CN105817206A - Micro-fluidic preparation method of carboxylated chitosan adsorbent - Google Patents
Micro-fluidic preparation method of carboxylated chitosan adsorbent Download PDFInfo
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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Abstract
The invention provides a micro-fluidic preparation method of a carboxylated chitosan adsorbent. The method comprises the following steps: 1, preparing carboxylated chitosan micro-droplets; 2, cross-linking the carboxylated chitosan micro-droplets; 3, cleaning carboxylated chitosan micro-spheres obtained in step 2 with an ethanol solution, an acetone solution and deionized water; and 4, freeze-drying chitosan micro-spheres obtained in step 3 to obtain the carboxylated chitosan adsorbent.
Description
Technical field
The invention belongs to water-treatment technology field, relate to a kind of carboxyl chitosan adsorbent microfluidic control Preparation Method, more particularly, it relates to a kind of novel carboxyl chitosan adsorbent microfluidic control Preparation Method for complex system industrial wastewater.
Background technology
Derived energy chemical industrial wastewater usually contains the complex components such as heavy metal ion (such as copper, cobalt, manganese), azo macromole (such as methyl orange), strong acid and strong base, existing method of wastewater treatment, such as neutralisation, reducing process, sulfuration method etc., it is faced with that single treatment amount is little, long processing period, treatment effect be not good enough, processing cost is high, there is the difficult problems such as secondary pollution.
Therefore, at present to processing method simply effectively, process that the cycle is short, processing cost is low, more and more higher to the cry of the efficient method of wastewater treatment of environment non-secondary pollution.
Summary of the invention
For derived energy chemical industrial wastewater complicated component, single treatment amount is little, long processing period, treatment effect be not good enough, processing cost is high, there is the difficult problems such as secondary pollution, the invention provides a kind of novel carboxyl chitosan adsorbent microfluidic control Preparation Method for complex system industrial wastewater；The novel carboxyl chitosan adsorbent prepared by this kind of method is utilized to have the feature such as morphology controllable, mechanical strength is high, rate of adsorption adsorbance fast, total is big, non-secondary pollution, repeatable utilization, and preparation method is the most effective, with low cost, Various Complex component waste water system can be processed efficiently, thus solve problems of the prior art.
On the one hand, the invention provides a kind of carboxyl chitosan adsorbent microfluidic control Preparation Method, the method comprises the following steps:
The preparation of (i) carboxyl chitosan microlayer model: respectively by the internal phase containing carboxyl chitosan with immiscible with described internal phase be interlinked to the outside in micro-fluidic chip, form carboxyl chitosan microlayer model, wherein, described internal phase is the aqueous solution of the glycerol being added with the carboxyl chitosan of 1-3 weight portion and 1-3 weight portion；Described foreign minister is the n-octyl alcohol solution of the Span 80 being added with 1-2 weight portion；
(ii) crosslinking of carboxyl chitosan microlayer model: the carboxyl chitosan microlayer model obtained in step (i) is transferred in crosslinking curing liquid, and reacts a period of time under slow stirring, obtain carboxyl chitosan microsphere；
(iii) the carboxyl chitosan microsphere obtained in ethanol solution, acetone soln and deionized water cleaning step (ii) is utilized successively；And
(iv) the chitosan microball lyophilizing that will obtain in step (iii), obtains carboxyl chitosan adsorbent.
In one preferred embodiment, in step (i), utilize External infusion pumping system, respectively described internal phase and foreign minister are passed through cross-current and decline in fluidic chip, the shearing force formed by the current difference of two phase flow, shears internal phase and becomes the carboxyl chitosan microlayer model of uniform particle sizes.
Another preferred embodiment in, the described cross-current fluidic chip that declines is that 3 strata methyl methacrylate plate are formed by hot pressing, and its intermediate layer is 0.3-1mm microchannel layers.
Another preferred embodiment in, the velocity ratio controlling described internal phase and foreign minister is 1:10 to 1:20.
Another preferred embodiment in, in step (ii), described crosslinking curing liquid is the normal octane solution of the Span 80 being added with the glutaraldehyde of 0.5-1 weight portion and 1-2 weight portion；Being proceeded to wherein by carboxyl chitosan microlayer model and be slowly stirred, control mixing speed is 400-500r/min, and the response time is 30-60 minute.
Another preferred embodiment in, in step (iii), the concentration of described ethanol solution is 10-20%, and the concentration of acetone soln is 10-30%；Ethanol solution, acetone soln and deionized water is utilized to clean carboxyl chitosan microsphere 3-4 time successively.
Another preferred embodiment in, in step (iv), described freeze temperature is-45 to-60 DEG C, and freeze-drying time controlled at 6-8 hour.
On the other hand, the invention provides a kind of carboxyl chitosan adsorbent, it is prepared in aforementioned manners.
Another further aspect, the present invention relates to the application for complex system industrial wastewater of the above-mentioned carboxyl chitosan adsorbent.
In one preferred embodiment, described complex system industrial wastewater includes derived energy chemical industrial wastewater.
Accompanying drawing explanation
Fig. 1 is the preparation flow schematic diagram of the novel carboxyl chitosan adsorbent according to an embodiment of the invention.
Fig. 2 be according to the crosslinking of an embodiment of the invention after novel carboxyl chitosan microsphere photo under an optical microscope.
Fig. 3 shows that the novel carboxyl chitosan adsorbent according to the embodiment of the present application 1 adsorbs the UV peak change curve of 0.01% methyl orange solution under neutrallty condition (pH=7).
Fig. 4 shows that the novel carboxyl chitosan adsorbent according to the embodiment of the present application 2 adsorbs 0.01% methyl orange solution UV peak change curve under acid condition (pH=3).
Detailed description of the invention
Term
Term chitosan (Chitosan) used herein, refers to the product of chitin deacetylase base.It is the unique natural alkalescence aminopolysaccharide of nature, has good biocompatibility, biological degradability and afterproduct avirulence of degrading.Its surface has substantial amounts of active amino and hydroxyl, is possible not only to and heavy metal ion formation metal complex, thus Adsorption of Heavy Metal Ions, organic macromolecular substances can also be adsorbed simultaneously.Additionally, by chitosan surface is carried out functional group's grafting, be possible not only to give its outstanding adsorption selectivity, make it have good catalytic performance especially.
Term used herein is micro-fluidic, it it is a kind of technology manipulating very low volume fluids grown up on micro-fluidic chip in recent years, its principle is: by two kinds of immiscible liquid, with one therein as continuous phase, another kind is dispersion phase, continuous phase and dispersion phase are entered chip by different entrances respectively, and in microchannel, dispersion phase is cut into the microlayer model of the uniform particle sizes of series of discrete under the effect of shearing force by continuous phase；Each drop is wrapped up by continuous phase independently, with extraneous without mass exchange, form a closed system, therefore can complete one group of chemical or biological reactions, and stable reaction conditions, reliable results as a microreactor.
Present inventor through extensive and after in-depth study find, for waste water complicated components in derived energy chemical industry, process that technique is loaded down with trivial details, operating cost and the problem such as the cost of raw material is the highest, using carboxyl chitosan as matrix, glutaraldehyde, as cross-linking agent, utilizes microflow control technique to prepare novel carboxyl chitosan adsorbent to process waste water；Compared with tradition chitosan absorbent, the novel carboxyl chitosan adsorbent prepared has the feature such as morphology controllable, mechanical strength is high, rate of adsorption adsorbance fast, total is big, non-secondary pollution, repeatable utilization, and preparation method is the most effective, with low cost, the heavy metal ion such as the azo macromole in waste water and copper chromium lead can be processed efficiently, the recovery of metal in waste water can be realized in conjunction with simple segregation apparatus, thus a kind of method providing high-efficient simple for derived energy chemical Industrial Wastewater Treatment, there is good industrial applications prospect.Based on above-mentioned discovery, the present invention is accomplished.
The technology design of the present invention is as follows:
Absorption method be a kind of simple effectively, the process cycle is short, processing cost is low, efficient method of wastewater treatment to environment non-secondary pollution, can perform well in processing derived energy chemical industrial wastewater.
Four amino can form stable metallo-chelate with a metal ion, owing to the amino on chitosan molecule chain presents linearly, more difficult with metal ion formation chelate.Carry out the cross-linked chitosan after schiff base reaction by glutaraldehyde and can shorten the distance between the amino on linear chitosan molecule chain, be more beneficial for forming chelate with metal ion.But, due to schiff base reaction amino to be consumed, the actual absorption property of the chitosan absorbent finally given is far smaller than theoretical absorption property.Carboxyl chitosan is utilized then to effectively raise the absorption property of adsorbent as carboxyl chitosan adsorbent prepared by matrix.First, a large amount of carboxyls present on carboxyl chitosan strand can form metallo-chelate by single or double coordination with metal ion, is greatly improved the absorbability of adsorbent.Secondly, on carboxyl chitosan, original amino can also form metallo-chelate with metal ion.Finally, due to carboxyl chitosan water solublity is better than common chitosan so that the final carboxyl chitosan adsorbent prepared presents neutrality, it is adaptable to broader waste water treatment conditions.
In a first aspect of the present invention, it is provided that a kind of novel carboxyl chitosan adsorbent microfluidic control Preparation Method for complex system industrial wastewater, the method comprises the following steps:
Step one: the preparation of carboxyl chitosan microlayer model: utilize External infusion pumping system, respectively the internal phase containing carboxyl chitosan and foreign minister immiscible with this internal phase are passed through cross-current and decline in fluidic chip, by controlling the flow velocity of two phase flow, internal phase is sheared and becomes the carboxyl chitosan microlayer model of a series of uniform particle sizes；
Step 2: the crosslinking of carboxyl chitosan microlayer model: the carboxyl chitosan microlayer model of step one gained is transferred in the crosslinking curing liquid containing glutaraldehyde cross-linking agent, and reacts a period of time under slow stirring；
Step 3: utilize ethanol solution, acetone soln and the carboxyl chitosan microsphere of deionized water cleaning step two gained diluted by a certain percentage successively；And
Step 4: by the chitosan microball lyophilizing a few hours under certain condition of step 3 gained, obtain novel carboxyl chitosan adsorbent.
In the present invention, the internal phase described in step one is the aqueous solution of the glycerol being added with the carboxyl chitosan of 1-3 weight portion and 1-3 weight portion, by changing content and then the regulation internal phase viscosities of glycerol；Described foreign minister is the n-octyl alcohol solution of the Span 80 being added with 1-2 weight portion.
In the present invention, cross-current described in step one fluidic chip that declines is that 3 strata methyl methacrylate (PMMA) plates are formed by hot pressing, its intermediate layer is the microchannel layers of 0.3-1mm, can be controlled the size of carboxyl chitosan microlayer model by the size changing microchannel.
In the present invention, in step one, the velocity ratio controlling internal phase and foreign minister is 1:10 to 1:20, and along with the increase of velocity ratio, microlayer model size is gradually reduced, but the uniformity improves.
In the present invention, the crosslinking curing liquid described in step 2 is the normal octane solution of the Span 80 being added with the glutaraldehyde of 0.5-1 weight portion and 1-2 weight portion；Being proceeded to wherein by carboxyl chitosan microsphere and be slowly stirred, control mixing speed is 400-500r/min, and the response time is 30-60 minute.
In the present invention, the concentration of the ethanol solution described in step 3 is 10-20%, and the concentration of acetone soln is 10-30%, cleans chitosan microball 3-4 time successively.
In the present invention, the freeze temperature described in step 4 is-45 to-60 DEG C, and freeze-drying time controlled at 6-8 hour.
In a second aspect of the present invention, it is provided that a kind of carboxyl chitosan adsorbent, it is prepared in aforementioned manners.
Below referring to accompanying drawing.
Fig. 1 is the preparation flow schematic diagram of the novel carboxyl chitosan adsorbent according to an embodiment of the invention.As shown in Figure 1, utilize External infusion pumping system 5, respectively the internal phase containing carboxyl chitosan and foreign minister immiscible with this internal phase are passed through cross-current and decline in fluidic chip 1, by controlling the flow velocity of two phase flow, internal phase is sheared and becomes the carboxyl chitosan microlayer model of a series of uniform particle sizes；The carboxyl chitosan microlayer model of gained is transferred in the crosslinking curing liquid 2 containing glutaraldehyde cross-linking agent, and cross-linking reaction a period of time under slow stirring, obtain carboxyl chitosan microsphere 3；Utilize the ethanol solution, acetone soln and the deionized water that dilute by a certain percentage to clean the carboxyl chitosan microsphere of gained successively, and by the chitosan microball of gained lyophilizing a few hours under certain condition, obtain novel carboxyl chitosan adsorbent 4.
Fig. 2 be according to the crosslinking of an embodiment of the invention after novel carboxyl chitosan microsphere photo under an optical microscope.As in figure 2 it is shown, novel carboxyl chitosan microsphere presents golden yellow translucent before curing, mean diameter is 476 μm, and CV (particle diameter deviation) value is less than 6%.
Fig. 3 shows that the novel carboxyl chitosan adsorbent according to the embodiment of the present application 1 adsorbs the UV peak change curve of 0.01% methyl orange solution under neutrallty condition (pH=7).As it is shown on figure 3, in adsorption process in neutral conditions, methyl orange absorbing wavelength under ultraviolet light is that 467nm keeps constant, and methyl orange UV absworption peak peak value originally was 2.152, carried out a peak value measurement every 10 minutes；Through 90 minutes, the UV absworption peak peak value measurement novel carboxyl chitosan adsorbent the most described by the present invention less than, it was demonstrated that methyl orange was complete.
Fig. 4 shows that the novel carboxyl chitosan adsorbent according to the embodiment of the present application 2 adsorbs 0.01% methyl orange solution UV peak change curve under acid condition (pH=3).As shown in Figure 4, in adsorption process in acid condition, methyl orange absorbing wavelength under ultraviolet light is still 467nm, and methyl orange UV absworption peak peak value originally was 1.493, carried out a peak value measurement every 10 minutes；Through 80 minutes, UV absworption peak peak value measurement less than, proving that methyl orange novel carboxyl chitosan adsorbent the most described by the present invention is complete, prove in acid condition simultaneously, novel carboxyl chitosan adsorbent of the present invention has more preferable adsorption effect to methyl orange.
Main advantages of the present invention are:
The present invention proposes a kind of novel carboxyl chitosan adsorbent microfluidic control Preparation Method for complex system industrial wastewater, as cross-linking agent, utilizes novel carboxyl chitosan adsorbent prepared by microflow control technique as matrix, glutaraldehyde using carboxyl chitosan.Compared with conventional adsorbent, this kind of novel carboxyl chitosan adsorbent has the features such as morphology controllable, mechanical strength height, non-secondary pollution, repeatable utilization, and preparation method is the most effective, with low cost, the heavy metal ion such as the azo macromole in waste water and copper chromium lead can be processed efficiently, the recovery of metal in waste water can be realized in conjunction with simple segregation apparatus.Compared with common chitosan absorbent, this kind of novel carboxyl chitosan adsorbent is due to the existence of a large amount of carboxyls, there is the features such as rate of adsorption adsorbance fast, total is big, and the carboxyl chitosan adsorbent finally prepared presents neutrality, it is applicable to broader waste water treatment conditions, a kind of method providing high-efficient simple for derived energy chemical Industrial Wastewater Treatment, has good industrial applications prospect.
Embodiment
The present invention is expanded on further below in conjunction with specific embodiment.It should be appreciated, however, that these embodiments are merely to illustrate the present invention and are not meant to limit the scope of the invention.The test method of unreceipted actual conditions in the following example, generally according to normal condition, or according to the condition proposed by manufacturer.Except as otherwise noted, all of percentage ratio and number are by weight.
Embodiment 1: utilizing novel carboxyl chitosan adsorbent adsorption concentration in neutral conditions is the methyl of 0.01%
Orange solution
The preparation of novel carboxyl chitosan adsorbent:
Step one: using the carboxyl chitosan that carboxylation degree is 80% (purchased from Shanghai Shi Feng Science and Technology Ltd.) of 2 weight portions and 1.5 weight portions glycerol be sufficiently mixed as internal phase, using the n-octyl alcohol solution of the Span 80 (purchased from Chemical Reagent Co., Ltd., Sinopharm Group) that is added with 2 weight portions as foreign minister；The cross-current that internal phase and foreign minister are passed through 0.5mm microchannel by External infusion system declines in fluidic chip, and the velocity ratio controlling internal phase and foreign minister is 1:15, prepares the carboxyl chitosan microlayer model of uniform particle sizes；
Step 2: the carboxyl chitosan microlayer model of gained in step one is transferred in crosslinking curing liquid (glutaraldehyde of 0.5 weight portion and the normal octane solution of the Span 80 of 2 weight portions), control mixing speed is 450r/min, react 30 minutes, make carboxyl chitosan microlayer model full cross-linked, be colourless become golden yellow；
Step 3: ethanol solution, the acetone soln of 20% and the deionized water utilizing concentration to be 10% successively the carboxyl chitosan microsphere of step 2 gained, cleans 3 times；
Step 4: carboxyl chitosan microsphere step 3 cleaned-50 DEG C of lyophilizations 6 hours in freeze dryer, obtains novel carboxyl chitosan adsorbent.
Concentration is the absorption of methyl orange solution of 0.01% in neutral conditions:
Weigh in 0.01% methyl orange solution that 0.05g novel carboxyl chitosan adsorbent adds the initial pH=7 of 25mL to.After the sample of 10 minutes extraction 1mL dilutes 3 times, ultraviolet-uisible spectrophotometer is utilized to detect its UV peak value.Fig. 3 shows methyl orange solution peak value versus time curve.
Experimental result:
After 90 minutes, can't detect methyl orange peak value under corresponding wavelength, it is believed that methyl orange is adsorbed completely.It is demonstrated experimentally that the novel carboxyl chitosan adsorbent of present invention methyl orange solution to 0.01% in neutral conditions has good absorption property..
Embodiment 2: utilizing novel carboxyl chitosan adsorbent (pH=3) adsorption concentration in acid condition is 0.01%
Methyl orange solution
The preparation of novel carboxyl chitosan adsorbent:
Method as described in embodiment 1 prepares novel carboxyl chitosan adsorbent.
(pH=3) concentration is the absorption of methyl orange solution of 0.01% in acid condition:
Weigh in 0.01% methyl orange solution that 0.05g novel carboxyl chitosan adsorbent adds the initial pH=3 of 25mL to.After the sample of 10 minutes extraction 1mL dilutes 3 times, ultraviolet-uisible spectrophotometer is utilized to detect its UV peak value.Fig. 4 shows methyl orange solution peak value versus time curve.
Experimental result:
After 80 minutes, can't detect methyl orange peak value under corresponding wavelength, and solution has been still acid, it is believed that methyl orange has been adsorbed completely.It is demonstrated experimentally that the novel carboxyl chitosan adsorbent of present invention methyl orange solution to 0.01% in acid condition has more preferable absorption property.
Embodiment 3: utilize the copper ion in novel carboxyl chitosan adsorbent copper-bath
The preparation of novel carboxyl chitosan adsorbent:
Method as described in embodiment 1 prepares novel carboxyl chitosan adsorbent.
The absorption of the copper ion in copper-bath:
Take 0.05g novel carboxyl chitosan adsorbent add to 25mL original ph be 5, copper ion concentration be 400ppm copper-bath in.Every the sample of 1 hour extraction 0.5mL, utilize electric coupling plasma mass spectrograph plasma light spectrometer that it is measured.Finally recording novel carboxyl chitosan adsorbent and reached adsorption equilibrium after 210 minutes, the maximal absorptive capacity to copper ion is 69.3mg/g.
Experimental result:
It is demonstrated experimentally that the chitosan absorbent of the present invention has the good rate of adsorption and absorbability to copper ion.
Above-mentioned listed embodiment is only presently preferred embodiments of the present invention, is not used for limiting the practical range of the present invention.The most all equivalence changes made according to the content of scope of the present invention patent and modification, all should be the technology category of the present invention.
The all documents mentioned in the present invention are incorporated as reference the most in this application, are individually recited as with reference to like that just as each document.In addition, it is to be understood that after the above-mentioned teachings having read the present invention, the present invention can be made various changes or modifications by those skilled in the art, these equivalent form of values fall within the application appended claims limited range equally.
Claims (10)
1. a carboxyl chitosan adsorbent microfluidic control Preparation Method, the method comprises the following steps:
The preparation of (i) carboxyl chitosan microlayer model: respectively by the internal phase containing carboxyl chitosan with immiscible with described internal phase be interlinked to the outside in micro-fluidic chip, form carboxyl chitosan microlayer model, wherein, described internal phase is the aqueous solution of the glycerol being added with the carboxyl chitosan of 1-3 weight portion and 1-3 weight portion；Described foreign minister is the n-octyl alcohol solution of the Span 80 being added with 1-2 weight portion；
(ii) crosslinking of carboxyl chitosan microlayer model: the carboxyl chitosan microlayer model obtained in step (i) is transferred in crosslinking curing liquid, and reacts a period of time under slow stirring, obtain carboxyl chitosan microsphere；
(iii) the carboxyl chitosan microsphere obtained in ethanol solution, acetone soln and deionized water cleaning step (ii) is utilized successively；And
(iv) the chitosan microball lyophilizing that will obtain in step (iii), obtains carboxyl chitosan adsorbent.
2. the method for claim 1, it is characterized in that, in step (i), utilize External infusion pumping system, respectively described internal phase and foreign minister are passed through cross-current and decline in fluidic chip, the shearing force formed by the current difference of two phase flow, shears internal phase and becomes the carboxyl chitosan microlayer model of uniform particle sizes.
3. method as claimed in claim 2, it is characterised in that the described cross-current fluidic chip that declines is that 3 strata methyl methacrylate plate are formed by hot pressing, and its intermediate layer is 0.3-1mm microchannel layers.
4. method as claimed in claim 2, it is characterised in that the velocity ratio controlling described internal phase and foreign minister is 1:10 to 1:20.
5. the method for claim 1, it is characterised in that in step (ii), described crosslinking curing liquid is the normal octane solution of the Span 80 being added with the glutaraldehyde of 0.5-1 weight portion and 1-2 weight portion；Being proceeded to wherein by carboxyl chitosan microlayer model and be slowly stirred, control mixing speed is 400-500r/min, and the response time is 30-60 minute.
6. the method for claim 1, it is characterised in that in step (iii), the concentration of described ethanol solution is 10-20%, and the concentration of acetone soln is 10-30%；Ethanol solution, acetone soln and deionized water is utilized to clean carboxyl chitosan microsphere 3-4 time successively.
7. the method for claim 1, it is characterised in that in step (iv), described freeze temperature is-45 to-60 DEG C, and freeze-drying time controlled at 6-8 hour.
8. a carboxyl chitosan adsorbent, it is to prepare by the method according to any one of claim 1-7.
9. the carboxyl chitosan adsorbent described in claim 8 is for the application of complex system industrial wastewater.
Apply the most as claimed in claim 9, it is characterised in that described complex system industrial wastewater includes derived energy chemical industrial wastewater.
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| CN115007132A (en) * | 2022-06-29 | 2022-09-06 | 南京工业大学 | Carbon nanotube supported dysprosium oxide catalyst and preparation method and application thereof |
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| KR20090083784A (en) * | 2008-01-30 | 2009-08-04 | 연세대학교 산학협력단 | Microfluidic devices incorporating non-spherical hydrogel microparticles for bioassay |
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