CN105771929B - The method that microfluidic control is modified carboxyl chitosan heavy metal wastewater thereby adsorbent for PEI - Google Patents
The method that microfluidic control is modified carboxyl chitosan heavy metal wastewater thereby adsorbent for PEI Download PDFInfo
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- CN105771929B CN105771929B CN201610159985.1A CN201610159985A CN105771929B CN 105771929 B CN105771929 B CN 105771929B CN 201610159985 A CN201610159985 A CN 201610159985A CN 105771929 B CN105771929 B CN 105771929B
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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Abstract
The present invention provides a kind of microfluidic controls for the method for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI, it declines in fluidic chip the described method includes: the dispersed phase containing carboxyl chitosan and the continuous phase containing n-octyl alcohol are each led into focused flow, dispersed phase and the current difference of continuous phase are 1:10-1:20, the carboxyl chitosan microlayer model that dispersed phase in microchannel is cut into as uniform particle sizes, carboxyl chitosan microlayer model is added in the normal octane solution of 80 surfactant of the glutaraldehyde cross-linking agent added with 0.5-1wt% and 1-2wt% Span and is crosslinked, it is modified through 0.5-1wt% polyethylenimine solution again, obtain polyethyleneimine-modified carboxyl chitosan adsorbent.Compared with conventional adsorbent, which has very strong absorption property to divalent heavy metal ions, can efficiently handle waste water in conjunction with separation equipment and recycle wherein heavy metal, the application prospect with industrialization.
Description
Technical field
The present invention relates to a kind of microfluidic controls for the method for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI, specifically
It is related in derived energy chemical industry, a kind of microfluidic control for effluent containing heavy metal ions processing is modified for PEI (polyethyleneimine)
The method of carboxyl chitosan heavy metal wastewater thereby adsorbent.
Background technique
Derived energy chemical industrial wastewater complicated components, usually containing includes the heavy metal ion such as copper, cobalt, manganese and other have
Machine macromolecular, suspended matter etc..Existing wastewater treatment method, such as neutralisation, reduction method, membrane filter method, vulcanization, are faced with
Single treatment amount is small, long processing period, treatment effect is not good enough, processing cost is high, there are the problems such as secondary pollution.And it adsorbs
Method, is the adsorbent using natural or artificial synthesized material, carries out physics and chemisorption to heavy metal ions in wastewater, not only not
Secondary pollution is generated, and there is the recyclable performance recycled.Absorption method is that one kind is simple and effective, process cycle is short, handling
With efficient wastewater treatment method low, without secondary pollution to environment.
Microlayer model is a kind of technology of the manipulation very low volume fluids to grow up on micro-fluidic chip in recent years, former
Reason are as follows: by two kinds of immiscible liquid, with one such for continuous phase, another kind is dispersed phase, continuous phase and dispersed phase
Enter chip by different entrances respectively, in microchannel, dispersed phase is cut by continuous phase a series of under the action of shear force
The microlayer model of discrete uniform particle sizes.Each drop is independent to be wrapped up by continuous phase, with the external world without mass exchange, forms an envelope
Closure system, therefore can be used as a microreactor, one group of chemical or biological reactions, and stable reaction conditions are completed, as a result may be used
It leans on.
Chitosan is unique natural alkaline glycosaminoglycan in the excellent natural macromolecular material nature of one kind, is had well
Biocompatibility, biological degradability, and catabolite is non-toxic.Its surface has a large amount of active amino and hydroxyl, no
Only metal complex can be formed with heavy metal ion, to adsorb heavy metal ion, while organic macromolecule can also be adsorbed
Substance.In addition, can not only assign its more outstanding absorption property, more by carrying out functional group's grafting to chitosan surface
It is to make it have certain adsorption selectivity.Heretofore described polyethyleneimine is exactly a kind of ideal functional group's grafting
Material, polyethyleneimine (PEI) are a kind of typical aqueous solution polyamine, are in aqueous solution in alkalinity, are possessed on strand a large amount of
Amido N atom, polyethyleneimine-modified can supplement amino, and the increase of amino amount is more advantageous in absorption industrial wastewater
Heavy metal ion.
Four amino can form stable metallo-chelate with a metal ion, due to the ammonia in chitosan molecule chain
Base is presented linearly, and it is more difficult to form chelate with metal ion.By with glutaraldehyde carry out schiff base reaction after cross-linked chitosan
It can be shortened the distance between the amino in linear chitosan molecule chain, be more advantageous to and form chelate with metal ion.But by
Amino is inherently consumed in schiff base reaction, the practical absorption property of finally obtained chitosan absorbent is far smaller than theory
Absorption property.The carboxyl chitosan adsorbent that simultaneously carboxyl chitosan is prepared as matrix then effectively raises adsorbent
Absorption property.Firstly, a large amount of carboxyls can pass through single or double coordination and metal present on carboxyl chitosan strand
Ion forms metallo-chelate, greatly improves the adsorption capacity of adsorbent.Secondly, original amino on carboxyl chitosan
Metallo-chelate can be formed with metal ion.Finally, due to which carboxyl chitosan water solubility is better than common chitosan, so that finally
Neutrality is presented in carboxyl chitosan adsorbent obtained, suitable for broader wastewater treatment condition.
Summary of the invention
For derived energy chemical industrial wastewater complicated component, single treatment amount is small, long processing period, treatment effect is not good enough, place
Manage it is with high costs, there are secondary pollution, in order to solve effluent containing heavy metal ions complex treatment process, operation in derived energy chemical industry
The problems such as expense and the relatively high cost of raw material, the present invention provides a kind of polyethyleneimine-modified carboxyl chitosan adsorbents
Handle the microfluidic control Preparation Method of copper cobalt manganese effluent containing heavy metal ions.Utilize polyethyleneimine-modified carboxylic prepared by such method
Changing chitosan absorbent has fast morphology controllable, high mechanical strength, the rate of adsorption, total large amount of adsorption, without secondary pollution, repeatable
The features such as utilization, and preparation method is simple and effective, low in cost, and it is useless can efficiently to handle Various Complex component heavy metal ion
Aqueous systems.
A kind of method of the microfluidic control of the present invention for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI, packet
Include following steps:
Step 1: prepared by carboxyl chitosan microlayer model: by syringe pump, by the dispersed phase containing carboxyl chitosan and containing
The continuous phase of n-octyl alcohol each leads into focused flow and declines in fluidic chip, and the current difference of dispersed phase and continuous phase is 1:10-1:20,
The carboxyl chitosan microlayer model that dispersed phase in microchannel is cut into as uniform particle sizes,
Step 2: carboxyl chitosan microlayer model is crosslinked: carboxyl chitosan microlayer model obtained by step 1 being transferred to and is added with
It in the normal octane solution of 80 surfactant of glutaraldehyde cross-linking agent and 1-2wt% Span of 0.5-1wt%, and is slowly stirred, controls
Mixing speed 300-400r/min processed, crosslinking time be 30-60 minute, then successively with the ethanol solution of 10-20wt% with go from
Sub- water cleaning, drying obtain carboxyl chitosan microballoon；
Step 3: the modification of carboxyl chitosan microballoon: by the resulting carboxyl chitosan microballoon of step 2 with 30-50wt%'s
After aqueous isopropanol cleans 3-4 times repeatedly, it is transferred in the aqueous isopropanol containing 0.3-0.5wt% epoxychloropropane, 40-50
It is impregnated 2-3 hours under DEG C water bath condition；Resulting carboxyl chitosan microballoon is transferred to 0.5-1wt% polyethylenimine solution again
In, it under the conditions of lower than 60 DEG C, is slowly stirred, reacts 3-5 hours；
Step 4: with deionized water, successively modified carboxyl chitosan microballoon resulting to step 3 cleans 3-4 times repeatedly；And
It is dried under conditions of 30-40 DEG C, drying time 3-10 hours, obtains polyethyleneimine-modified carboxyl chitosan adsorbent.
Dispersed phase described in step 1 is the ice vinegar of carboxyl chitosan and 0.5wt%-3wt% added with 2-4wt%
Sour mixed solution, continuous phase are the n-octyl alcohol solution added with 80 surfactant of 1-2wt% Span.
Focused flow described in step 1 decline fluidic chip be upper and lower 2 strata methyl methacrylate (PMMA) plate pass through
Hot pressing forms, and cover plate of upper layer contains 2 continuous phase entrances and a dispersed phase entrance, and lower layer's bottom plate is carved with cross microchannel slot
Road, three conduit endpoints of cross microchannel conduit and continuous phase and dispersed phase pass-through entry on cover board, a remaining slot
Road endpoint is drop outlets；Microchannel channel width is 500-1000 μm.
Wash number in step 2 is 3-4 times, and the drying temperature is 30-40 DEG C, and drying time is controlled in 6-10
Hour.
The invention has the following advantages:
The invention proposes a kind of microfluidic controls for the method for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI, adopts
With glutaraldehyde as cross linker, prepared by carboxyl chitosan microballoon to microflow control technique using polyethyleneimine and is modified.With it is common
Chitosan absorbent compare, PEI prepared by the present invention modified carboxyl chitosan adsorbent not only has uniform partial size
Size and controllable pattern, and the ammonia that carboxyl and polyethyleneimine-modified as provided by carboxyl chitosan are additionally provided
The presence of base, amino has significant absorption property to divalent heavy metal ions, improves the rate of adsorption and adsorption capacity, while simultaneous
Have the features such as high mechanical strength, without secondary pollution, reusable, and preparation method is simple and effective, low in cost, it can be efficient
Ground handles the heavy metal ion such as azo macromolecular and copper chromium lead in the effluent containing heavy metal ions of multi-component complex system, is applicable in
In broader wastewater treatment condition, a kind of method of high-efficient simple is provided for derived energy chemical commercial metal wastewater treatment,
With good industrial applications prospect.
Detailed description of the invention
Fig. 1 is the preparation flow of modified carboxyl chitosan adsorbent.
Fig. 2 is carboxyl chitosan particle photo under optical microscopy.460 ± 5 μm of average grain diameter, CV value is less than 5%.
Fig. 3 a is that focused flow declines the cover board and continuous phase and dispersed phase entrance of fluidic chip, and Fig. 3 b is that focused flow declines stream
Control the bottom plate and cross microchannel conduit of chip.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1: it is prepared in polyethyleneimine-modified carboxyl chitosan adsorbent absorption copper-bath using this patent
Copper ion.
Step 1: the shell that will be prepared by the glacial acetic acid of 2wt% carboxyl chitosan (viscosity 200mPaS) and 1.5wt% is poly-
Sugar aqueous solution is as dispersed phase, using the n-octyl alcohol solution added with 80 surfactant of 2wt% Span as continuous phase；By list
Dispersed phase and continuous phase are passed through focused flow respectively and declined in fluidic chip by channel injection pump and binary channels syringe pump, and partial size is made
Uniform carboxyl chitosan microlayer model；
Step 2: carboxyl chitosan microlayer model obtained in step 1 is passed into crosslinking curing liquid (0.7wt% penta 2
The normal octane solution of aldehyde, 2wt% Span 80) in, it is slowly stirred, reacts 1 hour, so that after chitosan drop is full cross-linked；According to
It is secondary to be respectively washed 3-4 times using diluted 20% ethanol solution and deionized water；The vacuum drying 8 hours under the conditions of 40 DEG C,
Obtain carboxyl chitosan microballoon；
Step 3: the resulting carboxyl chitosan microballoon of step 2 is cleaned 4 times with 50wt% aqueous isopropanol, to isopropanol
0.5wt% epoxychloropropane is added in solution, is slowly stirred, and is impregnated 2 hours；Carboxyl chitosan microballoon is transferred to again
In the polyethylenimine solution of 0.5wt%, it is slowly stirred under conditions of temperature is no more than 60 DEG C, to ensure fully reacting, instead
It is 4 hours between seasonable；
Step 4: repeated flushing, 40 DEG C of temperature strips successively are carried out to the resulting chitosan ball of step 3 with deionized water
Drying obtains polyethyleneimine-modified carboxyl chitosan adsorbent under part, and drying time is 10 hours；
Weighing 0.3g polyethyleneimine-modified carboxyl chitosan adsorbent to be added to 200mL initial pH value is that 5, copper ion is dense
Degree is in the copper-bath of 1000ppm.Standing adsorption takes the copper-bath of 5mL after equilibrium to be reacted, using ICP etc. from
Sub-light spectrometer measures it.Finally polyethyleneimine-modified carboxyl chitosan adsorbent is measured to reach after 100 hours
To adsorption equilibrium, the final adsorbance to copper ion is 69.2mg/g.It is demonstrated experimentally that chitosan absorbent of the invention to copper from
Son has good absorption property.
Embodiment 2: it is prepared in the adsorbing chlorinated cobalt liquor of polyethyleneimine-modified carboxyl chitosan adsorbent using this patent
Cobalt ions.
Polyethyleneimine-modified carboxyl chitosan adsorbent is made by embodiment 1.
Weighing 0.3g polyethyleneimine-modified carboxyl chitosan adsorbent to be added to 200mL initial pH value is that 5, cobalt ions is dense
Degree is in the cobalt chloride solution of 1000ppm.Standing adsorption takes the cobalt chloride solution of 5mL after equilibrium to be reacted, using ICP etc. from
Sub-light spectrometer measures it.Finally measuring modification of chitosan adsorbent reached adsorption equilibrium after 116 hours, to cobalt
The final adsorbance of ion is 56.7mg/g.It is demonstrated experimentally that chitosan absorbent of the invention has preferable inhale to cobalt ions
Attached performance.
Embodiment 3: prepared by the method modification of chitosan adsorbent selective absorption copper sulphate and aluminium chloride mixing
Copper ion in solution.
Polyethyleneimine-modified carboxyl chitosan adsorbent is made by embodiment 1.
Weigh 0.3g polyethyleneimine-modified carboxyl chitosan adsorbent be added to 200mL initial pH value be 5, copper ion and
Aluminium ion concentration is in the copper sulphate and aluminium chloride mixed solution of 1000ppm.Standing adsorption takes 5mL's after equilibrium to be reacted
Mixed solution measures it using ICP plasma light spectrometer.Finally measure polyethyleneimine-modified carboxyl chitosan
Adsorbent reached adsorption equilibrium after 102 hours, and the final adsorbance to copper ion is 68.7mg/g, to aluminum ions final suction
Attached amount is 0.2mg/g.It is demonstrated experimentally that polyethyleneimine-modified carboxyl chitosan adsorbent of the invention has preferably copper ion
Adsorption selectivity.
Claims (4)
1. a kind of microfluidic control is for the method for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI, which is characterized in that the side
Method the following steps are included:
Step 1: the preparation of carboxyl chitosan microlayer model: by syringe pump, by the dispersed phase containing carboxyl chitosan and containing just
The continuous phase of octanol each leads into focused flow and declines in fluidic chip, and the current difference of dispersed phase and continuous phase is 1:10-1:20, micro-
The carboxyl chitosan microlayer model that dispersed phase in channel is cut into as uniform particle sizes；
Step 2: carboxyl chitosan microlayer model is crosslinked: carboxyl chitosan microlayer model obtained by step 1 is transferred to added with 0.5-
It in the normal octane solution of 80 surfactant of glutaraldehyde cross-linking agent and 1-2wt% Span of 1wt%, and is slowly stirred, control is stirred
Speed 300-400r/min is mixed, crosslinking time is 30-60 minutes, then successively uses the ethanol solution and deionized water of 10-20wt%
Cleaning, drying, obtains carboxyl chitosan microballoon；
Step 3: the modification of carboxyl chitosan microballoon: by the isopropyl of the resulting carboxyl chitosan microballoon 30-50wt% of step 2
After alcoholic solution cleans 3-4 times repeatedly, it is transferred in the aqueous isopropanol containing 0.3-0.5wt% epoxychloropropane, 40-50 DEG C of water
It is impregnated 2-3 hours under the conditions of bath；Resulting carboxyl chitosan microballoon is transferred in 0.5-1wt% polyethylenimine solution again,
It under the conditions of lower than 60 DEG C, is slowly stirred, reacts 3-5 hours；Step 4: with deionized water successively to the resulting modification of step 3
Carboxyl chitosan microballoon cleans 3-4 times repeatedly；And dried under conditions of 30-40 DEG C, drying time 3-10 hours, obtain poly- second
The imine modified carboxyl chitosan adsorbent of alkene.
2. a kind of microfluidic control a kind of as described in claim 1 is for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI
Method, which is characterized in that dispersed phase described in step 1 is carboxyl chitosan and 0.5wt%-3wt% added with 2-4wt%
Glacial acetic acid mixed solution, continuous phase be the n-octyl alcohol solution added with 80 surfactant of 1-2wt% Span.
3. a kind of microfluidic control a kind of as described in claim 1 is for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI
Method, which is characterized in that the focused flow described in step 1 fluidic chip that declines is logical for upper and lower 2 strata methyl methacrylate plate
It crosses hot pressing to form, cover plate of upper layer contains 2 continuous phase entrances and a dispersed phase entrance, and lower layer's bottom plate is carved with cross microchannel
Conduit, three conduit endpoints of cross microchannel conduit and continuous phase and dispersed phase pass-through entry on cover board, it is one remaining
Conduit endpoint is microlayer model outlet；Microchannel channel width is 500-1000 μm.
4. a kind of microfluidic control a kind of as described in claim 1 is for the modified carboxyl chitosan heavy metal wastewater thereby adsorbent of PEI
Method, which is characterized in that wash number described in step 2 is 3-4 time, and the drying temperature is 30-40 DEG C, when drying
Between control at 6-10 hours.
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| CN111085148B (en) * | 2018-10-24 | 2021-12-21 | 中国科学院大连化学物理研究所 | Preparation method of chitosan microspheres with high specific surface area |
| CN109894099A (en) * | 2019-03-19 | 2019-06-18 | 西南科技大学 | A kind of trielement composite material and preparation method thereof based on polyethyleneimine |
| CN112090406A (en) * | 2020-08-24 | 2020-12-18 | 兰州理工大学 | Preparation method of polyethyleneimine modified chitosan magnetic composite material |
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| CN104741089A (en) * | 2015-02-15 | 2015-07-01 | 华东理工大学 | Method for preparing crosslinked-chitosan-system azo dye wastewater adsorbent |
| CN105396562A (en) * | 2015-12-18 | 2016-03-16 | 华东理工大学 | Microfluidic preparation method of porous chitosan metal ion adsorbent |
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| CN104741089A (en) * | 2015-02-15 | 2015-07-01 | 华东理工大学 | Method for preparing crosslinked-chitosan-system azo dye wastewater adsorbent |
| CN105396562A (en) * | 2015-12-18 | 2016-03-16 | 华东理工大学 | Microfluidic preparation method of porous chitosan metal ion adsorbent |
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