e</mi>
<mo>)</mo>
<mi>V</mi>
</mrow>
<mi>m</mi>
</mfrac>
</mrow>
In formula：The adsorbance of crosslinked chitosan microsphere, mgg when Qe is balance-1；Co and Ce is respectively the first of anion in water phase
Beginning concentration, mgL-1With concentration during balance, mgL-1；M be added crosslinked chitosan microsphere quality, g；V is liquid phase volume,
L；
(2) crosslinked chitosan microsphere regenerative process
Crosslinked chitosan microsphere after adsorption equilibrium is washed repeatedly repeatedly with deionized water, is done after blotting surface moisture with filter paper
It is dry to constant weight, used crosslinked chitosan microsphere is then added into the NaCl aqueous solution strippants that concentration is 0.5-2mol/L
In, it with the mass ratio for desorbing agent solution is more than 200 to keep crosslinked chitosan microsphere, and constant temperature oscillation is to measuring anions
Concentration no longer change.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704620A (en) * | 2018-07-02 | 2018-10-26 | 大连理工大学 | The preparation method and application of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water |
| CN108854987A (en) * | 2018-07-02 | 2018-11-23 | 大连理工大学 | The preparation method and application of iodide ion adsorbent material in a kind of waste water |
| CN109794227A (en) * | 2019-03-11 | 2019-05-24 | 大连理工大学 | The preparation method of the adsorbent material of bromoiodide in a kind of removal waste water |
| CN113996267A (en) * | 2021-11-23 | 2022-02-01 | 西南科技大学 | Preparation method of silicon-based fibrofelt-bismuth-based composite material and application of silicon-based fibrofelt-bismuth-based composite material in radioactive iodine adsorption |
| CN114015300A (en) * | 2021-10-25 | 2022-02-08 | 华麟海(海南)新材料科技有限公司 | Concrete protective coating capable of sterilizing and adsorbing sulfate ions and preparation method thereof |
| CN115487790A (en) * | 2022-10-25 | 2022-12-20 | 中国科学院生态环境研究中心 | Method for preparing adsorption desalting material from waste plastic |
| CN116328742A (en) * | 2023-04-27 | 2023-06-27 | 大连理工大学 | Core-shell magnetic molecularly imprinted polymer material, preparation method and application |
| CN117696018A (en) * | 2023-12-29 | 2024-03-15 | 苏州见远检测技术有限公司 | Preparation method of pretreatment filter medium for removing residual chlorine in tap water |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704620A (en) * | 2018-07-02 | 2018-10-26 | 大连理工大学 | The preparation method and application of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water |
| CN108854987A (en) * | 2018-07-02 | 2018-11-23 | 大连理工大学 | The preparation method and application of iodide ion adsorbent material in a kind of waste water |
| CN108704620B (en) * | 2018-07-02 | 2021-04-20 | 大连理工大学 | Preparation method and application of chitosan/hydrophobic montmorillonite adsorbing material for treating anions in wastewater |
| CN109794227A (en) * | 2019-03-11 | 2019-05-24 | 大连理工大学 | The preparation method of the adsorbent material of bromoiodide in a kind of removal waste water |
| CN109794227B (en) * | 2019-03-11 | 2022-04-12 | 大连理工大学 | Preparation method of adsorbing material for removing bromine iodide in wastewater |
| CN114015300A (en) * | 2021-10-25 | 2022-02-08 | 华麟海(海南)新材料科技有限公司 | Concrete protective coating capable of sterilizing and adsorbing sulfate ions and preparation method thereof |
| CN114015300B (en) * | 2021-10-25 | 2023-10-13 | 华麟海(海南)新材料科技有限公司 | Concrete protective coating capable of sterilizing and adsorbing sulfate ions and preparation method thereof |
| CN113996267A (en) * | 2021-11-23 | 2022-02-01 | 西南科技大学 | Preparation method of silicon-based fibrofelt-bismuth-based composite material and application of silicon-based fibrofelt-bismuth-based composite material in radioactive iodine adsorption |
| CN113996267B (en) * | 2021-11-23 | 2023-08-11 | 西南科技大学 | Preparation method of silicon-based fiber felt-bismuth-based composite material and application of silicon-based fiber felt-bismuth-based composite material in radioactive iodine adsorption |
| CN115487790A (en) * | 2022-10-25 | 2022-12-20 | 中国科学院生态环境研究中心 | Method for preparing adsorption desalting material from waste plastic |
| CN116328742A (en) * | 2023-04-27 | 2023-06-27 | 大连理工大学 | Core-shell magnetic molecularly imprinted polymer material, preparation method and application |
| CN117696018A (en) * | 2023-12-29 | 2024-03-15 | 苏州见远检测技术有限公司 | Preparation method of pretreatment filter medium for removing residual chlorine in tap water |
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