CN110064379A - The preparation method of the chitosan magnetic composite material of methyl orange in a kind of absorption effluent - Google Patents
The preparation method of the chitosan magnetic composite material of methyl orange in a kind of absorption effluent Download PDFInfo
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- CN110064379A CN110064379A CN201910445297.5A CN201910445297A CN110064379A CN 110064379 A CN110064379 A CN 110064379A CN 201910445297 A CN201910445297 A CN 201910445297A CN 110064379 A CN110064379 A CN 110064379A
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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
- B01J20/28002—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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- Chemical Kinetics & Catalysis (AREA)
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to technical field of sewage, particularly in a kind of absorption effluent the chitosan magnetic composite material of methyl orange preparation method and applications.The present invention is using montmorillonite as carrier, with chitosan, Fe3O4Particle is doping vario-property agent, is prepared for different chitosans and Fe3O4The chitosan magnetic composite material of doped particles ratio, obtained chitosan magnetic composite material has good absorption property to methyl orange, under the conditions of adsorbent dosage is 0.4g/L, pH 6.3, initial orange concentration is 40mg/L, the adsorption rate of chitosan magnetic is up to 99.6%；The present invention provides theoretical basis for application of the chitosan magnetic composite material in absorption effluent in methyl orange.
Description
Technical field
The present invention relates to technical field of sewage, and particularly the chitosan magnetic of methyl orange is multiple in a kind of absorption effluent
The preparation method and applications of condensation material.
Background technique
Water is the essential energy of Source of life, even more human lives and industrial and agricultural development, to sum up, the mankind are not from
Boiling water soruce.But with the progress of in these years human society, especially industrialized rapid development, the even global model in China
The environmental problem enclosed is increasingly serious, causes greatly to threaten to human lives and development.
Wherein, the discharge amount of dyeing waste water is every year with the increase of different ratios, gradually occupied in entire industrial wastewater compared with
Large scale.Global dyestuff annual output is about 80 to 900,000 tons, and the output of Chinese dyestuff just account for about in 15% to 20%, hand over
Easily amount occupy second place of the world for a long time, is referred to as " dyestuff big country ".However dyeing and printing sewage is without reasonably handling direct emission stream
Enter environment, produce serious water pollution, not only influenced neighbouring ecological environment, threatens the reasonable life of neighbouring biology
It deposits, has more affected indirectly the life and existence of the mankind.When China faces severe shortage of water resources, printing and dyeing are dirty
The untreated discharge of water, which is undoubtedly, to make the matter worse.It is ready to appear to face one effective sewage water treatment method of such predicament.
But dyeing waste water has organic component content larger, and constituent is more complicated, deeper to the pollution color of water body, to water quality shadow
The features such as big is rung, global generally acknowledged sewage treatment problem has been become.
In recent years with the development of dyeing, a large amount of novel printing and dyeing assistant enters printing and dyeing mill, so that many novel difficulties
Degradation of organic substances such as methyl orange enters water body, considerably increases the difficulty of printing and dyeing mill's sewage treatment.
Summary of the invention
The object of the present invention is to provide a kind of chitosan magnetic composite material of methyl orange in absorption effluent and its applications, originally
Invention is using montmorillonite as carrier, with chitosan, Fe3O4Particle is doping vario-property agent, is prepared for different chitosans and Fe3O4Particle
The chitosan magnetic composite material of doping ratio, obtained chitosan magnetic have good absorption property to methyl orange.
The technical solution provided by the present invention is:
The preparation method of the chitosan magnetic composite material of methyl orange in a kind of absorption effluent, comprising the following steps:
(1) FeSO is weighed4·7H2O solid, FeCl3·6H2O solid is placed in 250 mL three-neck flasks, is configured to FeCl3With
FeSO4Mixed solution；
(2) three-neck flask is put into 70 DEG C of thermostat water bath, toward equipped with FeCl3And FeSO4Mixed solution three necks burn
It is passed through nitrogen in bottle, is stirred under nitrogen protection with the speed of 100 r/min, NaOH solution tune is added dropwise into three-neck flask
PH to 10 is saved, black precipitate is generated in bottle, when liquid is in black, is further continued for being placed in 70 DEG C of waters bath with thermostatic control and is stirred to react 1.5h,
Bath temperature is reduced to 50 DEG C, stops stirring, substance will be generated with this condition and stand crystallization 1.5h；
(3) under the action of an external magnetic field, sediment is separated with supernatant liquor, incline supernatant liquor, and 200mL distilled water weight is added
After backwashing is washed to supernatant pH and is in neutrality, and lower sediment thing is then taken to be placed in 60 DEG C of 12 h of vacuum drying, grinding, crosses 200 meshes, system
Obtain Fe3O4Particle；
(4) 10 g montmorillonites are accurately weighed, be put into 250 mL conical flasks and are added 200 mL, 4 mol/L's in conical flask
H2SO4In solution, opens magnetic stirring apparatus and dissolution is sufficiently stirred, form montmorillonite suspension；Water bath with thermostatic control is held under the conditions of 50 DEG C
4 h of continuous dissolution reaction, pour into centrifuge tube for suspension in conical flask, are centrifuged 2 min under conditions of 8000 r/min, 25 DEG C；
Outwell supernatant liquor, be added appropriate distilled water wash repeatedly centrifugation be in neutrality to supernatant liquor, take lower layer's solid in 60 DEG C of dryings
12 h, ground 200 mesh, obtain acidifying montmorillonite；
(5) chitosan is weighed, be put into 250mL conical flask and is added in bottle in the HCl that 200 mL mass fractions are 0.005 %
Solution is sufficiently stirred dissolution using magnetic stirring apparatus and 60 DEG C of thermostatted waters is arranged, and with this condition after 3 h of stirring and dissolving, uses
Mass fraction is that 5% HCl solution adjusts pH to 5；Weigh acidifying montmorillonite, Fe3O4Particle is added in conical flask, changes constant temperature
Bath temperature continues after being stirred to react 4 h to 50 DEG C, and suspension in bottle is poured into centrifuge tube, in 8000 r/min, 25 DEG C of item
It is centrifuged under part, outwells supernatant liquor and appropriate distilled water is added washs centrifugation repeatedly and be in neutrality to supernatant liquor；Take lower layer's solid
It is spare with finely ground 200 meshes excessively afterwards of agate mortar in 60 DEG C of dry 12 h.
Preferably, FeSO in step (1)4·7H2O solid and FeCl3·6H2O solid n (FeSO in molar ratio4•
7H2O):n(FeCl3•6H2O)=3:4。
Preferably, the concentration of NaOH solution is 5 mol/L in step (2).
Preferably, montmorillonite and chitosan mass ratio are 1:1.6, montmorillonite and Fe in step (5)3O4Particle mass ratio
For 1:0.2.
The present invention also provides application of the chitosan magnetic in absorption effluent in methyl orange, the magnetic crust is poly-
The dosage of sugar is 0.4 g/L, pH 6.3, initial orange concentration is 40 mg/L.
Compared with prior art, the device have the advantages that it is as follows:
The obtained magnetic crust that the preparation method of the chitosan magnetic composite material of methyl orange obtains in absorption effluent of the invention
Polysaccharide composite material has good absorption property to methyl orange, adsorbent dosage be 0.4 g/L, pH 6.3, it is initial
Under the conditions of methyl orange concentration is 40 mg/L, the adsorption rate of chitosan magnetic is up to 99.6 %；The present invention is multiple for chitosan magnetic
Application of the condensation material in absorption effluent in methyl orange provides theoretical basis.
Detailed description of the invention
Fig. 1 is the XRD spectrum of magnetic montmorillonite/chitosan；
Fig. 2 is the XRD spectrum of montmorillonite；
Fig. 3 is Fe3O4XRD spectrum；
Fig. 4 is the FTIR map of two kinds of different composite materials.
Specific embodiment
Below with reference to concrete example, the present invention is described in further detail.
Embodiment 1:The preparation of chitosan magnetic composite material
(1) Fe3O4The preparation of particle
We are using coprecipitation come Fe processed herein3O4Particle.The ratio between amount by substance is n (Fe2+):n(Fe3+)=3:4 is prepared
FeCl3·6H2O and FeSO4·7H2The mixed solution of O, that is, take FeSO4·7H23 g of O solid, takes FeCl3·6H2O solid 3.88
G is put into 250 mL three-necked bottles, and 100 mL distilled water are added and sufficiently dissolve.It is passed through nitrogen into three-necked bottle, uses under nitrogen protection
The stirring of 100 r/min constant speed of mechanical agitator, and 70 DEG C of water bath with thermostatic control are controlled, it is slowly added dropwise 5 mol/L's into three-necked bottle
NaOH solution adjusts pH to 10, and black precipitate is generated in bottle, and liquid is in black.1.5 h of sustained response in 70 DEG C of waters bath with thermostatic control
Afterwards, bath temperature is reduced to 50 DEG C, stops mechanical stirring, will be generated substance with this condition and be stood 1.5 h of crystallization.By outer
Add magnetic fields to separate sediment with supernatant liquor, outwell supernatant liquor, 200 mL distilled water are added and are washed repeatedly to upper layer
Clear liquid is in neutrality, and is taken lower sediment thing in 60 DEG C of 12 h of vacuum drying, was fully ground 200 meshes, spare.
(2) preparation of acidifying montmorillonite
10 g montmorillonites are accurately weighed, be put into 250 mL conical flasks and are added 200 mL, 4 mol/L's in conical flask
H2SO4In solution, opens magnetic stirring apparatus and dissolution is sufficiently stirred, form montmorillonite suspension.Water bath with thermostatic control under the conditions of 50 DEG C
Continued dissolution reacts 4 h, and suspension in conical flask is poured into centrifuge tube, is centrifuged 2 under conditions of 8000 r/min, 25 DEG C
min.Outwell supernatant liquor, be added appropriate distilled water wash repeatedly centrifugation be in neutrality to supernatant liquor, take lower layer's solid in 60 DEG C
Dry 12 h, ground 200 mesh are spare.
(3) preparation of chitosan
It accurately weighs 1.6 g chitosans and (it is poly- to weigh 0.8 g, 1.0 g, 1.2 g, 1.4 g, 1.6 g, 1.8 g, 2.0 g shells respectively
Chitosan/montmorillonite that reaction prepares different chitosan contents is added in sugar), it is put into 250mL conical flask and is added in bottle
200 ml mass fractions are the HCl solution of 0.005 %, and dissolution is sufficiently stirred using magnetic stirring apparatus and 60 DEG C of thermostatted waters are arranged,
It the use of mass fraction is that 5% HCl solution adjusts pH to 5 with this condition after 3 h of stirring and dissolving.Weigh 1 g acidifying montmorillonite,
02gFe3O4Particle is added in conical flask, is changed water bath with thermostatic control temperature to 50 DEG C, is continued after being stirred to react 4 h, will be hanged in bottle
Turbid pours into centrifuge tube, is centrifuged under conditions of 8000 r/min, 25 DEG C, outwells supernatant liquor and that appropriate distilled water is added is anti-
After backwashing is washed centrifugation to supernatant liquor and is in neutrality.It takes lower layer's solid in 60 DEG C of dry 12 h, crosses 200 mesh afterwards with agate mortar is finely ground
It sieves to get chitosan magnetic composite material is arrived.
Embodiment 2:The characterization of chitosan magnetic
1) X-ray diffraction (XRD) is analyzed
XRD analysis uses powder pressing method.Appropriate amount of sample powder is taken to be added in dedicated diffraction film trap, gently with smooth glass plate
Tabletting, until obtaining smooth sample powder plane.Used test instrument is Japanese Shimadzu Corporation x-ray diffractometer 6000.It surveys
Strip part are as follows: Cu, Ka radiation, λ=0,1541 nm, test 40 KV of tube voltage, test 30 mA of tube current, scanning range be 2 θ=
5-70 °, scanning speed is 5 °/min, and step-length is 0.02 °.According to Bragg equation: λ=2dsin θ can assaying interlamellar spacing
Variation.
To chitosan magnetic/montmorillonite, montmorillonite raw ore and Fe3O4XRD diffraction analysis is carried out, map is respectively such as Fig. 1-
3。
From Fig. 1-3: chitosan magnetic and protomontronite mineral facies ratio, the 2 θ Angle Positions at diffractive features peak have former illiteracy
6.08 ° of de- stone, which become 5.74 ° of, can calculate the interplanar distance of chitosan magnetic by protomontronite according to Bragg equation
1.48 nm become 1.57 nm, and increasing degree is smaller, it is known that be between entering montmorillonite layer due to chitosan caused by, show chitosan
Effectively it is attached to montmorillonite.Furthermore the XRD spectrum of chitosan magnetic 2 θ=30.36 °, 35.64 °, 43.36 °, 53.84 °,
There is Fe at 57.34 °, 62.98 ° six3O4Characteristic absorption peak, show to be implicitly present in Fe in chitosan magnetic3O4, same table
Bright chitosan magnetic truly has magnetism, can realize magnetic separation under externally-applied magnetic field again.
2) Fourier infrared spectrograph (FT-IR) is analyzed
Infrared spectrum analysis uses pellet technique.It takes appropriate amount of sample powder that potassium bromide is added to be fully ground, uses film-making device
Print is suppressed, is 4000-500 cm in wave number using pure potassium bromide as background-1In the range of carry out infrared spectrum analysis.
From 4 figures: a is chitosan infared spectrum, and b is chitosan magnetic infared spectrum.Chitosan, chitosan magnetic this
Two kinds of compound adsorbents are in 3741 cm-1、3606 cm-1、3620 cm-1、3422 cm-1The characteristic peak at place is Interlayer Water of Montmorillonite
The absorption peak of O-H[16].In 2900 cm-1、2934 cm-1The characteristic peak at place is-CH in chitosan3、-CH2Asymmetric stretch vibration
Dynamic peak, in 1520 cm-1、1502 cm-1The characteristic peak at place is the protonation vibration absorption peak of amino in chitosan, is shown compound
In adsorbent chitosan and montmorillonite by electrostatic interaction in conjunction with.And chitosan magnetic/montmorillonite is in 574 cm-1The characteristic peak at place
For the stretching vibration peak of Fe-O, show Fe3O4Particle has loaded and chitosan magnetic.
In addition, the present invention has also inquired into the factors pair such as adsorption time, adsorbent amount, methyl orange initial concentration, pH, temperature
The influence of chitosan magnetic absorption methyl orange effect.
The result shows that being 1 g in smectite content, chitosan content is 1.6 g, Fe3O4When fraction of particle is 0. 2 g,
Preparing resulting chitosan magnetic has good absorption property to methyl orange.It is that 0.4 g/L, pH is in adsorbent dosage
6.3, under the conditions of initial orange concentration is 40 mg/L, the adsorption rate of chitosan magnetic is up to 99.6 %.The present invention is magnetism
Application of the Chitosan Composites in absorption effluent in methyl blue provides theoretical basis.
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (5)
1. the preparation method of the chitosan magnetic composite material of methyl orange in a kind of absorption effluent, which is characterized in that including following
Step:
(1) FeSO is weighed4·7H2O solid, FeCl3·6H2O solid is placed in 250 mL three-neck flasks, is configured to FeCl3With
FeSO4Mixed solution；
(2) three-neck flask is put into 70 DEG C of thermostat water bath, toward equipped with FeCl3And FeSO4Mixed solution three-neck flask
In be passed through nitrogen, stirred under nitrogen protection with the speed of 100 r/min, NaOH solution adjusting be added dropwise into three-neck flask
PH to 10 generates black precipitate in bottle, when liquid is in black, is further continued for being placed in 70 DEG C of waters bath with thermostatic control and is stirred to react 1.5h, drops
Low bath temperature stops stirring to 50 DEG C, will generate substance with this condition and stand crystallization 1.5h；
(3) under the action of an external magnetic field, sediment is separated with supernatant liquor, incline supernatant liquor, and 200mL distilled water weight is added
After backwashing is washed to supernatant pH and is in neutrality, and lower sediment thing is then taken to be placed in 60 DEG C of 12 h of vacuum drying, grinding, crosses 200 meshes, system
Obtain Fe3O4Particle；
(4) 10 g montmorillonites are accurately weighed, be put into 250 mL conical flasks and are added 200 mL, 4 mol/L's in conical flask
H2SO4In solution, opens magnetic stirring apparatus and dissolution is sufficiently stirred, form montmorillonite suspension；Water bath with thermostatic control is held under the conditions of 50 DEG C
4 h of continuous dissolution reaction, pour into centrifuge tube for suspension in conical flask, are centrifuged 2 min under conditions of 8000 r/min, 25 DEG C；
Outwell supernatant liquor, be added appropriate distilled water wash repeatedly centrifugation be in neutrality to supernatant liquor, take lower layer's solid in 60 DEG C of dryings
12 h, ground 200 mesh, obtain acidifying montmorillonite；
(5) chitosan is weighed, be put into 250mL conical flask and is added in bottle in the HCl that 200 mL mass fractions are 0.005 %
Solution is sufficiently stirred dissolution using magnetic stirring apparatus and 60 DEG C of thermostatted waters is arranged, and with this condition after 3 h of stirring and dissolving, uses
Mass fraction is that 5% HCl solution adjusts pH to 5；Weigh acidifying montmorillonite, Fe3O4Particle is added in conical flask, changes constant temperature
Bath temperature continues after being stirred to react 4 h to 50 DEG C, and suspension in bottle is poured into centrifuge tube, in 8000 r/min, 25 DEG C of item
It is centrifuged under part, outwells supernatant liquor and appropriate distilled water is added washs centrifugation repeatedly and be in neutrality to supernatant liquor；Take lower layer's solid
It is spare with finely ground 200 meshes excessively afterwards of agate mortar in 60 DEG C of dry 12 h.
2. the preparation method of chitosan magnetic composite material according to claim 1, which is characterized in that in step (1)
FeSO4·7H2O solid and FeCl3·6H2O solid n (FeSO in molar ratio4•7H2O):n(FeCl3•6H2O)=3:4。
3. the preparation method of chitosan magnetic composite material according to claim 1, which is characterized in that in step (2)
The concentration of NaOH solution is 5 mol/L.
4. the preparation method of chitosan magnetic composite material according to claim 1, which is characterized in that covered in step (5)
De- stone and chitosan mass ratio are 1:1.6, montmorillonite and Fe3O4Particle mass ratio is 1:0.2.
5. application of the chitosan magnetic composite material according to claim 1 to 4 in absorption effluent in methyl orange,
It is characterized in that, the dosage of the chitosan magnetic is 0.4 g/L, pH 6.3, initial orange concentration is 40 mg/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| US20040146855A1 (en) * | 2003-01-27 | 2004-07-29 | Marchessault Robert H. | Formation of superparamagnetic particles |
| CN102989426A (en) * | 2012-12-21 | 2013-03-27 | 福建师范大学福清分校 | Hydrothermal liquid phase preparation method of magnetic kaolinite/chitosan composite |
| CN103920472A (en) * | 2014-04-11 | 2014-07-16 | 江苏大学 | Preparation method of magnetic chitosan composite microsphere adsorbent |
| CN105312023A (en) * | 2015-10-16 | 2016-02-10 | 南京农业大学 | Magnetic adsorbent for removing dye in water and preparation method and application thereof |
| CN109603771A (en) * | 2019-01-10 | 2019-04-12 | 盐城工学院 | A kind of preparation method of chitosan magnetic-montmorillonite-based nano complex microsphere |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20040146855A1 (en) * | 2003-01-27 | 2004-07-29 | Marchessault Robert H. | Formation of superparamagnetic particles |
| CN102989426A (en) * | 2012-12-21 | 2013-03-27 | 福建师范大学福清分校 | Hydrothermal liquid phase preparation method of magnetic kaolinite/chitosan composite |
| CN103920472A (en) * | 2014-04-11 | 2014-07-16 | 江苏大学 | Preparation method of magnetic chitosan composite microsphere adsorbent |
| CN105312023A (en) * | 2015-10-16 | 2016-02-10 | 南京农业大学 | Magnetic adsorbent for removing dye in water and preparation method and application thereof |
| CN109603771A (en) * | 2019-01-10 | 2019-04-12 | 盐城工学院 | A kind of preparation method of chitosan magnetic-montmorillonite-based nano complex microsphere |
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| 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 |
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Application publication date: 20190730 |