CN108704620A - The preparation method and application of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water - Google Patents
The preparation method and application of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water Download PDFInfo
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- CN108704620A CN108704620A CN201810709321.7A CN201810709321A CN108704620A CN 108704620 A CN108704620 A CN 108704620A CN 201810709321 A CN201810709321 A CN 201810709321A CN 108704620 A CN108704620 A CN 108704620A
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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
- B01J20/12—Naturally occurring clays or bleaching earth
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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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- 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
- 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
- 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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Abstract
The invention discloses a kind of preparation method and applications of chitosan/hydrophobic montmorillonite sorbing material of anion in processing waste water, belong to dirty water decontamination handles technical field in environmental protection.Using hydrophobically modified montmorillonite particle as emulsion stabilizer, using chitosan acetic acid solution as inner aqueous phase, atoleine obtains chitosan/montmorillonite microballoon as organic dispersion medium, glutaraldehyde as crosslinking agent, by lotion cross-linking method.The chitosan being prepared using this method/montmorillonite microsphere adsorbing agent has good absorption property and adsorption capacity to anion in water, and the system after hydrophobically modified is easier to be separated from the water.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 period is short, and regeneration treatment is convenient, is a kind of fertile absorber for handling anion in waste water.
Description
Technical field
The invention discloses a kind of preparation methods of chitosan/hydrophobic montmorillonite sorbing material of anion in processing waste water
And application, belong to dirty water decontamination handles technical field in environmental protection.
Background technology
Wastewater treatment is one of environmental pollution key problems-solving.Industrial wastewater complicated component, often containing the huge sum of money such as copper
Belong to ion, halogen and oxygen-containing acid group anionoid etc..Different valence state anion in waste water, such as halogen and chromate ion
Deng there is certain application value, if direct emission, not only pollute and environment and result in waste of resources.
By taking the iodine waste water of one of halogen as an example, such waste water is typically derived from nuclear industry, existing treatment technology, as ion is handed over
Resin method, cupric iodide method, blowout method etc. are changed, the effect for handling iodine is different.Ion-exchange-resin process is suitable for from low concentration
Material liquid in carry iodine, and the selectivity of adsorbent is good, but adsorbent is easy to be interfered by other impurities in material liquid, mistake
Journey is relatively complicated.Iodate process for copper is relative complex, and organic efficiency is not high.Blowout method yield is higher, easy to operate, but contains to iodine
Amount requirement is stringenter, and cost of equipment is high, and energy source and power consumption is big, is generally adapted large-scale production.Absorption method technical process
It is relatively easy, the rate of adsorption is fast, adsorption capacity is big and trace processing capacity is strong, have in processing anion waste water certain excellent
Gesture.
The present invention prepares chitosan/hydrophobic montmorillonite crosslinked microsphere by emulsion-crosslinking method, uses it in absorption water not
Same anion.The deficiencies of complicated the invention avoids traditional handicraft, the removal for anion in waste water provide Technical Reference.
Invention content
The shortcomings of present invention is directed to current silver-based, copper-based sorbing material cost is big, preparation process is complicated, provides one kind and goes
Except the method for anion in waste water.The present invention is with the prices of raw materials are cheap, adsorption efficiency is high, the period is short, simple for process, easily-controllable
System, absorption cost it is controllable and can large-scale application in the production the features such as.
Technical scheme of the present invention：
The preparation method of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water, steps are as follows：
(1) preparation of hydrophobically modified montmorillonite particle
Aquation 4-6h at being 40-60 DEG C in temperature by the montmorillonite slurry of a concentration of 3-5% of w/v；It will be equivalent to montmorillonite
It is ethyl alcohol that the modifying agent dioctadecyl dimethyl ammonium chloride of 1.0CEC~8.0CEC, which is dissolved in ethanol water in ethanol water,
Volume ratio with water is 3:1-1:1, solution is starched in the montmorillonite being added after aquation, reacts 4-6h；Stop reaction, centrifuge, receives
Collection precipitation；It filters, filter cake is collected in ethanol water washing, dries 12-24h to get the montmorillonite particle of hydrophobically modified；
(2) preparation of chitosan-acetic acid solution
At room temperature, the chitosan of a mass parts is added in the acetic acid solution of a concentration of 0.1-2% of v/v, stirring keeps shell poly-
It is stood overnight after sugared fully dissolving；
(3) preparation of Pickering lotions
Step (1) gains are scattered according to a concentration of 2-5% of w/v in atoleine, stirring for 24 hours, keeps particle abundant
Dispersion；Under 5000-8000rpm homogenous disperses, by the acetum of the chitosan of step (2) by volume 1:1-1:3 are added
In aforesaid liquid paraffin, emulsification pretreatment 10-15min obtains Pickering lotions；
(4) preparation of chitosan/hydrophobic montmorillonite microballoon
Pickering lotions obtained by step (3) are warming up to 30-50 DEG C in water-bath, appropriate volume score, which is added dropwise, is
50% glutaraldehyde is stirred to react 4-6 hours, by gains be added EtOH Sonicate be demulsified 0.5-1 hour, after filtering use ethyl alcohol and
Deionized water is washed 2-3 times respectively, after freezing, 12-24 hours is dried in vacuo in 20-30 DEG C to constant weight, obtains chitosan/hydrophobic illiteracy
De- soil microballoon.
The ethyl alcohol is absolute ethyl alcohol；
The solvent is deionized water.
The cross-linked chitosan obtained using the method for the present invention/hydrophobic montmorillonite microballoon adsorbs anion：
(1) adsorption process：
The adsorbent for weighing 5 parts of above-mentioned preparations of 0.1g respectively is added in 100mL anionic water solution in constant temperature oscillator
In, adsorption operations are carried out under constant temperature oscillation.Survivor ion concentration in analysis water phase is measured at regular intervals until balance.
Adsorbance (Qe) is calculated using following formula
Adsorbance (the mmolg of chitosan/hydrophobic montmorillonite microballoon when Qe is balance in formula-1)；Co and Ce is respectively water
Initial concentration (the mmolL of anion in phase-1) and concentration (mmolL when balance-1)；M is added adsorbent mass (g)；V
For liquid phase volume (L).
(2) adsorbent reactivation process
Microballoon after adsorption equilibrium is washed repeatedly repeatedly with deionized water, is dried to perseverance after blotting surface moisture with filter paper
Weight, is then added into the NaCl aqueous solution strippants of a certain amount of (100-500mL).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 a kind of cloudy using chitosan/hydrophobic montmorillonite microballoon adsorption treatment
The method of ion waste water, this method use emulsification and cross linked means, select glutaraldehyde as cross linker, obtain having high-specific surface area
Chitosan/hydrophobic montmorillonite microballoon is for adsorbing.Compared with conventional anion processing method, chitosan and illiteracy that the present invention chooses
De- soil derives from a wealth of sources, and safe and non-toxic；Adsorbent preparation process is simple, do not introduce metal ion, surfactant cause it is secondary
Pollution, and size is controllable, it is easily operated；Using chitosan and modified montmorillonoid amino protonated in acidic aqueous solution with it is cloudy from
The characteristics of being acted between son generation charge, has compared with high-adsorption-capacity anion, and regenerative process is easy.
Description of the drawings
Fig. 1 is the electron microscope for handling chitosan/hydrophobic montmorillonite sorbing material of anion in waste water of the present invention.
Fig. 2 is the regenerability for handling chitosan/hydrophobic montmorillonite sorbing material of anion in waste water and changing with number
Phenogram.
Specific implementation mode
Illustrate the present invention with reference to specific example, however, it should be understood that these examples are merely to illustrate the present invention without structure
At limitation of the scope of the invention.
A kind of cross-linked chitosan/hydrophobic montmorillonite micro-sphere absorption material preparation method is as follows：
It is interior with natural macromolecular material chitosan acetic acid solution using hydrophobically modified montmorillonite particle as emulsion stabilizer
Water phase, atoleine obtain chitosan/hydrophobic illiteracy as organic dispersion medium, glutaraldehyde as crosslinking agent, by lotion cross-linking method
De- soil microballoon.
It is as follows：
(1) by montmorillonite that mass-volume concentration is 5% slurry be 40 DEG C in temperature at aquation 4h；It will be equivalent to montmorillonite
The modifying agent dioctadecyl dimethyl ammonium chloride of 3.0CEC is dissolved in ethanol water, and ethanol water is the body of second alcohol and water
Product is than being 1:1, solution is starched in the montmorillonite being added after aquation, reacts 4h；Stop reaction, centrifuge, collects precipitation；It filters, second
Alcohol solution washs, and collects filter cake, dries 12h to get the montmorillonite particle of hydrophobically modified；
(2) chitosan powdered 2g is added in the acetic acid solution that 100mL mass concentrations are 1%, stirring makes chitosan
Fully dissolving；
(3) liquid paraffin 40mL is taken, 1.6g steps (1) gains are first added, magnetic agitation for 24 hours, keeps particle abundant
Dispersion；20mL steps (2) gains are added, in the high speed dispersion homogenizer 12min of 7000rpm；
(4) step (3) gains are warming up to 40 DEG C in water-bath, the glutaraldehyde that 1.0mL volume fractions are 50% are added dropwise,
It is stirred to react 4 hours；
(5) product of step (4) reaction gained is demulsified, 300mL ethyl alcohol and 400mL deionization moisture are used in filtering respectively
Chong Xi not be 3 times, until the pH value of cleaning solution reaches neutral.
(6) step (5) gains are dry in freeze drier to be no less than 12h, obtain cross-linked chitosan/hydrophobic montmorillonite
Microballoon.
With 3 specific experiments, the present invention will be described in detail below：
(1) the accurate chitosan/hydrophobic montmorillonite microballoon for weighing the above-mentioned preparations of 0.1g, 100mL chlorine ion concentrations, which are added, is
In 0.1mmol/L aqueous solutions, 4h is vibrated at 25 DEG C, 8000rpm is centrifuged 10 minutes, surveys its supernatant iodide ion concentration, profit
It is 0.091mmol/g to calculate adsorbance with above-mentioned formula, and removal effect reaches 90% or more, and processed waste water reaches surface water
Environmental quality secondary standard.
(2) the accurate chitosan/hydrophobic montmorillonite microballoon for weighing the above-mentioned preparations of 0.1g, 100mL iodide ion concentrations, which are added, is
In 0.1mmol/L aqueous solutions, being vibrated 4 hours at 35 DEG C, 8000rpm is centrifuged 10 minutes, surveys its supernatant iodide ion concentration,
It is 0.095mmol/g to calculate adsorbance using above-mentioned formula, and removal effect reaches 95% or more, and processed waste water reaches earth's surface
Quality of water environment secondary standard.
(3) the accurate chitosan/hydrophobic montmorillonite microballoon for weighing the above-mentioned preparations of 0.2g, it is dense to be added 100mL sulfate ions
Degree is that 4h is vibrated at 25 DEG C in 0.1mmol/L aqueous solutions, and 8000rpm is centrifuged 10 minutes, and it is dense to survey its supernatant iodide ion
Degree, it is 0.093mmol/g to calculate adsorbance using above-mentioned formula, and removal effect reaches 90% or more, and processed waste water reaches
Surface water environment quality secondary standard.
Claims (2)
1. the preparation method of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water, which is characterized in that step
It is rapid as follows：
(1) preparation of hydrophobically modified montmorillonite particle
Aquation 4-6h at being 40-60 DEG C in temperature by the montmorillonite slurry of a concentration of 3-5% of w/v；It will be equivalent to montmorillonite 1.0CEC
The modifying agent dioctadecyl dimethyl ammonium chloride of~8.0CEC is dissolved in ethanol water, and ethanol water is second alcohol and water
Volume ratio is 3:1-1:1, solution is starched in the montmorillonite being added after aquation, reacts 4-6h；Stop reaction, centrifuge, collects precipitation；
It filters, filter cake is collected in ethanol water washing, dries 12-24h to get the montmorillonite particle of hydrophobically modified；
(2) preparation of chitosan-acetic acid solution
At room temperature, chitosan is added in the acetic acid solution of a concentration of 0.1-2% of v/v, stirring is quiet after so that chitosan is fully dissolved
It sets overnight；
(3) preparation of Pickering lotions
Step (1) gains are scattered according to a concentration of 2-5% of w/v in atoleine, stirring for 24 hours, keeps particle fully dispersed；
Under 5000-8000rpm homogenous disperses, by the acetum of the chitosan of step (2) by volume 1:1-1:3 are added above-mentioned liquid
In body paraffin, emulsification pretreatment 10-15min obtains Pickering lotions；
(4) preparation of chitosan/hydrophobic montmorillonite microballoon
Pickering lotions obtained by step (3) are warming up to 30-50 DEG C in water-bath, it is 50% that appropriate volume score, which is added dropwise,
Glutaraldehyde is stirred to react 4-6 hours, and EtOH Sonicate, which is added, in gains is demulsified 0.5-1 hours, and ethyl alcohol and deionization are used after filtering
Water washs 2-3 times respectively, after freezing, 12-24 hours is dried in vacuo in 20-30 DEG C to constant weight, it is micro- to obtain chitosan/hydrophobic montmorillonite
Ball.
2. the application that a kind of cross-linked chitosan/hydrophobic montmorillonite microballoon is used to adsorb anion.
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Cited By (8)
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| CN109316949A (en) * | 2018-11-01 | 2019-02-12 | 长沙凯天工研院环保服务有限公司 | Plastic processing emission-control equipment |
| CN109589939A (en) * | 2018-12-13 | 2019-04-09 | 常州大学 | The preparation method of the compound bead of sandwich type UiO-66/ chitosan UiO-66 of high absorption property |
| CN109603766A (en) * | 2018-12-18 | 2019-04-12 | 黑龙江大学 | A kind of preparation method and its removal anionic surfactant of chitosan microball |
| CN110787773A (en) * | 2019-09-30 | 2020-02-14 | 南京工业大学 | Method for compositely modifying montmorillonite aerogel material by using blocky chitosan |
| CN110813261A (en) * | 2019-11-22 | 2020-02-21 | 安徽工业大学 | Preparation method of magnetic chitosan/montmorillonite/humic acid composite microcapsule adsorption material for wastewater treatment |
| CN111871380A (en) * | 2020-07-10 | 2020-11-03 | 大连理工大学 | Preparation method and application of adsorption material for removing anions in water |
| WO2022109661A1 (en) * | 2020-11-24 | 2022-06-02 | Crc Care Pty Ltd | Modified clay sorbents |
| CN117942946A (en) * | 2024-03-12 | 2024-04-30 | 涧纳(上海)环保科技有限公司 | Composite adsorbent and preparation method thereof |
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| CN109316949A (en) * | 2018-11-01 | 2019-02-12 | 长沙凯天工研院环保服务有限公司 | Plastic processing emission-control equipment |
| CN109589939A (en) * | 2018-12-13 | 2019-04-09 | 常州大学 | The preparation method of the compound bead of sandwich type UiO-66/ chitosan UiO-66 of high absorption property |
| CN109589939B (en) * | 2018-12-13 | 2020-05-12 | 常州大学 | Preparation method of sandwich type UiO-66/chitosan @ UiO-66 composite bead with high adsorption performance |
| CN109603766A (en) * | 2018-12-18 | 2019-04-12 | 黑龙江大学 | A kind of preparation method and its removal anionic surfactant of chitosan microball |
| CN110787773A (en) * | 2019-09-30 | 2020-02-14 | 南京工业大学 | Method for compositely modifying montmorillonite aerogel material by using blocky chitosan |
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| CN111871380A (en) * | 2020-07-10 | 2020-11-03 | 大连理工大学 | Preparation method and application of adsorption material for removing anions in water |
| WO2022109661A1 (en) * | 2020-11-24 | 2022-06-02 | Crc Care Pty Ltd | Modified clay sorbents |
| CN117942946A (en) * | 2024-03-12 | 2024-04-30 | 涧纳(上海)环保科技有限公司 | Composite adsorbent and preparation method thereof |
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