CN106423087A - Preparation method of magnetic chitosan carbon spheres and application thereof in adsorbing and removing Cr (VI) in water - Google Patents
Preparation method of magnetic chitosan carbon spheres and application thereof in adsorbing and removing Cr (VI) in water Download PDFInfo
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- 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
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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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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Abstract
The invention relates to oral powder in traditional Chinese medicine compatibility, in particular to allergy decocting powder used for treating skin allergy by utilizing pure traditional Chinese medicine and a preparation method. The allergy decocting powder is characterized by being prepared from the following traditional Chinese medicine raw materials in parts by weight: 10 to 20 parts of radix bupleuri, 15 to 35 parts of fructus mume, 15 to 20 parts of radix paeoniae alba, 20 to 35 parts of radix saposhnikoviae, 10 to 15 parts of liquorice root, 15 to 25 parts of bombyx batryticatus, 10 to 15 parts of dried radix rehmanniae, 5 to 10 parts of fructus schisandrae and 5 to 15 parts of exocarpium zingiberis recentis. The allergy decocting powder disclosed by the invention has the characteristic that reasonable compatibility of medicine is guided by traditional Chinese medicine theories of treating based on syndrome differentiation, treating diseases from the root and harmonizing nutrient and defense; the allergy decocting powder has the advantages that used traditional Chinese medicine materials all accord with regulations of Pharmacopoeia of the People's Republic of China, and raw materials of the traditional Chinese medicine are safe and reliable.
Description
Technical field
The invention belongs to technical field of water pollution control is and in particular to arrive a kind of preparation method of chitosan magnetic carbon ball,
The invention still further relates to the method going Cr in eliminating water (VI) using the chitosan magnetic carbon ball of above-mentioned preparation.
Background technology
Heavy metal chromium is one of pollutant of China's priority acccess control, is mainly derived from plating, metallurgy, process hides, printing and dyeing and change
The three wastes of the industries such as work discharge.Chromium is in water body mainly presented in Cr (III) and Cr (VI).Compared with Cr (III), Cr
(VI) toxicity is higher, be absorbed by the body can cause have a stomach-ache, bad habit, diarrhoea, vomiting, the disease such as hepatocarcinoma.
At present, the processing method of chromate waste water mainly have chemical precipitation method, ion exchange, membrane separation process, photocatalytic method,
Electrochemical process, biochemical process etc..Absorption method has the advantages that simple to operate, cost is relatively low, high treating effect, is widely used in
Processing waste water containing chrome.However, during some traditional adsorbent Adsorption Cr (VI), exist that adsorbance is low or absorption reaches
Shortcoming to balance required time length.
Shitosan is a kind of prepared natural cationic polysaccharide by chitin deacetylase base, has bio-compatible
Property, environment friendly the features such as, on its strand be rich in OH and NH2Isoreactivity group, can be made by electrostatic or complexation
With pollutant such as Adsorption of Heavy Metal Ions from waste water.
Chinese patent " a kind of new and effective chromium remover and preparation method thereof " (application number 200910053681.7, open
Number 101927153A, publication date on December 29th, 2010) with shitosan and chitosan for main reactant, then be aided with stabilizer,
The compositions such as water, prepare a kind of chromium remover.
Chinese patent " a kind of Magnetic chitosan microsphere treatment agent and preparation method thereof " (application number 201310097557.7,
Publication number 103127914A, publication date on June 5th, 2013) it is that tourmaline and chitosan magnetic micro-sphere mixed powder are added Sargassum
In sour sodium and polyvinyl alcohol, dissolving, mixing, then solidify balling-up, for Cr (VI) in Adsorption water.
Chinese patent " preparation method of modified magnetic chitosan microball adsorbent for heavy metal " (application number
201310189171.9, publication number 103263895A, publication date August in 2013 28 days) first magnetic is prepared for raw material with shitosan
Property chitosan microball, then carries out grafting modification, obtains a kind of Cr (VI) adsorbent to it.
A kind of Chinese patent " preparation method of the adsorbent of the absorption Cr (VI) based on shitosan " (application number
201410199659.4, publication number 103933951A, publication date on July 23rd, 2014) shitosan that is widely present with nature
For raw material, carry out hydro-thermal reaction in high-pressure hydrothermal reaction kettle, obtain rich in OH and NH2And acidproof new carbon materials
Material adsorbent.
A kind of Chinese patent " acid resistance chitosan magnetic micro-sphere, preparation method and applications " (application number
201410608653.8, publication number 104437395A, publication date on March 25th, 2015) with Chitosan powder as raw material, by breast
Liquid cross-linking method prepares coated magnetic SiO2Chitosan microball.Simultaneously in order to improve the adsorbance of microsphere further, with dendritic poly-
Aziridine is modified to adsorbent for functional group, obtains modification of chitosan microsphere, can be used for Cr in Adsorption water
(Ⅵ).
Chinese patent " removes the Cr in waste water with walnut shell biological carbon using the adsorbent that beta-schardinger dextrin-shitosan is combined
(VI) method " (application number 201510585777.3, publication number 105236507A, publication date on January 13rd, 2016) first by β-
Cyclodextrin shitosan is combined, and then carries out high-temperature calcination, prepared walnut shell by drying the walnut shell biomass clayed into power
Beta-schardinger dextrin-shitosan is finally compound to biological carbon surface by charcoal.
" magnetic adsorbent that a kind of shitosan is combined with magnetic biological carbon removes the side of Cr (VI) in waste water to Chinese patent
Method " (application number 201510126324.4, publication number 104787831A, publication date on July 22nd, 2015) is first with FeCl3·
6H2O soaks to Herba Eichhorniae biomass, and then the biomass soaked are carried out with pyrolysis calcining, thus magnetic bio is obtained
Charcoal, then shitosan is compound to magnetic bio carbon surface.
Chinese patent " a kind of remove magnetic adsorbent of heavy metal and preparation method thereof in eliminating water " (application number
201610186666.X, publication number 105664884A, publication date on June 15th, 2016) by chitosan magnetic polyvinylalcohol microsphere
Successively through the modified gained modified with Carbon bisulfide of glutaraldehyde cross-linking, preparation one kind removes the magnetic adsorbent of Cr in eliminating water (VI) to ball.
Adsorbent Adsorption Cr (VI) better performances of preparation in above-mentioned patent.But, because shitosan is in acid water
It is susceptible in solution dissolve and formed colloid, generally cannot directly use in acid condition.But can only for Cr (VI)
Just can there is good result in acid condition.In order to improve stability in acid condition it is necessary to be modified to shitosan,
As crosslinked reaction with glutaraldehyde, epoxychloropropane and ethylenediamine etc..These cross-linking modified preparation process are considerably complicated, and
Need substantial amounts of organic solvent, be also easy to produce secondary pollution, sometimes also result in the decline of absorption property.In addition, in above-mentioned patent
It is difficult to solid-liquid separation after middle part adsorbent absorption.So that finding more easy, green and effective shitosan absorption
The preparation method of agent, had both retained the active group of shitosan, enabled simple and quick solid-liquid separation again.
Content of the invention
The present invention is intended to provide a kind of preparation process is simple, low cost, easy to operate, adsorption capacity are big, stable compared with extensive chemical
Property and be capable of simple and quick separate remove waste water in Cr (VI) adsorbent preparation method and application.
The principle of the present invention:Prepare magnetic cobalt ferrite first with hydro-thermal method, then use hydro-thermal method by shitosan carbonization
It is supported on the surface of magnetic cobalt ferrite, obtain chitosan magnetic carbon ball.This adsorbent surface had both been rich in OH and NH2Isoreactivity
Group, kernel cobalt ferrite has certain magnetic, is capable of quickly and easily separating using Magnet.
The technical solution adopted in the present invention is that the preparation method of chitosan magnetic micro-sphere, specifically according to following steps reality
Apply:
The preparation of I magnetic cobalt ferrite
(1) it is 2 according to iron salt and cobalt salt mol ratio:1 weighs FeCl respectively3·6H2O and CoCl2·6H2O is dissolved in 50mL and steams
In distilled water;
(2) under magnetic stirring, it is more than to Deca 2mol/L sodium hydroxide solution in the solution being obtained by step (1) to pH
11, solution is transferred in hydrothermal reaction kettle (filling degree≤75%), is placed in 180 DEG C of hydro-thermal reactions 24h in high temperature furnace;
(3), after natural cooling, the solid-liquid that step (2) is obtained carries out Magneto separate, gained solid 0.1mol/LHCl and steaming
Distilled water cyclic washing, to neutral, dried, is ground and sieve, that is, obtain Armco magnetic iron acid cobalt.
The preparation of II chitosan magnetic micro-sphere
(1) it is 1~4 according to shitosan and magnetic cobalt ferrite mass ratio:After 1 weighs shitosan and cobalt ferrite, plus distilled water
Ultrasonic be allowed to dissolving dispersion;
(2) solution obtaining step (1) transfers to (filling degree≤75%) in hydrothermal reaction kettle, is placed in high temperature furnace
180 DEG C of hydro-thermal reaction 12~48h;
(3), after natural cooling, the solid-liquid that step (2) is obtained carries out Magneto separate, gained solid dehydrated alcohol and distillation
Water cyclic washing, to neutral, dried, is ground and sieve, that is, obtain chitosan magnetic micro-sphere.
Further, answering on the chitosan magnetic carbon ball that above-mentioned preparation method obtains Cr (VI) in Adsorption water
With.
Further, the optimum condition of above-mentioned application is:Under the conditions of 298K, 150r/min, Cr (VI) initial concentration
For 100~600mg/L, pH value of solution is 2, and adsorption time is 5min~48h, Magneto separate afterwards.The now maximum adsorption of Cr (VI)
Measure as 274.8mg/g.
Compared with prior art, the present invention has the following advantages:
(1) adsorbent that the present invention provides adopts hydro-thermal method to prepare, this process is simple, and energy consumption is low, easy to operate;Prepare
Adsorbent physical and chemical stability strong, can use in the range of wider pH;There is preferable magnetic, can be in externally-applied magnetic field bar
It is separated from water under part, reach solid-liquid separation effect.
(2) adsorbent surface that the present invention provides is rich in OH and NH2Isoreactivity group, it is possible to use this adsorbent
Cr (VI) in Adsorption water, under conditions of 298K, pH=2 and 150r/min, the theoretical maximum adsorbance of this adsorbent is
274.8mg/g, shows that the chitosan magnetic carbon ball providing the present invention is used for Cr (VI) in Adsorption water and has good warp
Ji benefit and environmental benefit.
Brief description
Fig. 1 is scanning electron microscope (SEM) figure of chitosan magnetic carbon ball in the embodiment of the present invention 4.
Fig. 2 is infrared spectrum (FTIR) figure of chitosan magnetic carbon ball in the embodiment of the present invention 4;
Wherein:A represents cobalt ferrite, and B represents chitosan magnetic carbon ball.
Fig. 3 is X-ray diffraction (XRD) figure of chitosan magnetic carbon ball in the embodiment of the present invention 4;
Wherein:A represents cobalt ferrite, and B represents chitosan magnetic carbon ball.
Fig. 4 is the hysteresis curve figure of chitosan magnetic carbon ball in the embodiment of the present invention 4;
Wherein:A represents cobalt ferrite, and B represents chitosan magnetic carbon ball.
Specific embodiment
Below by example, the present invention is described in further detail, but the present invention is not limited to following embodiments.
First, the preparation of adsorbent
Embodiment 1
1st, the preparation of magnetic cobalt ferrite
(1) weigh 2.71g FeCl respectively3·6H2O and 1.19g CoCl2·6H2O is dissolved in 50mL distilled water;
(2) under magnetic stirring, it is more than to Deca 2mol/L sodium hydroxide solution in the solution being obtained by step (1) to pH
11, solution is transferred in 100mL hydrothermal reaction kettle (filling degree≤75%), is placed in 180 DEG C of hydro-thermal reactions 24h in high temperature furnace;
(3), after natural cooling, the solid-liquid that step (2) is obtained carries out Magneto separate, gained solid 0.1mol/LHCl and steaming
Distilled water cyclic washing, to neutral, dried, grinds and sieve for 60 DEG C, that is, obtaining Armco magnetic iron acid cobalt.
2nd, the preparation of chitosan magnetic carbon ball
(1) it is 1 according to shitosan and magnetic cobalt ferrite mass ratio:1 weighs shitosan and cobalt ferrite, plus after 50mL distilled water
It is allowed to dissolving dispersion after ultrasonic 15min;
(2) solution obtaining step (1) transfers to (filling degree≤75%) in 100mL hydrothermal reaction kettle, is placed in high temperature
180 DEG C of hydro-thermal reactions 24h in stove;
(3), after natural cooling, the solid-liquid that step (2) is obtained carries out Magneto separate, gained solid dehydrated alcohol and distillation
Water cyclic washing, to neutral, dried, grinds and sieve for 60 DEG C, that is, obtaining chitosan magnetic micro-sphere.
Embodiment 2
1st, the preparation of magnetic cobalt ferrite
With embodiment 1.
2nd, the preparation of chitosan magnetic carbon ball
With embodiment 1, except that adding shitosan and magnetic cobalt ferrite mass ratio to be 2:1.
Embodiment 3
1st, the preparation of magnetic cobalt ferrite
With embodiment 1.
2nd, the preparation of chitosan magnetic carbon ball
With embodiment 1, except that adding shitosan and magnetic cobalt ferrite mass ratio to be 3:1.
Embodiment 4
1st, the preparation of magnetic cobalt ferrite
With embodiment 1.
2nd, the preparation of chitosan magnetic carbon ball
With embodiment 1, except that adding shitosan and magnetic cobalt ferrite mass ratio to be 4:1.
Embodiment 5
1st, the preparation of magnetic cobalt ferrite
With embodiment 1.
2nd, the preparation of chitosan magnetic carbon ball
With embodiment 4, except that the hydro-thermal reaction time should be 12h.
Embodiment 6
1st, the preparation of magnetic cobalt ferrite
With embodiment 1.
2nd, the preparation of chitosan magnetic carbon ball
With embodiment 4, except that the hydro-thermal reaction time should be 48h.
2nd, in chitosan magnetic carbon ball Adsorption water Cr (VI) embodiment
Embodiment 7
Weigh the adsorbent of preparation in 0.050g embodiment 1, be added to 40mLK2Cr2O7(pH=2,300mg/ in solution
L), vibrate under conditions of 298K, 150r/min to adsorption equilibrium, after Magneto separate, measure Cr (VI) residual concentration in supernatant,
Result of calculation is listed in Table 1 below.
Embodiment 8
With embodiment 7, except that weighing the adsorbent of preparation in 0.050g embodiment 2.
Embodiment 9
With embodiment 7, except that weighing the adsorbent of preparation in 0.050g embodiment 3.
Embodiment 10
With embodiment 7, except that weighing the adsorbent of preparation in 0.050g embodiment 4.
Embodiment 11
With embodiment 7, except that weighing the adsorbent of preparation in 0.050g embodiment 5.
Embodiment 12
With embodiment 7, except that weighing the adsorbent of preparation in 0.050g embodiment 6.
The adsorbent of table 1 each embodiment preparation compares to the absorption property of Cr (VI)
As shown in Table 1, under the same conditions, in embodiment 1~4, the adsorbent of preparation to the clearance of Cr in water (VI) is in
Increasing trend, and all solid-liquid sharp separation can be realized by externally-applied magnetic field.In addition, as can also be seen from Table 1, chitosan magnetic carbon
The adsorbent absorption property that ball is prepared in embodiment 4 is best.
Embodiment 13
Weigh the adsorbent of preparation in several pieces 0.050g embodiment 4, be added separately to (pH in 20mL potassium bichromate solution
=2,300mg/L), vibrate under conditions of 298K, 150r/min, presetting point in time sampling, measuring after Magneto separate
Cr (VI) residual concentration in clear liquid, result of calculation is listed in Table 2 below.
Table 2 adsorption dynamics adsorption kinetics
As shown in Table 2, the adsorbent that the present invention provides is very fast to Cr (VI) rate of adsorption, substantially can reach after absorption 2h
Balance, clearance is up to 91.7%.
Embodiment 14
Weigh the adsorbent of preparation in 0.050g embodiment 4, be added to (pH=in 40mL difference pH value potassium bichromate solution
2~8,300mg/L), vibrate under conditions of 298K, 150r/min to adsorption equilibrium, after Magneto separate, measure Cr in supernatant
(VI) residual concentration, result of calculation is listed in Table 3 below.
The impact of table 3 pH
As shown in Table 3, in the adsorbent Adsorption water that the present invention provides, Cr (VI) reduces with the rising of pH, and acidity is got over
The strong removal being more conducive to Cr (VI), works as pH=2, Cr (VI) clearance is up to 91.4%.
Embodiment 15
Weigh in several pieces 0.050g embodiment 4 adsorbent of preparation, be added separately to 40mL variable concentrations (100~
600mg/L) (pH=2) in potassium bichromate solution, vibrate under conditions of 298K, 150r/min to adsorption equilibrium, after Magneto separate
Measure Cr (VI) residual concentration in supernatant, result of calculation is listed in Table 4 below.
Table 4 adsorption isotherm
F and L-type linear fit are carried out to table 4 data, result meets L-type absorption.Inhaled according to L-type Equation for Calculating theoretical maximum
Attached amount is 274.8mg/g.
Claims (3)
1. a kind of preparation method of chitosan magnetic carbon ball, its feature is comprising the following steps:
(1) preparation of magnetic cobalt ferrite:
It is 2 according to iron salt and cobalt salt mol ratio:1 weighs FeCl respectively3·6H2O and CoCl2·6H2O is dissolved in 50mL distilled water,
Under magnetic stirring Deca 2mol/L sodium hydroxide solution to pH be more than 11, after solution is transferred in hydrothermal reaction kettle, be placed in
180 DEG C of hydro-thermal reactions 24h in high temperature furnace;After natural cooling, with 0.1mol/L HCl and distilled water cyclic washing to neutral, dry
Dry, grinding is sieved, and obtains final product magnetic cobalt ferrite;
(2) preparation of chitosan magnetic carbon ball:
Mass ratio according to shitosan and cobalt ferrite is 1~4:1 weighs the magnetic ferrous acid that shitosan and step (1) obtain respectively
After cobalt, plus distilled water ultrasonic be allowed to dissolving dispersion, after solution is transferred in hydrothermal reaction kettle, be placed in 180 DEG C of water in high temperature furnace
Thermal response 12~48h;After natural cooling, the solid-liquid obtaining is carried out with Magneto separate, gained solid dehydrated alcohol and distilled water are anti-
After backwashing is washed to neutrality, dries, grinds and sieve, that is, obtains chitosan magnetic micro-sphere.
2. answering on the chitosan magnetic carbon ball that preparation method as claimed in claim 1 obtains Cr (VI) in Adsorption water
With.
3. the application on chitosan magnetic carbon ball as claimed in claim 2 Cr (VI) in Adsorption water is it is characterised in that be somebody's turn to do
Application condition be:Under the conditions of 298K, 150r/min, Cr (VI) initial concentration is 100~600mg/L, and pH value of solution is 2, inhales
The attached time is 5min~48h, Magneto separate afterwards.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106914219A (en) * | 2017-04-07 | 2017-07-04 | 安徽工业大学 | A kind of application of magnetic carbosphere Cr VI in waste water is removed |
CN109289787A (en) * | 2018-10-31 | 2019-02-01 | 山东大学 | A kind of preparation method of the co-modified biological carbon composite of iron, cyclodextrin |
CN110064378A (en) * | 2019-05-08 | 2019-07-30 | 广州大学 | A kind of high absorption property chitosan magnetic carbon ball and its preparation method and application |
CN110975463A (en) * | 2019-03-07 | 2020-04-10 | 乐清市智格电子科技有限公司 | Preparation process of environment-friendly air purification material |
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2016
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106914219A (en) * | 2017-04-07 | 2017-07-04 | 安徽工业大学 | A kind of application of magnetic carbosphere Cr VI in waste water is removed |
CN109289787A (en) * | 2018-10-31 | 2019-02-01 | 山东大学 | A kind of preparation method of the co-modified biological carbon composite of iron, cyclodextrin |
CN110975463A (en) * | 2019-03-07 | 2020-04-10 | 乐清市智格电子科技有限公司 | Preparation process of environment-friendly air purification material |
CN110064378A (en) * | 2019-05-08 | 2019-07-30 | 广州大学 | A kind of high absorption property chitosan magnetic carbon ball and its preparation method and application |
CN110064378B (en) * | 2019-05-08 | 2021-10-26 | 广州大学 | Magnetic chitosan carbon sphere with high adsorption performance and preparation method and application thereof |
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