CN106268637A - A kind of viscose rayon adsorbing material modified based on graphene oxide and preparation thereof and application - Google Patents
A kind of viscose rayon adsorbing material modified based on graphene oxide and preparation thereof and application Download PDFInfo
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- CN106268637A CN106268637A CN201610665829.2A CN201610665829A CN106268637A CN 106268637 A CN106268637 A CN 106268637A CN 201610665829 A CN201610665829 A CN 201610665829A CN 106268637 A CN106268637 A CN 106268637A
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- graphene oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- 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 a kind of viscose rayon adsorbing material modified based on graphene oxide and preparation thereof and application, adsorbing material raw material includes: graphene oxide and viscose rayon；Preparation: configuration graphene oxide solution, is then uniformly sprayed at graphene oxide on viscose rayon.It is applied to dye adsorption.The viscose rayon adsorbing material adsorbance of graphene oxide modification prepared by the present invention is big, and method is simple to operate, and reaction condition is gentle, the most less, low cost, it is adaptable to large-scale production.
Description
Technical field
The invention belongs to adsorbing material and preparation thereof and application, particularly to a kind of based on graphene oxide modification
Viscose rayon adsorbing material and preparation thereof and application.
Background technology
China is textile printing and dyeing industry the first big country, and textile printing and dyeing industry is the discharge rich and influential family of industrial wastewater, contains in waste water
Having substantial amounts of dyestuff, wherein during Colour Difference, the dyestuff of 10-20% is discharged in waste water, therefore, to Wastewater Dyes
Process also is that we need the root problem of solution.
Fiber-like adsorbing material intramolecular has a lot of hydroxy groups, and has the characteristic of porous, and people pass through chemical modification,
Improve its absorption property.Viscose rayon belongs to regenerated celulose fibre, has preferable adsorptivity.Have been reported viscose rayon with
Carbon fibe can make the viscose rayon of high adsorption.
Graphene and its derivant have many inherent advantages as adsorbing material.First, Graphene is monolayer
Structure, all of atom is all surface atom, thus Graphene has great specific surface area.The active adsorption surface of Graphene
It is even more taller than CNTs, this is because pollutant are difficult to diffuse into the inner surface of CNTs.Secondly, with traditional absorption
Agent is compared, and pollutant absorption on Graphene adsorbing material has adsorption dynamics adsorption kinetics faster.The hole of Graphene adsorbing material
Shape structure makes pollutant have higher diffusion rate, and directly results in the higher rate of adsorption.Furthermore, compare other efficient
Adsorbing material, the production cost of Graphene adsorbing material is lower.Finally, Graphene adsorbing material can process multiple pollution simultaneously
Thing.Graphene adsorbing material processes heavy metal, dyestuff, little molecular organic pollutants and greasy dirt etc. higher adsorbance.For
The demand that adaptation is different, the functionalization of Graphene adsorbing material is important channel.Wherein utilizing more is graphene oxide,
It is most important material with carbon element adsorbent, because it is cheap, be readily produced, adsorbance is big.
Summary of the invention
The technical problem to be solved is to provide a kind of viscose rayon adsorption material modified based on graphene oxide
Expecting and prepare and application, the inventive method is quick, easy, effective, be applicable to scale operates.
A kind of viscose rayon adsorbing material modified based on graphene oxide of the present invention, described adsorbing material raw material bag
Including: graphene oxide and viscose rayon, wherein graphene oxide, the ratio of viscose rayon are 150～300mg:300～600mg.
A kind of preparation method of the viscose rayon adsorbing material modified based on graphene oxide of the present invention, including:
Configuration graphene oxide solution, then graphene oxide is uniformly sprayed on viscose rayon, dry, obtain based on
The viscose rayon adsorbing material that graphene oxide is modified.
The concentration of described graphene oxide solution is 15-20mg/ml.
Described drying is the oven for drying at 55-65 DEG C.
The application of a kind of viscose rayon adsorbing material modified based on graphene oxide of the present invention, is applied to the suction of dyestuff
Attached, particularly as follows: the viscose rayon adsorbing material modified based on graphene oxide is joined in dye solution, concussion, then survey
The modified viscose rayon of examination graphene oxide is to the clearance of dye solution and maximal absorptive capacity.
Described dye solution is malachite green oxalate dye solution, and concentration is 25～60.00mg/ml, volume be 10～
50.00ml。
The described viscose rayon adsorbing material modified based on graphene oxide is 450～900mg:250 with the ratio of dyestuff
～3000mg.
Described concussion is: shaking table shakes, and the concussion time is 10～150 minutes, and concussion speed is 100-150 beat/min.
The modified viscose rayon of test graphene oxide is to the clearance of dye solution and maximal absorptive capacity: utilize ultraviolet to divide
Light photometer is at wavelength 619nm, and before and after detection absorption, the absorbance of dye solution changes, and is calculated clearance and maximum
Adsorbance.
The preparation of graphene oxide in the present invention, particularly as follows:
A () pre-oxidizes: by K2S2O8、P2O5, concentrated sulphuric acid mixing, under 80-100 DEG C of water bath condition, stirring, add Graphene,
Reaction, sucking filtration, washs, dries, and obtains pre-oxidised samples；Wherein K2S2O8、P2O5, concentrated sulphuric acid, the ratio of Graphene be 15～
20g:15～20g:70～90ml:15～20g；
B () aoxidizes: under condition of ice bath, join in concentrated sulphuric acid by above-mentioned pre-oxidised samples, dispersed, is subsequently adding
KMnO4After transfer in 35-45 DEG C of water-bath react, then in ice bath lower the temperature, constant volume, be subsequently adding H2O2, left undisturbed overnight；Acid
Purification；Fractional centrifugation, obtains graphene oxide；Wherein concentrated sulphuric acid, KMnO4、H2O2Ratio be 700～900ml:100～
110g:35～40ml.
Consumption K in described step (a)2S2O8It is 15～20g, P2O5Being 15～20g, concentrated sulphuric acid is 70～90ml.
In described step (b), consumption concentrated sulphuric acid is 700～900ml, KMnO4It is 100～110g, H2O2It is 35～40ml.
In described step (a), the response time is 10-40min.
Sucking filtration, washing in described step (a), dry for: add deionized water, then use buchner funnel sucking filtration, deionization
Water rinses, until pH value is 5～6, is placed on filter paper and overnight dries after terminating.
Described step (b) is lowered the temperature as being down to about 0-10 DEG C in ice bath.
Described step (b) acid purification is: after removing supernatant, rinses with PTFE film filtration, dilute hydrochloric acid, repeats 5～6 times,
Then it is washed with deionized, is centrifuged.
Described step (b) constant volume is that the liquid taken out in ice bath is divided into two, and is respectively charged into 2 2L round-bottomed flasks, and divides
It is not settled to 2L with deionized water.
Fractional centrifugation is broadly divided into two stages,
1) first stage: be centrifuged with less rotating speed and less time, remove deposit (centrifuge tube lower floor reunion shape thing
Matter), retain supernatant.
2) second stage: be centrifuged with bigger rotating speed and long period, remove supernatant, retain deposit, until supernatant
Liquid pH stable is about neutrality.
Described step (b) fractional centrifugation is divided into two stages, and wherein the first stage is: be centrifuged 5-with 500～1500rpm
10min, removes deposit, retains supernatant；Second stage is: rotating speed 8000～12000rpm is centrifuged 15～30min, removes
Supernatant, retains deposit, and washing is until supernatant pH stable is 6.4～7.0.
Beneficial effect
The viscose rayon adsorbing material of a kind of new graphene oxide modification of the present invention is as a kind of new adsorbent, energy
Effective absorbing dye, graphene oxide based on material with carbon element, not only can active adsorption, there is environmental protection, the effect such as nontoxic simultaneously,
Have a wide range of applications；
The viscose rayon adsorbing material adsorbance of graphene oxide modification prepared by the present invention is big, graphene oxide modification
When viscose rayon quality is 500mg, the adsorbance to dyestuff just can reach 800mg, and the inventive method is simple to operate simultaneously, instead
Answer mild condition, the most less, low cost, it is adaptable to large-scale production；
The present invention relates to a kind of Novel adsorption functions expanding based on graphene oxide kind of conventional adsorbent, with biography
The activated carbon of sorbent of system compares, the viscose rayon adsorbing material that graphene oxide is modified, and the rate of adsorption is high, and adsorbance is big,
The fields such as the process that can apply to Wastewater Dyes.
Accompanying drawing explanation
Fig. 1 is the SEM picture of the viscose rayon adsorbing material of middle graphene oxide modification；
Fig. 2 viscose rayon adsorbing material that to be viscose rayon modified to the clearance of malachite green oxalate dyestuff and graphene oxide
Clearance to malachite green oxalate dyestuff；
Fig. 3 is the viscose rayon adsorbing material of the graphene oxide modification adsorbance to malachite green oxalate dyestuff in embodiment 3.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
Step 1: first preparation mass concentration is the graphene oxide of 20mg/ml, and the quality of precise viscose rayon is
500mg。
Step 2: be sprayed on uniformly on viscose glue face paper by graphene oxide with spray gun, sprays graphene oxide 15ml,
It is placed on the oven for drying of 60 DEG C, obtains the viscose rayon adsorbing material that graphene oxide is modified.See the SEM of Fig. 1.
The mensuration of viscose rayon adsorption efficiency, comprises the steps:
Step 1: preparation mass concentration is that the malachite green oxalate dyestuff 200ml of 25.00mg/ml is stand-by.
Step 2: weigh 6 parts of 500mg viscose rayons and be put into respectively in the conical flask that 6 specifications are 50ml, in conical flask
Being separately added into the malachite green oxalate dyestuff 30ml that concentration is 25.00mg/ml, concussion speed is 100 beats/min.
Step 3: earthquake 20 minutes respectively, 40 minutes, 60 minutes, 80 minutes, 100 minutes, measures absorption when 120 minutes
Malachite green oxalate dye solution absorbance under 619nm front and back, is calculated as follows adsorption efficiency:
R (%)=(C0-Ct)/C0x 100
R is the t adsorption efficiency to malachite green oxalate dyestuff, C0And CtBe respectively malachite green oxalate dyestuff initial concentration and
In the concentration of t, see Fig. 2.
Embodiment 2
The mensuration of the viscose rayon adsorbing material adsorption efficiency that graphene oxide is modified, comprises the steps:
Step 1: preparation mass concentration is that the malachite green oxalate dyestuff 200ml of 25.00mg/ml is stand-by.
Step 2: weighing the modified viscose rayon of 6 parts of 500mg graphene oxides and being put into 6 specifications respectively is the taper of 50ml
In Ping, being separately added into the malachite green oxalate dyestuff 30ml that concentration is 25.00mg/ml in conical flask, concussion speed is 100 beats/min
Clock.
Step 3: earthquake 20 minutes respectively, 40 minutes, 60 minutes, 80 minutes, 100 minutes, measures absorption when 120 minutes
Malachite green oxalate dye solution absorbance under 619nm front and back, is calculated as follows adsorption efficiency:
R (%)=(C0-Ct)/C0x 100
R is the t adsorption efficiency to malachite green oxalate dyestuff, C0And CtBe respectively malachite green oxalate dyestuff initial concentration and
In the concentration of t, see Fig. 2.
From in Fig. 2: the percent of decolourization of the viscose rayon adsorbing material that graphene oxide is modified, within 20 minutes, percent of decolourization is the highest
Reaching 50%, when adsorption time is 80 minutes, percent of decolourization just can reach 85%, far above the decolouring of the activated carbon of homogenous quantities
Rate.
Embodiment 3
The mensuration of the viscose rayon adsorbing material adsorbance that graphene oxide is modified, comprises the steps:
Step 1: preparation mass concentration is 25.00mg/ml, 30.00mg/ml, 35.00mg/ml, 40.00mg/ml,
The malachite green oxalate dyestuff of 45.00mg/ml, 50.00mg/ml is stand-by.
Step 2: weighing the modified viscose rayon of 6 parts of 500mg graphene oxides and being put into 6 specifications respectively is the taper of 50ml
In Ping, being separately added into concentration in conical flask is 25.00mg/ml, 30.00mg/ml, 35.00mg/ml, 40.00mg/ml,
The malachite green oxalate dyestuff 30ml of 45.00mg/ml, 50.00mg/ml.6 conical flasks are placed on shaking table concussion 100 minutes, shake
Swinging speed is 100 beats/min.
Step 3: measure malachite green oxalate dye solution extinction under 619nm before and after absorption respectively under 6 variable concentrations
Degree,
It is calculated as follows adsorbance:
Q=(C0-Ct)V0/M
Q is the t adsorbance to malachite green oxalate dyestuff, mg/g；V0For initial soln volume, ml；C0And CtIt is respectively hole
The initial concentration of passeris montani saturati malachite green dyestuff and in the concentration of t, the quality of the viscose rayon that M graphene oxide is modified.For seeing Fig. 3.
Claims (10)
1. a viscose rayon adsorbing material based on graphene oxide modification, it is characterised in that: described adsorbing material raw material bag
Include: graphene oxide and viscose rayon, wherein the ratio 150～300mg:300～600mg of graphene oxide, viscose rayon.
2. a preparation method for the viscose rayon adsorbing material modified based on graphene oxide as claimed in claim 1, bag
Include: configuration graphene oxide solution, then graphene oxide is uniformly sprayed on viscose rayon, dries, obtain based on oxidation
The viscose rayon adsorbing material that Graphene is modified.
The preparation method of a kind of viscose rayon adsorbing material modified based on graphene oxide the most according to claim 2,
It is characterized in that: the concentration of described graphene oxide solution is 15-20mg/ml.
The preparation method of a kind of viscose rayon adsorbing material modified based on graphene oxide the most according to claim 2,
It is characterized in that: described sprinkling is for spray with spray gun.
The preparation method of a kind of viscose rayon adsorbing material modified based on graphene oxide the most according to claim 2,
It is characterized in that: described drying is: dry under the conditions of 55-65 DEG C.
6. an application for the viscose rayon adsorbing material modified based on graphene oxide as claimed in claim 1, its feature
It is: be applied to the absorption of dyestuff, particularly as follows: the viscose rayon adsorbing material modified based on graphene oxide is joined dyestuff
In solution, concussion, the viscose rayon that then test graphene oxide the is modified clearance to dye solution.
The application of a kind of viscose rayon adsorbing material modified based on graphene oxide the most according to claim 6, it is special
Levying and be: described dye solution is malachite green oxalate dye solution, concentration is 25～60.00mg/ml.
The application of a kind of viscose rayon adsorbing material modified based on graphene oxide the most according to claim 6, it is special
Levy and be: the described viscose rayon adsorbing material modified based on graphene oxide is 450～900mg:250 with the mass ratio of dyestuff
～3000mg.
The application of a kind of viscose rayon adsorbing material modified based on graphene oxide the most according to claim 6, it is special
Levy and be: described concussion is: shaking table shakes, and the concussion time is 10～150 minutes, and speed is 100～150 beats/min.
The application of a kind of viscose rayon adsorbing material modified based on graphene oxide the most according to claim 6, it is special
Levy and be: the modified viscose rayon of test graphene oxide is to the clearance of dye solution and maximal absorptive capacity: utilize ultraviolet to divide
Light photometer is at wavelength 619nm, and before and after detection absorption, the absorbance of dye solution changes, and is calculated clearance and maximum
Adsorbance.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108193298A (en) * | 2018-01-19 | 2018-06-22 | 杭州高烯科技有限公司 | A kind of preparation method of the regenerated celulose fibre of surface coating graphene oxide |
| CN110552077A (en) * | 2019-09-11 | 2019-12-10 | 长沙学院 | reduced graphene oxide doped electrospinning reinforced nanofiber material and preparation method and application thereof |
| CN113026347A (en) * | 2021-02-20 | 2021-06-25 | 河北科技大学 | Graphene oxide/fiber composite material and adsorption method thereof |
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Cited By (4)
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| CN110552077A (en) * | 2019-09-11 | 2019-12-10 | 长沙学院 | reduced graphene oxide doped electrospinning reinforced nanofiber material and preparation method and application thereof |
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Application publication date: 20170104 |