CN108579628A - A kind of kappa-carrageenan/graphene oxide gel bead and its preparation method and application - Google Patents
A kind of kappa-carrageenan/graphene oxide gel bead and its preparation method and application Download PDFInfo
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The present invention provides a kind of preparation methods of κ carragheens/graphene oxide gel bead, belong to field of waste water treatment.κ carragheens, graphene oxide and water are mixed, gel is obtained；Obtained gel is added drop-wise to balling-up in calcium chloride solution, obtains κ carragheens/graphene oxide gel bead.Graphene oxide is encapsulated in κ carragheen gel balls by the present invention, and κ carragheens/graphene oxide gel ball has been made.Being cross-linked with each other and accumulate due to graphene oxide and κ carragheens, κ carragheens/graphene oxide gel bead forms fine and close pore structure, hole increases the adsorption area of material, and there are many holes and fold in the inside of gel ball, the aperture for being doped with the pure carragheen gelled pill of gel ball aperture ratio of graphene oxide is small, fold is intensive, and hole and intensive fold provide big specific surface area for absorption organic dyestuff, improve adsorbance.
Description
Technical field
The present invention relates to technical field of waste water processing more particularly to a kind of kappa-carrageenan/graphene oxide gel bead and
Preparation method and application.
Background technology
Every year, the organic dyestuff more than 700,000 tons is widely used in the industrial circles such as leather, printing and dyeing, weaving and plastics.
About 15% organic dyestuff is discharged into environment during using dyestuff, therefore produces a large amount of Industry Waste
Water.Also, these organic dyestuff are toxic, nondegradable mostly, can generate harm to organism.Therefore by pollutant from ring
Removal is a research topic being of great significance in the water body of border.
As boiomacromolecule, natural polysaccharide is made of a large amount of glycogen rings being connected on long-chain, is distributed in plant mostly
In object, fungi, simultaneously as its is widely distributed, cheap, environmental-friendly, nontoxic etc., make its food, medicine, biology,
The fields such as environment have a wide range of applications.Long-chain in polysaccharide makes it have good adsorption applications potentiality with abundant hydroxyl,
A variety of natural polysaecharides adsorbents have been obtained for studying at present.Carragheen is the sulphur being obtained by extraction from some kinds of red algae
Esterification polysaccharide polymer polymer.Carragheen can be divided into 7 because of the difference of sulfate group content and position in its structure
Kind, wherein it is most commonly seen with kappa-carrageenan, using also most extensive.Kappa-carrageenan is mainly extracted from Eucheuma algae,
It is made of α (1 → the 3)-D- galactolipin -4- sulfate and β (1 → 4) -3,6- dehydration-D- galactolipin disaccharide units repeated.
Since kappa-carrageenan contains abundant hydroxyl and sulfonic acid group, can be used for adsorbing the Cationic organic dyes in water.Existing skill
In art, cellulose is extracted as raw material using bamboo shoots leftover bits and pieces and carries out modified as Luo Wen is superfine, add kappa-carrageenan and in epoxy
Chloropropane crosslinking under be prepared bamboo shoots composite hydrogel (referring to《The preparation and representation of modified bamboo shoots fiber water gel and its right
Methylene blue adsorption number performance study》, Luo Wen is superfine, modern food science and technology, 2015,31 (3):165~171), but exist to dye
Expect the low problem of adsorption capacity.
Invention content
In consideration of it, the purpose of the present invention is to provide a kind of kappa-carrageenan/graphene oxide gel bead and its preparation sides
Method and the application in waste water absorption.Kappa-carrageenan/the graphene oxide gel obtained using preparation method provided by the invention
Bead has fine and close pore structure, improves adsorption capacity.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
A kind of preparation method of kappa-carrageenan/graphene oxide gel bead, includes the following steps：
(1) kappa-carrageenan, graphene oxide and water are mixed, obtains gel, kappa-carrageenan mass concentration in the gel
It is 0.5%~1.5%；
(2) gel that the step (1) obtains is added drop-wise to balling-up in calcium chloride solution, obtains kappa-carrageenan/oxidation stone
Black alkene gelled pill.
Preferably, the volume ratio of the quality of kappa-carrageenan, the quality of graphene oxide and water is in the step (1)
0.5g:0.1~0.3g:35~100mL.
Preferably, the volume ratio of the quality of the kappa-carrageenan, the quality of graphene oxide and water is 0.5g:0.1~
0.3g:50mL。
Preferably, in the step (2) calcium chloride solution a concentration of 0.5mol/L.
Preferably, the amount ratio of gel and calcium chloride solution is 1g in the step (2):5mL~3g:50mL.
Preferably, further include after balling-up in the step (2)：Obtained balling-up system is cured and washed successively, is obtained
Kappa-carrageenan/graphene oxide gel bead.
Kappa-carrageenan/the graphene oxide gel obtained the present invention also provides preparation method described in above-mentioned technical proposal is small
Ball, including kappa-carrageenan and the graphene oxide that is encapsulated in the kappa-carrageenan.
Preferably, the mass ratio of the kappa-carrageenan and graphene oxide is 5：1~3；
Also contain residual calcium ion in the kappa-carrageenan/graphene oxide gel bead, the calcium ion is in κ-OK a karaoke club
Mass content in glue/graphene oxide gel bead is 6.60~7.89%.
Preferably, the average grain diameter of the kappa-carrageenan/graphene oxide gel bead is 2.87~2.99mm.
The present invention also provides the kappa-carrageenan described in above-mentioned technical proposal/graphene oxide gel beads in wastewater treatment
In application.
The present invention provides a kind of preparation methods of kappa-carrageenan/graphene oxide gel bead, by kappa-carrageenan, oxidation
Graphene and water mixing, obtain gel；Obtained gel is added drop-wise to balling-up in calcium chloride solution, obtains kappa-carrageenan/oxidation
Graphene gel bead.Graphene oxide (GO) is encapsulated in kappa-carrageenan gel ball (κ-Car GBs) by the present invention, is made
Kappa-carrageenan/graphene oxide gel ball (κ-Car/GO GBs).It is mutual due to graphene oxide and kappa-carrageenan (κ-Car)
Crosslinking and accumulation, kappa-carrageenan/graphene oxide gel bead form fine and close pore structure, and hole increases the adsorption plane of material
Product, and there are many holes and fold in the inside of gel ball, the pure OK a karaoke club glue gel of gel ball aperture ratio for being doped with graphene oxide is small
The aperture of ball is small, and fold is intensive, and hole and intensive fold provide big specific surface area for absorption organic dyestuff, improve absorption
Amount.Embodiment statistics indicate that, kappa-carrageenan produced by the present invention-graphene oxide gel bead holds the absorption of methylene blue
Amount up to arrives 662mg/g.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the absorption isotherm of four kinds of gelled pills of the invention；
Fig. 2 is the grain size distribution of four kinds of gelled pills of the invention；
Fig. 3 is the scanning electron microscope spectrogram of inventive gel bead；
Fig. 4 is the infrared spectrogram of graphene oxide of the present invention, four kinds of gelled pills and kappa-carrageenan；
Fig. 5 is the Raman figure of graphene oxide of the present invention, four kinds of gelled pills and kappa-carrageenan.
Specific implementation mode
The present invention provides a kind of preparation methods of kappa-carrageenan/graphene oxide gel bead, include the following steps：
(1) kappa-carrageenan, graphene oxide and water are mixed, obtains gel, kappa-carrageenan mass concentration in the gel
It is 0.5%~1.5%；
(2) gel that the step (1) obtains is added drop-wise to balling-up in calcium chloride solution, obtains kappa-carrageenan/oxidation stone
Black alkene gelled pill.
The present invention mixes kappa-carrageenan (κ-Car), graphene oxide (GO) and water, obtains gel, κ-in the gel
Carragheen mass concentration is 0.5%~1.5%.In the present invention, the quality of kappa-carrageenan, the quality of graphene oxide and water
Volume ratio is preferably 0.5g:0.1~0.3g:35~100mL, more preferably 0.5g:0.1~0.3g:50mL, most preferably
0.5g:0.2g:50mL.In the present invention, in the gel kappa-carrageenan mass concentration between 0.5%~1.5% can balling-up,
Concentration is too low to be unable to balling-up, and concentration is too high, and viscosity increase cannot be added drop-wise in calcium chloride solution.
The present invention does not have the source of the kappa-carrageenan, graphene oxide special restriction, using people in the art
Commercial goods known to member.
The present invention does not have the addition sequence of the kappa-carrageenan, graphene oxide and water special restriction, adopts with ability
Charging sequence known to field technique personnel adds water specifically, as first mixed kappa-carrageenan and graphite oxide.
The present invention does not have the concrete mode of the mixing special restriction, using mixing well known to those skilled in the art
Mode, specifically, such as ultrasound, the present invention does not have special restriction to the time of ultrasound, power, and raw material mixing can be made equal
It is even.
After obtaining gel, the gel is added drop-wise to balling-up in calcium chloride solution by the present invention, obtains kappa-carrageenan/oxidation stone
Black alkene gelled pill.In the present invention, the concentration of the calcium chloride solution is preferably 0.5mol/L.
In the present invention, the amount ratio of the gel and calcium chloride solution is preferably 1g:5mL~3g:50mL.The present invention is logical
The dosage for crossing control calcium chloride solution ensures that the concentration of calcium chloride in balling-up system reaches 0.1mol/L, and it is small can to obtain gel
Ball.
The present invention does not have the mode of the dropwise addition special restriction, and it is molten to be preferably added drop-wise to calcium chloride dropwise with syringe
In liquid.
In the present invention, preferably further include after the balling-up：Obtained balling-up system is cured and washed successively, κ-is obtained
Carragheen/graphene oxide gel bead (κ-Car/GO GBs.).
After balling-up, the present invention preferably cures obtained balling-up system.In the present invention, the solidification is preferably room
It is stood in calcium chloride solution under temperature, the concentration of the calcium chloride solution is preferably consistent with said program, and details are not described herein.
In the present invention, the cured time is preferably 1~3h, more preferably 2h；The solidification temperature is preferably room temperature, is not needed
Additional heating or cooling.In the present invention, the solidification can improve the stability of gelled pill.
After the completion of solidification, the present invention preferably washes cured product, and it is small to obtain kappa-carrageenan/graphene oxide gel
Ball.The present invention does not have special restriction to the dosage and number of washing, can rinse out extra calcium ion.
Kappa-carrageenan/the graphene oxide gel obtained the present invention also provides preparation method described in above-mentioned technical proposal is small
Ball, including kappa-carrageenan and the graphene oxide that is encapsulated in the kappa-carrageenan.
In the present invention, the average grain of the kappa-carrageenan/graphene oxide gel bead is preferably 2.87~2.99mm,
More preferably 2.88~2.97mm.
In the present invention, the mass ratio of the kappa-carrageenan and graphene oxide is preferably 5：1~3, more preferably 5：2；
Also contain residual calcium ion in the kappa-carrageenan/graphene oxide gel bead, the calcium ion is in kappa-carrageenan/oxidation stone
Mass content in black alkene gelled pill is preferably 6.60~7.89%, and more preferably 7.29~7.68%.
In the present invention, there are many holes and fold, κ-OK a karaoke club in the inside of the kappa-carrageenan/graphene oxide gel bead
The aperture smaller of the pure kappa-carrageenan gel ball of aperture ratio of glue/graphene oxide gel bead, with graphene oxide doped amount
Increase, aperture is smaller and smaller, and fold is more dense, these apertures and intensive fold are the impurity adsorbed in waste water, such as organic
Dyestuff provides big specific surface area, than the adsorbance higher of pure kappa-carrageenan gel ball.
The present invention also provides the kappa-carrageenan described in above-mentioned technical proposal/graphene oxide gel beads in wastewater treatment
In application.
In the present invention, the kappa-carrageenan/graphene oxide gel bead can be used for handling the waste water containing dyestuff, institute
It is preferably methylene blue to state dyestuff.
In the present invention, the waste water is preferred from the productions such as paper dyeing, cotton spinning fiber printing-dyeing industry, bast fibre spinning dyeing
Raw industrial wastewater.
In the present invention, the concentration of the methylene blue in waste is preferably 600mg/L；The kappa-carrageenan/oxidation stone
The quality of black alkene gelled pill and the volume ratio of waste water are preferably 11.5mg：20mL.
With reference to embodiment to kappa-carrageenan provided by the invention/graphene oxide gel bead and preparation method thereof and
Using being described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
The graphene oxide for weighing 0.5g kappa-carrageenans and 0.1g respectively is put into conical flask, and 50mL distilled water is then added
Ultrasonic certain time makes it be uniformly dispersed.Then it is dripped to syringe in the calcium chloride solution of 0.5M, it is solid in calcium chloride solution
After changing two hours, taking-up distilled water flushing falls extra calcium ion, finally obtains κ-Car/GO (5:1)GBs.
Embodiment 2
It is same as Example 1, the graphene oxide of 0.2g is differed only in, the κ-Car/GO (5 for being:2)GBs.
Embodiment 3
It is same as Example 1, the graphene oxide of 0.3g is differed only in, the κ-Car/GO (5 for being:3)GBs.
Comparative example
It is same as Example 1, it differs only in and does not add graphene oxide, the pure kappa-carrageenan gel ball for being
(κ-Car GBs)。
Adsorption test
In adsorption experiment, the gelled pill that the Examples 1 to 3 of dry weight 11.5mg and comparative example obtain is put into first
In 50mL conical flasks, 20mL, 600mg/L methylene blue solution are then added, is finally placed on 25 DEG C of water-bath constant temperature oscillator
Middle oscillation 12h.Sample is taken out, the gelled pill and solution of absorption methylene blue are separated, the ultraviolet-visible of the solution is measured
Spectrum, then calculates its concentration, Fig. 1 is the absorption isotherm of four kinds of gelled pills, and wherein a is：κ-Car GBs、b：κ-Car/GO
(5:1)GBs、c：κ-Car/GO(5:2)GBs、d：κ-Car/GO(5:3) GBs, from figure 1 it appears that pure κ-Car GBs
Adsorbance is minimum, and with the increase of graphene oxide doped amount, the adsorbance of kappa-carrageenan/graphene oxide gel ball is also therewith
Increase, up to 662mg/g.This may be because being cross-linked with each other and accumulating for graphene oxide and kappa-carrageenan, makes κ-card
Glue/graphene oxide gel ball is drawn to form fine and close pore structure, to improve adsorbance.This shows kappa-carrageenan/oxidation
Graphene gel ball has good absorption property, promises to be good Dye Adsorption material.
The grain size distribution of four kinds of gelled pills is shown in that Fig. 2, wherein a are：κ-Car GBs、b：κ-Car/GO(5:1)GBs、c：
κ-Car/GO(5:2)GBs、d：κ-Car/GO(5:3) GBs, with granularmetric analysis software (Nano Measurer 1.2) random measurement
Go out the diameter of 200 balls in each gelled pill, and calculates average diameter (table 1).It is coagulated for four kinds it can be seen from Fig. 2 and table 1
The grading curve of glue bead all meets normal distribution.This shows the size of gel ball than more uniform.
The average diameter of 1 four kinds of gelled pills of table
The content of calcium ion is shown in Table 2 in different gelled pills, as can be seen from Table 2, calcium ion plays crosslinking in gelled pill
Effect, calcium ion content is different in four kinds of gelled pills, but all 7% or so.
The calcium ion content of 2 four kinds of gelled pills of table
The internal structure and pattern of gelled pill are obtained by scanning electron microscope, and Fig. 3 gives the section of four kinds of gelled pills
Figure, wherein a is：κ-Car GBs、b：κ-Car/GO(5:1)GBs、c：κ-Car/GO(5:2)GBs、d：κ-Car/GO(5:3)
GBs is doped with the gel ball aperture of graphene oxide it can be seen in figure 3 that there are many holes and fold in the inside of gelled pill
Than the aperture smaller of pure kappa-carrageenan gel ball, in addition, for kappa-carrageenan/graphene oxide gel ball, with graphite oxide
The increase of alkene doping, aperture is smaller and smaller, and fold is more dense.Also exactly these apertures and intensive fold are to be adsorbed with engine dyeing
Material provides big specific surface area, and therefore, the adsorbance of kappa-carrageenan/graphene oxide gel ball is than pure kappa-carrageenan gel ball
Adsorbance higher.
Fig. 4 is the infrared spectrogram of graphene oxide, four kinds of gelled pills and kappa-carrageenan.It can be seen from Fig. 4 that
3424cm-1The broad peak and 1394cm at place-1The peak at place is the stretching vibration of O-H keys and the bending vibration of c h bond respectively, the two
Peak can be observed in material used, illustrate that these types of material all contains hydroxyl.In the infrared spectrogram of graphene oxide
In, 1639cm-1And 1068cm-1The peak at place corresponds to the stretching vibration of the stretching vibration and C-O keys of C=O keys respectively.In κ-OK a karaoke club
In the infrared spectrum of glue and pure kappa-carrageenan gelled pill, the flexural vibrations peak of O-H keys is in 1639cm in kappa-carrageenan structure-1
Place, 1068cm-1、929cm-1And 846cm-1C-O keys flexible shaking in glucosides connects 3,6- dehydration-D- galactolipins is corresponded to respectively
Dynamic peak, the stretching vibration peak for connecting hydroxyl and the sulfonic stretching vibration peak of connection.The infrared spectrogram of κ-Car/GO GBs with
The infrared spectrogram difference of κ-Car GBs is little, this may be because the peak of graphene oxide is covered by the peak of kappa-carrageenan.
Fig. 5 is the Raman figure of graphene oxide, four kinds of gelled pills and kappa-carrageenan.As seen from Figure 5, graphite oxide
Olefinic base material usually shows two characteristic peaks, and the wherein peaks D are generally related with defect to the confusion degree in material, and the peaks G by
Symmetrical sp2The stretching motion of carbon atom generates.There are the peaks D in the spectrogram of graphene oxide and three kinds of κ-Car/GO GBs
(1355cm-1) and the peaks G (1601cm-1) the two peaks, and do not observe this in the Raman spectrum of κ-Car GBs and kappa-carrageenan
Two peaks.All contain graphene oxide in three kinds of κ-Car/GO GBs of this explanation.And adulterate the drawing of graphene oxide gel ball
The no significant change compared with the spectrum of graphene oxide composite material of graceful spectrum, this shows in carragheen/graphene oxide gel ball,
Graphene oxide also maintains original structure feature, does not have to destroy the structure of graphene oxide composite material in preparation process.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of kappa-carrageenan-graphene oxide gel bead, includes the following steps：
(1) kappa-carrageenan, graphene oxide and water are mixed, obtains gel, kappa-carrageenan mass concentration is in the gel
0.5%~1.5%；
(2) gel that the step (1) obtains is added drop-wise to balling-up in calcium chloride solution, obtains kappa-carrageenan/graphene oxide
Gelled pill.
2. preparation method according to claim 1, which is characterized in that the quality of kappa-carrageenan, oxidation in the step (1)
The quality of graphene and the volume ratio of water are 0.5g:0.1~0.3g:35~100mL.
3. preparation method according to claim 2, which is characterized in that the quality of the kappa-carrageenan, graphene oxide
Quality and the volume ratio of water are 0.5g:0.1~0.3g:50mL.
4. preparation method according to claim 1, which is characterized in that calcium chloride solution is a concentration of in the step (2)
0.5mol/L。
5. preparation method according to claim 1 or 4, which is characterized in that gel and calcium chloride solution in the step (2)
Amount ratio be 1g:5mL~3g:50mL.
6. preparation method according to claim 1, which is characterized in that further include after balling-up in the step (2)：It will obtain
Balling-up system cure and wash successively, obtain kappa-carrageenan/graphene oxide gel bead.
7. the kappa-carrageenan that preparation method described in claim 1~6 any one obtains/graphene oxide gel bead, including
Kappa-carrageenan and the graphene oxide being encapsulated in the kappa-carrageenan.
8. kappa-carrageenan according to claim 7/graphene oxide gel bead, which is characterized in that the kappa-carrageenan
Mass ratio with graphene oxide is 5：1~3；
Also contain residual calcium ion in the kappa-carrageenan/graphene oxide gel bead, the calcium ion is in kappa-carrageenan/oxygen
Mass content in graphite alkene gelled pill is 6.60~7.89%.
9. kappa-carrageenan according to claim 7 or 8/graphene oxide gel bead, which is characterized in that the κ-OK a karaoke club
The average grain diameter of glue/graphene oxide gel bead is 2.87~2.99mm.
10. kappa-carrageenan/graphene oxide gel bead described in claim 7~9 any one answering in the treatment of waste water
With.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109464988A (en) * | 2018-11-23 | 2019-03-15 | 上海海洋大学 | A kind of preparation method of carragheen gel ball |
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