CN105251466A - Preparation method and application of magnetic chitosan lignosulfonate graphene oxide adsorbent - Google Patents
Preparation method and application of magnetic chitosan lignosulfonate graphene oxide adsorbent Download PDFInfo
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- CN105251466A CN105251466A CN201510647899.0A CN201510647899A CN105251466A CN 105251466 A CN105251466 A CN 105251466A CN 201510647899 A CN201510647899 A CN 201510647899A CN 105251466 A CN105251466 A CN 105251466A
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Abstract
The invention discloses a preparation method and application of a magnetic chitosan lignosulfonate graphene oxide adsorbent. The adsorbent comprises a graphene oxide matrix, and the surface of the matrix is grafted with a magnetic chitosan lignosulfonate complex and contains a large quantity of oxygen-containing functional groups and aromatic groups. The preparation method includes the steps that first, a graphene oxide solution and magnetofluid are prepared; then, magnetic chitosan and sodium lignosulphonate are compounded; next, graphene oxide and the magnetic chitosan lignosulfonate complex are combined, and washing, drying, grinding and screening are performed to obtain the final product. The product has an excellent adsorption effect on methylene blue dye, has the advantages of being wide in raw material source, low in cost, large in adsorption quantity, easy to separate and recycle, free of secondary pollution and the like and can be used for treating wastewater in printing and dyeing mills, chemical plants and the like.
Description
Technical field
The invention belongs to environment functional material and water treatment new technical field, be specifically related to a kind of preparation method and its usage of chitosan magnetic lignosulfonates graphene oxide adsorbent.
Background technology
Water body dye discoloration endangers larger problem of environmental pollution.Methylene blue dye, as a kind of phenthazine salt, is widely used in cotton, fiber crops, silk fabric, the dyeing of paper and the painted of bamboo and wood, has a large amount of wastewater containing methylene blues to discharge every year.Although the toxicity of methylene blue is not very strong, still environment and biology are harmful to.The methylene blue of low dosage is just enough to affect attractive in appearance, transparency and the gas solubility of water body, and then affects hydrobiological existence, destroys the ecological balance.And a large amount of methylene blues is once enter in human body, dizziness, vomiting can be caused, feel sick, diarrhoea, cyanosis, jaundice, quadriplegia, necrosis, even carcinogenic lethal, serious threat is caused to the health of the mankind.Therefore, wastewater containing methylene blue must effectively process before it is discharged into natural water.The method of current degradation of methylene blue mainly contains absorption method, hyperfiltration, ion-exchange, the precipitation method, Fenton's reaction edman degradation Edman, oxidation degradation method etc.Compared with additive method, absorption method because its operating cost is low, efficiency is high, the advantage such as strong adaptability, easy to operate, the reusing of adsorbent, secondary pollution be little and receive increasing concern, conventional adsorbent has biological carbon, montmorillonite, CNT etc.But most sorbing material due to its low adsorption capacity, difficult be separated and produce secondary pollution and limit its practical application, therefore prepare a kind of sorbing material that can address these problems there is very large realistic meaning.
Graphene oxide, as the important derivatives of Graphene, not only inherits the advantage of the huge specific area of the Graphene fragrant multi-layer sheet structure orderly with arrangement, and introduces a large amount of oxygen-containing functional groups as carboxyl, epoxy radicals, carboxyl etc.The introduction of these functional groups as adsorption site adsorption fouling thing, but can add its hydrophilicity simultaneously, makes it be difficult to afterwards be separated from waste water in absorption.Directly adding magnetic to graphene oxide is a good selection, but can occupy adsorption site like this, thus reduces adsorption capacity.In order to ensure adsorption capacity, reaching segregative object simultaneously, introducing magnetic fluid, shitosan and lignosulfonates.Shitosan, also known as chitosan, is that the chitin extensively existed by nature obtains through deacetylation, has biodegradability, good biocompatibility, be rich in a large amount of amino and hydroxyl.Sodium lignin sulfonate is the important by-products of China's paper industry, wide material sources, is also a kind of natural polymers simultaneously, has very strong dispersiveness and undefined structure, containing a large amount of hydroxyls and aromatic structure.By being loaded on shitosan by magnetic nano-particle, then form floccule with sodium lignin sulfonate, floccule is combined with graphene oxide the most at last, material is so not only made to have magnetic, easily separated, and introduce a large amount of oxygen-containing functional groups and aromatic structure, ensure the adsorption capacity of material.
Summary of the invention
Technical problem to be solved by this invention is: for existing technical problem, researches and develops a kind of efficient, easily separated, environmentally friendly chitosan magnetic lignosulfonates graphene oxide adsorbent that can be used for processing methylene blue in waste.
The present invention proposes a kind of preparation method of chitosan magnetic lignosulfonates graphene oxide adsorbent, to surface of graphene oxide by the grafting of chitosan magnetic lignosulfonates complex, the adsorbent of such preparation realizes quick separating by externally-applied magnetic field, the introducing of shitosan and lignosulfonates makes adsorbent contain more oxygen-containing functional group and aromatic radical, and concrete steps are as follows:
(1) by 2.0 ~ 6.0g graphite powder, 1.0 ~ 5.0gK
2s
2o
8, 1.0 ~ 5.0gP
2o
5be mixed to join 8 ~ 24mLH
2sO
4in (95% ~ 98%), 4 ~ 5h is stirred under the water bath condition of 70 ~ 80 DEG C, 0.3 ~ 1.0L ultra-pure water is added after being cooled to room temperature, place 12h, the product obtained is washed to neutrality, vacuum drying at 50 ~ 80 DEG C again, joins dried product the H that 80 ~ 240mL temperature is 0 ~ 4 DEG C
2sO
4in (95% ~ 98%), then add 1.0 ~ 5.0gNaNO
3with 10.0 ~ 40.0gKMnO
4, at 0 ~ 4 DEG C, stir 2 ~ 3h, add 100 ~ 500mL ultra-pure water, under 90 ~ 100 DEG C of conditions, stir 1 ~ 2h, then add 0.3 ~ 1.0L ultra-pure water and 10 ~ 40mLH
2o
2(20 ~ 40wt%), stirred at ambient temperature 2 ~ 3h, then use HCl (5 ~ 10%) and ultra-pure water cleaning to neutral, and constant volume, ultrasonic disperse 2h at 30 ~ 50 DEG C, obtains the graphene oxide that mass concentration is 2.0 ~ 6.0g/L;
(2) 100 ~ 120mLFe is got
3+(0.4 ~ 0.6M) and 100 ~ 120mLFe
2+(0.2 ~ 0.4M) solution mixes, NaOH (100 ~ 200g/L) is added until pH is 8.5 ~ 9.5 under 50 ~ 60 DEG C of water bath condition, after stirring 10min, temperature rises to 60 ~ 70 DEG C, add 0.6 ~ 0.8mL Tween 80 again, reconcile pH after Keep agitation 30 ~ 50min to neutral, wash 3 times, ultrasonic disperse 40min at 30 ~ 50 DEG C, constant volume obtains the magnetic fluid that mass concentration is 30 ~ 40g/L;
(3) get 1.0 ~ 2.0g shitosan to be added in 50 ~ 100mL acetic acid (1 ~ 2wt%) and to dissolve completely at 40 ~ 50 DEG C, add 10 ~ 20mL magnetic fluid, pH to 5.5 ~ 6.5 are regulated after Keep agitation 30min, then sodium lignin sulfonate (20g/L is dropwise added, pH=5.5 ~ 6.5) form floccule, add 5 ~ 10mL glutaraldehyde (1 ~ 2wt%) to be again cross-linked, at 60 DEG C, react 2 ~ 3h, for subsequent use;
(4) under room temperature, 0.02 ~ 0.03MEDC and 0.05 ~ 0.06MNHS is added in (1), Keep agitation 2 ~ 3h obtains the graphene oxide solution of activated carboxyl, after (3) are added reaction 2 ~ 3h, add 5 ~ 10mL glutaraldehyde (1 ~ 2wt%) to be again cross-linked, 2 ~ 3h is reacted at 60 DEG C, dropwise add NaOH, regulate pH to 8.0 ~ 10.0, final product ultra-pure water is washed till neutrality, vacuum drying at 50 ~ 60 DEG C, grinding, 150 orders sieve, and namely obtain chitosan magnetic lignosulfonates graphene oxide composite material adsorbent.
In above-mentioned preparation method, the order of preparation first prepares graphene oxide solution and magnetic fluid, then by chitosan magnetic and sodium lignin sulfonate compound, then is combined with chitosan magnetic sodium lignin sulfonate complex by graphene oxide.
In above-mentioned preparation method, described Fe
2+for in ferrous sulfate and frerrous chloride any one, described Fe
3+for in ferric trichloride and ferric sulfate any one.
The methylene blue in waste water removed by the chitosan magnetic lignosulfonates graphene oxide adsorbent utilizing the inventive method to prepare.
In above-mentioned application, described adsorbent is consumption preferably 0.5 ~ 1.0g/L in waste water, and methylene blue initial concentration is 20 ~ 500mg/L.
In above-mentioned application, the condition preferable ph of described adsorption reaction is 2.0 ~ 11.0, and the reaction time is 5 ~ 1440min, and temperature is 20 ~ 50 DEG C.
Compared with prior art, the invention has the advantages that:
1. the raw material sources used is extensive, and cheap, preparation method and simple to operate, does not need special chemical industry equipment, effectively can realize suitability for industrialized production.
2. chitosan magnetic lignosulfonates graphene oxide adsorbent site of the present invention is many, high to the removal efficiency of methylene blue in waste, and it has answering property of magnetic, easily separation and recovery from solution.
3. product is nontoxic, can not produce secondary pollution after absorption, environmentally friendly.
Accompanying drawing explanation
Fig. 1 is the ESEM schematic diagram of the chitosan magnetic lignosulfonates graphene oxide adsorbent of the embodiment of the present invention 1;
Fig. 2 is the B-H loop schematic diagram of the chitosan magnetic lignosulfonates graphene oxide adsorbent of the embodiment of the present invention 1;
Detailed description of the invention
Below with reference to Figure of description and specific embodiment, the present invention is described in further details.
Embodiment 1:
A kind of chitosan magnetic lignosulfonates graphene oxide adsorbent of the present invention, this adsorbent comprises graphene oxide matrix, and on matrix, load is magnetic shitosan lignosulfonates complex.This adsorbent is prepared by following methods:
1) by 6.0g graphite powder, 5.0gK
2s
2o
8, 5.0gP
2o
5be mixed to join 24mLH
2sO
4(98%) in, under the water bath condition of 80 DEG C, stir 4.5h, after being cooled to room temperature, add 1L ultra-pure water, place 12h, the product obtained is washed to neutrality, then vacuum drying at 60 DEG C, dried product is joined the H that 240mL temperature is 0 ~ 4 DEG C
2sO
4(98%) in, then 5.0gNaNO is added
3and 30gKMnO
4, at 0 ~ 4 DEG C, stir 2h, add 500mL ultra-pure water, under 90 DEG C of conditions, stir 2h, then add 1L ultra-pure water and 30mLH
2o
2(30wt%), stirred at ambient temperature 2h, then use HCl (10%) and ultra-pure water cleaning to neutral, and constant volume, ultrasonic disperse 2h at 40 DEG C, obtains the graphene oxide that mass concentration is 5.0g/L;
(2) 120mLFe is got
3+(0.6M) and 120mLFe
2+(0.4M) solution mixing, NaOH (200g/L) is added until pH is 9.0 under 55 DEG C of water bath condition, after stirring 10min, temperature rises to 65 DEG C, add 0.8mL Tween 80 again, reconcile pH after Keep agitation 30min to neutral, wash 3 times, ultrasonic disperse 40min at 40 DEG C, constant volume obtains the magnetic fluid that mass concentration is 40g/L.
(3) get 1.0g shitosan to be added in 50mL acetic acid (1wt%) and to dissolve completely at 50 DEG C, add 10mL magnetic fluid, pH to 6.5 is regulated after Keep agitation 30min, then sodium lignin sulfonate (20g/L is dropwise added, pH=6.5) floccule is formed, add 5mL glutaraldehyde (1wt%) to be again cross-linked, at 60 DEG C, react 2h, for subsequent use;
(4) 0.03MEDC and 0.06MNHS is added in (1) under room temperature, Keep agitation 2h obtains the graphene oxide solution of activated carboxyl, (3) are added reaction 2h after, then add 5mL glutaraldehyde (1wt%) be cross-linked, 2h is reacted at 60 DEG C, dropwise add NaOH, regulate pH to 9.0, final product ultra-pure water is washed till neutrality, vacuum drying at 60 DEG C, grinding, 150 orders sieve, and namely obtain described adsorbent.
Above-mentioned obtained chitosan magnetic lignosulfonates graphene oxide adsorbent outward appearance is black, observes under being placed on ESEM, its exterior appearance as shown in Figure 1, the many folds of adsorbent surface.Fig. 2 is the hysteresis graph of chitosan magnetic lignosulfonates graphene oxide, shows that adsorbent possesses good superparamagnetism.
Embodiment 2:
Chitosan magnetic lignosulfonates graphene oxide adsorbent embodiment 1 prepared is applied to the process of methylene blue waste water, comprise the following steps, get the methylene blue solution 20mL that ten parts of initial concentrations are 50mg/L, 2 are respectively with NaOH or salt acid for adjusting pH, 3, 4, 5, 6, 7, 8, 9, 10, 11, add 10mg adsorbent respectively, be placed in constant temperature water bath vibration case, temperature is regulated to be 30 DEG C, rotating speed is 160rpm, take out after reaction 24h, with magnet, adsorbent is separated from waste water, under wavelength is 665nm condition with in ultraviolet specrophotometer wastewater measurement not by the methylene blue count adsorbed, the adsorbance result calculated is as shown in table 1:
Table 1: different pH value removes the impact of methylene blue in waste to chitosan magnetic lignosulfonates graphene oxide
As shown in Table 1, there is impact to absorption in condition of different pH.More favourable to the removal of methylene blue when pH is higher, when pH is 10, adsorbance reaches maximum.(the theoretical adsorbance maximum of the methylene blue in this embodiment is 100mg/g)
Embodiment 3:
Chitosan magnetic lignosulfonates graphene oxide adsorbent embodiment 1 prepared is applied to the process of methylene blue waste water, comprise the following steps: get five parts of 20mL methylene blue solution initial concentrations and be respectively 20, 50, 100, 100, 200mg/L, adjust ph is 10, add 10mg adsorbent respectively, be placed in constant temperature water bath vibration case, temperature is regulated to be 30 DEG C, rotating speed is 160rpm, take out after reaction 24h, with magnet, adsorbent is separated from waste water, under wavelength is 665nm condition with in ultraviolet specrophotometer wastewater measurement not by the methylene blue count adsorbed, the adsorbance result calculated is as shown in table 2:
Table 2: different initial concentration is on the impact of chitosan magnetic lignosulfonates graphene oxide adsorbed water Methylene Blue
As shown in Table 2, be the adsorbance that under the condition of 20mg/L, this adsorbent has 39.92mg/g at initial concentration, and increase with initial concentration and increase, substantially reach stable after being increased to certain value.
Embodiment 4:
Chitosan magnetic lignosulfonates graphene oxide adsorbent embodiment 1 prepared is applied to the process of methylene blue waste water, comprise the following steps: get the methylene blue solution that initial concentration is 100mg/L, the pH value regulating solution is 10, add 10mg adsorbent respectively, be placed in constant temperature water bath vibration case, temperature is regulated to be 30 DEG C, rotating speed is 160rpm, adsorption reaction starts 5, 30, 60, 120, 180, 350, take out after 720min, with magnet, adsorbent is separated from waste water, under wavelength is 665nm condition with in ultraviolet specrophotometer wastewater measurement not by the methylene blue count adsorbed, the adsorbance result calculated is as shown in table 4:
Table 3: the differential responses time is on the impact of chitosan magnetic lignosulfonates graphene oxide ink alkene adsorbed water Methylene Blue
As shown in Table 3, along with the growth of time, the adsorbance of this adsorbent to methylene blue increases gradually, increasess slowly after 3 hours, substantially reaches adsorption equilibrium.
Below be only the preferred embodiment of the present invention, protection scope of the present invention be not only confined to above-described embodiment, conceives various process programs without substantial differences all in protection scope of the present invention with the present invention.
Claims (5)
1. a chitosan magnetic lignosulfonates graphene oxide adsorbent, it is characterized in that described adsorbent comprises graphene oxide matrix, grafting chitosan magnetic lignosulfonates complex on matrix, the final material obtained is containing a large amount of oxygen-containing functional group and aromatic radical.
2. a preparation method for chitosan magnetic lignosulfonates graphene oxide adsorbent as claimed in claim 1, comprises step:
(1) by 2.0 ~ 6.0g graphite powder, 1.0 ~ 5.0gK
2s
2o
8, 1.0 ~ 5.0gP
2o
5be mixed to join 8 ~ 24mLH
2sO
4in (95% ~ 98%), 4 ~ 5h is stirred under the water bath condition of 70 ~ 80 DEG C, 0.3 ~ 1.0L ultra-pure water is added after being cooled to room temperature, place 12h, the product obtained is washed to neutrality, vacuum drying at 50 ~ 80 DEG C again, joins dried product the H that 80 ~ 240mL temperature is 0 ~ 4 DEG C
2sO
4in (95% ~ 98%), then add 1.0 ~ 5.0gNaNO
3with 10.0 ~ 40.0gKMnO
4, at 0 ~ 4 DEG C, stir 2 ~ 3h, add 100 ~ 500mL ultra-pure water, under 90 ~ 100 DEG C of conditions, stir 1 ~ 2h, then add 0.3 ~ 1.0L ultra-pure water and 10 ~ 40mLH
2o
2(20 ~ 40wt%), stirred at ambient temperature 2 ~ 3h, then use HCl (5 ~ 10%) and ultra-pure water cleaning to neutral, and constant volume, ultrasonic disperse 2h at 30 ~ 50 DEG C, obtains the graphene oxide that mass concentration is 2.0 ~ 6.0g/L;
(2) 100 ~ 120mLFe is got
3+(0.4 ~ 0.6M) and 100 ~ 120mLFe
2+(0.2 ~ 0.4M) solution mixes, NaOH (100 ~ 200g/L) is added until pH is 8.5 ~ 9.5 under 50 ~ 60 DEG C of water bath condition, after stirring 10min, temperature rises to 60 ~ 70 DEG C, add 0.6 ~ 0.8mL Tween 80 again, regulate pH to neutral after Keep agitation 30 ~ 50min, wash 3 times, ultrasonic disperse 40min at 30 ~ 50 DEG C, constant volume obtains the magnetic fluid that mass concentration is 30 ~ 40g/L;
(3) get 1.0 ~ 2.0g shitosan to be added in 50 ~ 100mL acetic acid (1 ~ 2wt%) and to dissolve completely at 40 ~ 50 DEG C, add 10 ~ 20mL magnetic fluid, pH to 5.5 ~ 6.5 are regulated after Keep agitation 30min, then sodium lignin sulfonate (20g/L is dropwise added, pH=5.5 ~ 6.5) form floccule, add 5 ~ 10mL glutaraldehyde (1 ~ 2wt%) to be again cross-linked, at 60 DEG C, react 2 ~ 3h, for subsequent use;
(4) under room temperature, 0.02 ~ 0.03MEDC and 0.05 ~ 0.06MNHS is added in (1), Keep agitation 2 ~ 3h obtains the graphene oxide solution of activated carboxyl, after (3) are added reaction 2 ~ 3h, add 5 ~ 10mL glutaraldehyde (1 ~ 2wt%) to be again cross-linked, 2 ~ 3h is reacted at 60 DEG C, dropwise add NaOH, regulate pH to 8.0 ~ 10.0, final product ultra-pure water is washed till neutrality, vacuum drying at 50 ~ 60 DEG C, grinding, 150 orders sieve, and namely obtain chitosan magnetic lignosulfonates graphene oxide composite material adsorbent.
3. the preparation method of chitosan magnetic lignosulfonates graphene oxide according to claim 2, it is characterized in that, the order of preparation first prepares graphene oxide solution and magnetic fluid, then by chitosan magnetic and sodium lignin sulfonate compound, then graphene oxide is combined with chitosan magnetic lignosulfonates complex obtains described product.
4. as a purposes for claim 2 chitosan magnetic lignosulfonates graphene oxide adsorbent, it is characterized in that, remove the methylene blue in waste water with described adsorbent.
5. the purposes according to right 4, is characterized in that, the consumption of described adsorbent in waste water is 0.5 ~ 1.0g/L.
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