CN105236507B - The method that the adsorbent being combined using beta cyclodextrin chitosan and walnut shell charcoal removes the Cr VI in waste water - Google Patents
The method that the adsorbent being combined using beta cyclodextrin chitosan and walnut shell charcoal removes the Cr VI in waste water Download PDFInfo
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- CN105236507B CN105236507B CN201510585777.3A CN201510585777A CN105236507B CN 105236507 B CN105236507 B CN 105236507B CN 201510585777 A CN201510585777 A CN 201510585777A CN 105236507 B CN105236507 B CN 105236507B
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Abstract
The method that the adsorbent being combined the invention discloses a kind of beta cyclodextrin chitosan and walnut shell charcoal removes Cr VI in waste water, the compound includes first being combined beta cyclodextrin and chitosan, then the grafting beta cyclodextrin chitosan on the biological carbon matrix of walnut shell；The step of preparation method, includes：First beta cyclodextrin chitosan is combined, then the walnut shell biomass progress high-temperature calcination clayed into power will be dried, walnut shell charcoal is made, beta cyclodextrin chitosan is finally compound to biological carbon surface；This using the step of be：The composite is added in containing the hexavalent chromium wastewater that concentration is 20~800mg/L, composite usage amount is 0.1~1g/L, it is 2~9 in pH, vibrated at 20~50 DEG C of temperature after adsorption reaction for a period of time, adsorbent is separated and collected by filtering or precipitation, the removal to hexavalent chromium in waste water is completed.The present invention is with low cost, technique is simple, absorption property is high, waste is effectively utilized and easily separated, advantages of environment protection.
Description
Technical field
The present invention relates to application of the charcoal composite biological material in field of waste water treatment, more particularly to beta cyclodextrin shell
The walnut shell charcoal of glycan modification removes the application of the Cr VI in waste water.
Background technology
Heavy metal pollution of water body is the larger problem of environmental pollution of current harm influence, and the pollution of heavy metal chromium is wherein normal
One of water breakthrough body pollution.Heavy metal chromium pollution is mainly derived from cosmetic material, leather preparation, metal parts chromium plating part, work
Industry pigment and tanning, rubber and ceramic raw material etc.；The toxicity of chromium is relevant with the valence state that it is present, and Cr VI is than trivalent chromium toxicity
It is high 100 times, and be easily absorbed by the body and accumulate in vivo, trivalent chromium and Cr VI can be converted mutually.If human body excess intake
Chromium, can cause the poisoning symptoms such as abdominal discomfort and diarrhoea, cause allergic dermatitis or eczema, and breathing enters human body, had to respiratory tract
Stimulate and corrosiveness, cause pharyngitis, bronchitis etc. to endanger.China《Integrated wastewater discharge standard》(GB8978-1996) in
Total chrome content must not exceed 1.5mg/L in clear stipulaties industrial wastewater, and content of 6-valence Cr ions must not exceed 0.5mg/L.It is conventional at present
Minimizing technology mainly have membrane processing method, ion-exchange, the precipitation method and absorption method.Absorption method is substantially adsorbent activity table
In face of the attraction of chromium ion, and because being received more and more attention in its efficient, low price and recoverable wastewater the advantages of heavy metal,
The active charcoal of conventional adsorbent, humic acid, sepiolite, polysaccharide resins etc..But because most of inorganic adsorbents source is not enriched,
Organic adsorbent limited sorption capacity and limit it and use, therefore prepare a kind of wide material sources, the suction of cheap and high adsorption capacity
Attached dose has very big actual application value and meaning.
Charcoal be bio-organic materials (biomass) in anoxic or anoxybiotic environment, after low temperature thermal cracking generate fragrance
The solid product of infusibility.Because it has the structures such as loose porous, aligned orderly aromatic rings lamella so that charcoal is being inhaled
There are very big potentiality in terms of the pollutants such as heavy metal, organic matter, dyestuff in attached waste water.Walnut shell belongs to endocarp.Experiment card
It is bright, in degreasing, it is broken into graininess and there is good adsorption effect into heavy metal chromium after charcoal by high-temperature calcination, rises
The effect of twice laid is arrived.Chitosan is also known as chitosan, is that the chitin being widely present by nature passes through de- second
Acyl effect is obtained.There is active hydroxyl and amino in chitosan macromolecular, occur chelation with stronger and heavy metal
Respond.Cyclodextrin is that amylose is generated under the cyclodextrin glycosyltransferase effect produced by bacillus
A series of general name of cyclic oligosaccharides.The molecule hole of beta cyclodextrin is moderate, has a wide range of application, production cost is low, is industrial at present
Using most cyclodextrin products, but his hydrophobic region and catalytic activity are limited, make it in application by a definite limitation.Cause
This, first by beta cyclodextrin and chitosan valid link, then is combined with walnut charcoal, is increased biological carbon surface weight with this
The adsorption site of metal and the quantity of functional group, so as to improve the adsorption capacity of its heavy metal.
The content of the invention
The technical problem to be solved in the present invention be overcome the deficiencies in the prior art there is provided a kind of adsorption capacity is big, cost is low,
Prepare the simple and environmentally safe method for removing Cr VI in waste water.
In order to solve the above technical problems, technical scheme proposed by the present invention is to be given birth to using beta cyclodextrin chitosan with walnut shell
The method that the compound adsorbent of thing charcoal removes the Cr VI in waste water, the described method comprises the following steps：Take a certain amount of sexavalence
Chromium concn waste water, a certain amount of beta cyclodextrin chitosan biological carbon adsorbent is added in waste water, is vibrated in constant temperature oscillator
Absorption, staticly settles or is separated by filtration after having reacted, and completes the removal to Cr VI in waste water.
In above-mentioned technical proposal, the beta cyclodextrin chitosan biological carbon adsorbent is made by following steps：
(1) chitosan of 6g beta cyclodextrins and 1g is dissolved in 120ml 1mol/L hydrochloric acid solution, adds in three-necked bottle, stirs
Uniform milky white solution is mixed, when being heated to 85 DEG C or so bleach, 50% glutaraldehyde 3ml is added dropwise, continues heating response 1h
After be changed into faint yellow taking-up；
(2) the product regulation pH value in (1) to 7~8 is changed into after brown with 1mol/L NaOH solution, cooled down, precipitation,
Filtering, dry beta cyclodextrin chitosan product；
(3) it will dry and wear into granular walnut shell biomass and be put into tube furnace, and 300~600 DEG C, lead to N2, burning 1~
2h, that is, obtain walnut shell charcoal.Obtained magnetic bio charcoal is washed with deionized 2~3 times, 50~60 DEG C of drying are ground
Mill, crosses 150 mesh sieves；
(4) take 2g walnut shell charcoal to be dissolved in 200ml ultra-pure waters, be put into ultrasonic disperse 2h in ultrasonic case.Again plus
PH to 7.0 is adjusted after entering 0.1M each 50ml of NHS and EDC, then continuing magnetic force stirring 2.5h；
(5) take in charcoal suspension of the beta cyclodextrin chitosan product in 4g (2) in (4), add 10ml penta 2
Aldehyde, ultrasonic disperse 10min is placed in 65 DEG C and vibrates 2h, then adjusts pH to 7.0, filtering, 50 DEG C of drying, grindings, crosses 150 mesh sieves, i.e.,
Obtain beta cyclodextrin chitosan biological charcoal composite material adsorbent.
In above-mentioned preparation method, the order of preparation is first to prepare beta cyclodextrin chitosan and walnut shell charcoal, then prepares β
Cyclodextrin chitosan walnut shell biology carbon composite.
The present invention also provides a kind of biological carbon composite of above-mentioned beta cyclodextrin chitosan walnut shell and is applied to remove sexavalence
The method of chromium ion, comprises the following steps：The composite is added in containing the hexavalent chromium wastewater that concentration is 20~800mg/L,
Composite usage amount is 0.1~1g/L, is vibrated at 20~50 DEG C after adsorption reaction for a period of time, and precipitation or filtering will be compound
Thing is separated with waste water, completes the removal to hexavalent chromium.
In above-mentioned application, the pH value of the adsorption reaction is preferably 2~9；
In above-mentioned application, the sorption reaction time is preferably 1~24 hour；
In above-mentioned technical proposal, the constant temperature oscillator rotating speed is preferably 100~160 revs/min.
Compared with prior art, the advantage of the invention is that：
1. the beta cyclodextrin chitosan walnut shell charcoal of the present invention, with specific surface area is big, pore space is big, aperture chi
The characteristics of very little small, surface functionalities are rolled into a ball more and easily combined with metal ion, and adsorption efficiency is high, with environment friendly, attaches most importance to
The improvement of metal chrome waste water proposes new method.
2. raw material sources enrich, cost is low, and its preparation method and technique are simple, can effectively realize industrial metaplasia
Production；
3. the removal efficiency of the beta cyclodextrin chitosan walnut shell charcoal heavy metal Cr VI of the present invention is high, work is handled
Skill is simple and easily operated.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the biological carbon composite of beta cyclodextrin chitosan walnut shell of the embodiment of the present invention 1；
After Fig. 2 is the beta cyclodextrin chitosan biological charcoal walnut shell composite adsorbing hexavalent chromium of the embodiment of the present invention 1
XPS spectrum figure.
Embodiment
The present invention is described in further details below with reference to Figure of description and specific embodiment.
Embodiment 1：
A kind of biological carbon composite of beta cyclodextrin chitosan walnut shell of the present invention, the composite is by with lower section
It is prepared by method：
(1) chitosan of 6g beta cyclodextrins and 1g is dissolved in 120ml 1mol/L hydrochloric acid solution, adds in three-necked bottle, stirs
Uniform milky white solution is mixed, when being heated to 85 DEG C or so bleach, 50% glutaraldehyde 3ml is added dropwise, continues heating response 1h
After be changed into faint yellow taking-up；
(2) the product regulation pH value in (1) to 7~8 is changed into after brown with 1mol/L NaOH solution, cooled down, precipitation,
Filtering, dry beta cyclodextrin chitosan product；
(3) it will dry and wear into granular walnut shell biomass and be put into tube furnace, and 300~600 DEG C, lead to N2, burning 1~
2h, that is, obtain walnut shell charcoal.Obtained magnetic bio charcoal is washed with deionized 2~3 times, 50~60 DEG C of drying are ground
Mill, crosses 150 mesh sieves；
(4) take 2g walnut shell charcoal to be dissolved in 200ml ultra-pure waters, be put into ultrasonic disperse 2h in ultrasonic case.Again plus
PH to 7.0 is adjusted after entering 0.1M each 50ml of NHS and EDC, then continuing magnetic force stirring 2.5h；
(5) take in charcoal suspension of the beta cyclodextrin chitosan product in 4g (2) in (4), add 10ml penta 2
Aldehyde, ultrasonic disperse 10min is placed in 65 DEG C and vibrates 2h, then adjusts pH to 7.0, filtering, 50 DEG C of drying, grindings, crosses 150 mesh sieves, i.e.,
Obtain beta cyclodextrin chitosan/biology charcoal composite material adsorbent.
Embodiment 2：
The biological carbon composite of beta cyclodextrin chitosan walnut shell prepared by embodiment 1 is applied to hexavalent chromium waste water
Processing, comprise the following steps：8 parts of 100mg/L chromium solution is configured, it is respectively 2 to adjust pH with 1mol/L NaOH and HCl,
3,4,5,6,7,8 and 9.The biological carbon composite of above-mentioned beta cyclodextrin chitosan walnut shell is added, adsorbent amount is 0.1g/L.
It is respectively placed in 25 DEG C of constant temperature oscillations.Water-bath constant temperature oscillator rotating speed is 160rpm, and duration of oscillation is 24h.After reaction terminates, put
Upper solution is taken in filter filtration on paper or quiescent setting, the separating adsorbent from solution, adsorption process terminates.Use ultraviolet spectrometry light
Degree method determines the content of Cr VI not to be adsorbed in waste water, and the adsorbance of calculating the results are shown in Table 1.
Table 1：Different pH value remove the influence of Cr VI in waste water to beta cyclodextrin chitosan biological carbon composite
As shown in Table 1, condition of different pH is very big to Adsorption Effect.Adsorbent is conducive to remove Cr VI when pH is relatively low
Remove, adsorbance reaches maximum when pH is 2, and as pH is raised, adsorbance is gradually reduced.(chromium solution in the embodiment is theoretical
Absorbance maximum is 50mg/g)
Embodiment 3：
The biological carbon composite of beta cyclodextrin chitosan walnut shell prepared by embodiment 1 is applied to hexavalent chromium waste water
Processing, comprise the following steps：The hexavalent chromium solution that 50mL initial concentrations are 100mg/L is taken, the pH value of regulation solution is 2.0,
Add beta cyclodextrin chitosan biological carbon composite made from embodiment 1, the consumption of the compound is 0.1g/L, respectively 25,
35 and 45 DEG C of thermostatic control oscillator vibration carries out adsorption reaction, and the rotating speed of water-bath constant temperature oscillator is 160rpm, is taken after 24 hours
Go out to be placed in filter filtration on paper or quiescent setting takes upper solution, the separating adsorbent from solution, adsorption process terminates, with ultraviolet point
Light photometry determines the content of Cr VI not to be adsorbed in waste water, and the adsorbance of calculating the results are shown in Table 2.
Table 2：Adsorbance data of the beta cyclodextrin chitosan biological carbon composite to chromium under condition of different temperatures
As shown in Table 2, it is that the compound is 47.4mg/g to the adsorbance of chromium ion under conditions of 25 DEG C in reaction temperature,
And be slightly increased with the increase of initial temperature, when temperature is 45 DEG C, adsorbance reaches 49.7mg/g.(the chromium in the embodiment
Solution theory absorbance maximum is 50mg/g)
Embodiment 4：
The biological carbon composite of beta cyclodextrin chitosan walnut shell prepared by embodiment 1 is applied to hexavalent chromium waste water
Processing, comprise the following steps：The hexavalent chromium solution that 50mL initial concentrations are 100mg/L is taken, the pH value of regulation solution is 2.0,
Beta cyclodextrin chitosan biological carbon composite made from embodiment 1 is added, the consumption of the adsorbent is 0.1g/L, in 25 DEG C of perseverances
Tepidarium oscillator carries out vibration adsorption reaction, and rotating speed is 160rpm, adsorption reaction starts 5,10,30,120,360,720,
Taking-up is placed in filter filtration on paper after 1080 and 1440 minutes or quiescent setting takes upper solution, the separating adsorbent from solution, inhales
Attached process terminates, with the content of Cr VI not to be adsorbed in determined by ultraviolet spectrophotometry each sample, the adsorbance knot of calculating
Fruit is shown in Table 3.
Table 3：Adsorbance data of the beta cyclodextrin chitosan biological carbon composite to chromium under the differential responses time
As shown in Table 3, growth over time, the compound gradually increases the adsorbance of crome metal, after 24 hours
Increases slowly, basically reach adsorption equilibrium.(the theoretical absorbance maximum of chromium solution in the embodiment is 50mg/g)
Embodiment 4：
The biological carbon composite of beta cyclodextrin chitosan walnut shell prepared by embodiment 1 is applied to hexavalent chromium waste water
Processing, comprise the following steps：The hexavalent chromium solution that four initial concentrations are respectively 20,50,100 and 200mg/L is taken, is adjusted molten
The pH value of liquid is 2.0, adds beta cyclodextrin chitosan biological carbon composite made from embodiment 1, and the consumption of the compound is
0.1g/L, carries out vibration adsorption reaction, the rotating speed of water-bath constant temperature oscillator is 160rpm, and 24 is small in 25 DEG C of thermostatic control oscillator vibrations
When after take out be placed in filter filtration on paper or quiescent setting take upper solution, the separating adsorbent from solution, adsorption process terminates, use
The content of Cr VI not to be adsorbed in determined by ultraviolet spectrophotometry waste water, the adsorbance of calculating the results are shown in Table 4.
Table 4：Adsorbance data of the beta cyclodextrin chitosan biological carbon composite to chromium under differential responses initial concentration
As shown in Table 4, the compound is to the adsorbance of Cr VI under conditions of initial concentration is 20mg/L
10.05mg/g, and increase with initial concentration and increase, adsorbance reaches 79.25mg/g when initial concentration is 82.3mg/L.
It the above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
With various process programs of the present inventive concept without substantial differences in protection scope of the present invention.
Claims (4)
1. a kind of utilization beta cyclodextrin chitosan biological carbon composite removes the method for hexavalent chromium in waste water, methods described
Comprise the following steps：The composite, composite usage amount are added in containing the hexavalent chromium wastewater that concentration is 20~800mg/L
For 0.1~1g/L, regulation pH value is 2~9, in the thermostatic control oscillator vibration that reaction temperature is 20~50 DEG C, controls oscillator
100~160 revs/min of rotating speed, 1~24h of oscillating reactions, reaction is placed in filter filtration on paper after terminating or quiescent setting takes upper strata molten
Liquid, the separating adsorbent from solution completes the removal to hexavalent chromium；The chitosan-modified composite of the beta cyclodextrin
Adsorbent is through the following steps that prepare：(1) chitosan of 6g beta cyclodextrins and 1g is dissolved in 120ml 1mol/L salt
Acid solution, is added in three-necked bottle, stir to obtain milky white solution, when being heated to 85 DEG C or so bleach, and the penta of dropwise addition 50%
Dialdehyde 3ml, faint yellow taking-up is changed into after continuing heating response 1h；
(2) the product regulation pH value in (1) to 7~8 is changed into after brown with 1mol/L NaOH solution, cooled down, precipitation, mistake
Filter, dry beta cyclodextrin chitosan product；
(3) it will dry and wear into granular walnut shell biomass and be put into tube furnace, and 300~600 DEG C, lead to N2, 1~2h is burnt, is produced
To walnut shell charcoal, obtained magnetic bio charcoal is washed with deionized 2~3 times, 50~60 DEG C of drying, grinding crosses 150
Mesh sieve；
(4) take 2g walnut shell charcoal to be dissolved in 200ml ultra-pure waters, be put into ultrasonic disperse 2h in ultrasonic case, add
PH to 7.0 is adjusted after 0.1M each 50ml of NHS and EDC, then continuing magnetic force stirring 2.5h；
(5) take in charcoal suspension of the beta cyclodextrin chitosan product in 4g (2) in (4), add 10ml glutaraldehydes, surpass
Sound disperses 10min, is placed in 65 DEG C and vibrates 2h, then adjusts pH to 7.0, and filtering, 50 DEG C of drying, excessively grinding, 150 mesh sieves obtain β
Cyclodextrin chitosan biological charcoal composite material adsorbent.
2. utilization beta cyclodextrin chitosan biological carbon composite according to claim 1 removes hexavalent chromium in waste water
Method, it is characterised in that：The concentration of hexavalent chromium is controlled in 20~800mg/L in the waste water.
3. utilization beta cyclodextrin chitosan biological carbon composite according to claim 1 removes hexavalent chromium in waste water
Method, it is characterised in that：The pH value of the adsorption reaction is 2~9.
4. utilization beta cyclodextrin chitosan biological carbon composite according to claim 1 removes hexavalent chromium in waste water
Method, it is characterised in that：The adsorption reaction temperature is 20~50 DEG C.
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| CN111001397B (en) * | 2019-12-31 | 2022-11-18 | 东北农业大学 | Method for synthesizing beta-cyclodextrin conjugated biochar by microwave-assisted one-pot method and application thereof |
| CN111215036A (en) * | 2020-01-10 | 2020-06-02 | 北京工业大学 | Preparation method and application of EDTA (ethylene diamine tetraacetic acid) modified magnetic chitosan cyclodextrin adsorbent |
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| CN115925078A (en) * | 2022-12-29 | 2023-04-07 | 咸阳师范学院 | Method for treating heavy metal ions in sewage |
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| US5906960A (en) * | 1995-08-15 | 1999-05-25 | Arctech, Inc. | Adsorbent |
| CN104787831A (en) * | 2015-03-23 | 2015-07-22 | 湖南大学 | Method for removing hexavalent chromium in wastewater through magnetic adsorbent compounded by chitosan and magnetic biological carbon |
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