CN107868261A - A kind of carboxymethyl chitosan/oxidized graphene composite aquogel and its preparation and application - Google Patents
A kind of carboxymethyl chitosan/oxidized graphene composite aquogel and its preparation and application Download PDFInfo
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- CN107868261A CN107868261A CN201711270786.9A CN201711270786A CN107868261A CN 107868261 A CN107868261 A CN 107868261A CN 201711270786 A CN201711270786 A CN 201711270786A CN 107868261 A CN107868261 A CN 107868261A
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- carboxymethyl chitosan
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- composite aquogel
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- oxidized graphene
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/54—Aqueous solutions or dispersions
Abstract
The invention belongs to technical field of function materials, discloses a kind of carboxymethyl chitosan/oxidized graphene composite aquogel and its preparation and application.The preparation method of the carboxymethyl chitosan/oxidized graphene composite aquogel includes following preparation process：Carboxymethyl chitosan sugar aqueous solution is weighed, adds a certain amount of graphene oxide water solution, is stirred, finely dispersed carboxymethyl chitosan and graphene oxide dispersion is made；Lower a certain amount of TPMDMTI of dropwise addition is kept stirring for, ultrasonic deaeration, at room temperature reaction a period of time, carboxymethyl chitosan/oxidized graphene composite aquogel is made, described carboxymethyl chitosan sugar aqueous solution mass concentration is 10%.The preparation method preparation technology of the present invention is simple, easily operated, suitable for industrialized production.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of carboxymethyl chitosan/oxidized graphene Compound Water
Gel and its preparation and application.
Background technology
Chitosan is also known as chitosan, and containing a certain amount of amino and hydroxyl because of its surface can rise to metal ion
To complexing, relatively stable complex compound is formed, metal ion that can be effectively in adsorbent solution.Chitosan can not be direct
It is dissolved in the aqueous solution, can only be dissolved in acid solution, but in acid condition, chitosan is easily degraded and the ammonia on its surface
Base mainly exists in the form of-NH3+, is not easy to complexing of metal ion, largely limits it and purifies neck in wastewater treatment
Application in domain.
Carboxymethyl chitosan be chitosan in the basic conditions with chloroacetate reaction made from a kind of water soluble chitosan spread out
Biology, because the introducing of carboxyl, improve its dissolubility in water.In addition, the carboxyl being introduced into can be with the metal in solution
Ion coordination, the metal ion in adsorbent solution, so as to reach the purpose of purification sewage.But because carboxymethyl chitosan is dissolved in
In water, after the completion of absorption, it is difficult to complex compound is kept completely separate out from system, therefore probe into out a kind of adsorption capacity it is strong and
The metal ion adsorption material for being easy to separate from system has very actual meaning.
Important growth of the graphene oxide as graphene, because its surface contain more oxygen-containing functional group such as-OH ,-
COOH ,-O-, C=O etc., graphene oxide thin slice is promoted to have very strong water-wet behavior, so as to be easily dispersed water and organic molten
In agent.In addition, graphene oxide thin slice has larger specific surface area and a large amount of carboxyl functional groups, promote itself and other materials
It is compound, while composite material strength performance, thermal stability is improved, effectively improve its suction-operated to metal ion.
The content of the invention
In order to solve the shortcomings that above prior art and weak point, primary and foremost purpose of the invention is to provide a kind of carboxylic
The preparation method of methyl chitosan/graphene oxide composite aquogel.
Another object of the present invention is to provide carboxymethyl chitosan/oxidized graphene made from above-mentioned preparation method to answer
Heshui gel.
It is still another object of the present invention to provide above-mentioned carboxymethyl chitosan/oxidized graphene composite aquogel as gold
Belong to the application of ionic complexing agent.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel, comprises the following steps：By graphite oxide
Aqueous solution adds carboxymethyl chitosan sugar aqueous solution and stirred, and obtains finely dispersed carboxymethyl chitosan and oxidation stone
Black alkene dispersion liquid；Be added dropwise under the conditions of being kept stirring for a certain amount of 4,4 '-dimethyl triphenyl methane -2,2 ', 5,5 '-four isocyanides
Acid esters (hereinafter referred to as TPMDMTI), ultrasonic deaeration, at room temperature reaction a period of time, extruding filter out unnecessary moisture, made
Carboxymethyl chitosan/oxidized graphene composite aquogel is obtained, described carboxymethyl chitosan sugar aqueous solution mass concentration is 10%.
The carboxymethyl chitosan sugar aqueous solution is made by following steps：Carboxymethyl chitosan is weighed, is dissolved in deionized water
In the carboxymethyl chitosan sugar aqueous solution of certain mass concentration is made, magnetic agitation to carboxymethyl chitosan is completely dissolved, and obtains carboxylic
The methyl chitosan aqueous solution；Described deionized water resistivity is 18.2M Ω cm.
Preferably, graphene oxide water solution used is prepared according to improved Hummers methods, wherein graphene oxide
Content be 5.0mg/mL.
Preferably, it is contained in the carboxymethyl chitosan in the carboxymethyl chitosan solution and graphene oxide water solution
The mass ratio of graphene oxide is (30~40):1；More preferably 35:1.
Preferably, the TPMDMTI additions are the 1.5~2.0% of the quality of carboxymethyl chitosan.
Preferably, the rotating speed of the stirring is 300~350r/min.
Preferably, TPMDMTI rate of addition is controlled in 1-2 drops/s.
Preferably, the ultrasonic power of the ultrasonic deaeration is 300~400w, 15~20min of time.
Preferably, the time of room temperature reaction is 3~4h.
Carboxymethyl chitosan/oxidized graphene composite aquogel made from above-mentioned preparation method.
Above-mentioned carboxymethyl chitosan/oxidized graphene composite aquogel is removing electricity as metal plating waste water adsorbent
Plate the application in industrial wastewater heavy metal ion.
Above-mentioned application process is preferably：Carboxymethyl chitosan/oxidized graphene composite aquogel is put into containing a huge sum of money
Belong in ion plating industrial wastewater, carry out oscillation treatment at room temperature, reduce the content of heavy metal ion in metal plating waste water.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) carboxymethyl chitosan/oxidized graphene composite aquogel preparation method preparation technology of the invention is simple, is easy to grasp
Make, suitable for industrialized production.
(2) carboxymethyl chitosan/oxidized graphene composite aquogel produced by the present invention can effectively reduce electroplating industry
The content of heavy metal ions in wastewater, wherein Pb2+ maximal absorptive capacities are that 471.12mg/g, Ni2+ maximal absorptive capacity are
197.54mg/g, Cd2+ maximal absorptive capacity are 97.47mg/g.
(3) carboxymethyl chitosan/oxidized graphene composite aquogel is used to remove metal plating waste water heavy metal ion
Afterwards, composite aquogel still keeps good mechanical strength, is easy to separate from system for handling, before having good application
Scape.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Graphene oxide water solution used is prepared via a method which in the embodiment of the present invention：
(1) fill in dense H2SO4 reaction vessels, add a certain amount of graphite powder and NaNO3, after stirring 20min in ice-water bath,
Add KMnO4, then react 45min at 40 DEG C, add deionized water, react 20min at 95 DEG C, continuously add from
The H2O2 of sub- water and certain volume, now reaction system be changed into glassy yellow.
(2) deionized water centrifuge washing is used after product is filtered, removes unnecessary acid.Product after washing be put into from
In sub- water, be ultrasonically treated (power 360W, 8min), it is scattered in deionized water, then dialysis remove residual metal from
Son, it is graphene oxide water solution that supernatant is taken after high speed centrifugation (rotating speed 5000r/min).
Carboxymethyl chitosan used is prepared via a method which in the embodiment of the present invention：
(1) 20.0g chitosans are weighed, 27.0gNaOH, are added in the isopropanol water solution that 200mL volume fractions are 50%,
At a temperature of 65 DEG C, swelling and basification 45min.40mL is then added dropwise dissolved with the chloroacetic aqueous isopropanols of 30g,
It is 2-3 drops/s to control rate of addition, reacts 3h at 65 DEG C.After reaching the reaction time, it is 70% to add 500mL volume fractions
Ethanol solution terminating reaction, with volume fraction be 80% ethanol water fully wash gained solid, obtain pure
Carboxymethyl chitosan sodium salt.
(2) 5.0g carboxymethyl chitosan sodium salts obtained above are weighed, are added to the second that 500mL volume fractions are 80%
In alcoholic solution, magnetic agitation 15min, carboxymethyl chitosan sodium salt suspension is made.50mL is then added, volume fraction is
37% concentrated hydrochloric acid, magnetic agitation 40min, it is 80% ethanol water centrifuge washing to neutrality with volume fraction, is dried in vacuo
Final carboxymethyl chitosan is obtained, its substitution value (Ds) is 0.81.
Embodiment 1
Carboxymethyl chitosan 5g is weighed, is dissolved in the aqueous solution for being made that mass concentration is 5% in 95g water, magnetic agitation to carboxymethyl
Chitosan is completely dissolved, and then adds 33mL graphene oxide water solutions (wherein the content of graphene oxide is 5.0mg/mL),
1h is stirred with 300r/min, finely dispersed carboxymethyl chitosan and graphene oxide dispersion is made.It is kept stirring for lower dropwise addition
0.075gTPMDMTI, ultrasonic deaeration (power 300w, time 15min), 3h is reacted at room temperature, it is unnecessary that extruding filters out
Moisture, carboxymethyl chitosan/oxidized graphene composite aquogel is made.
Embodiment 2
Carboxymethyl chitosan 10g is weighed, is dissolved in the aqueous solution for being made that mass concentration is 5% in 190g water, magnetic agitation to carboxylic
Methyl chitosan is completely dissolved, and then adding 57ml graphene oxide water solutions, (wherein the content of graphene oxide is 5.0mg/
ML), 1h is stirred with 350r/min, finely dispersed carboxymethyl chitosan and graphene oxide dispersion is made.It is kept stirring for down
0.175gTPMDMTI is added dropwise, ultrasonic deaeration (power 350w, time 15min), reacts 3.5h at room temperature, extruding filters out
Unnecessary moisture, carboxymethyl chitosan/oxidized graphene composite aquogel is made.
Embodiment 3
Carboxymethyl chitosan 15g is weighed, is dissolved in the aqueous solution for being made that mass concentration is 5% in 285g water, magnetic agitation to carboxylic first
Base enclosure glycan is completely dissolved, and then adding 75ml graphene oxide water solutions, (wherein the content of graphene oxide is 5.0mg/
ML), 1h is stirred with 400r/min, finely dispersed carboxymethyl chitosan and graphene oxide dispersion is made.It is kept stirring for down
0.30gTPMDMTI is added dropwise, ultrasonic deaeration (power 400w, time 20min) reacts 4h at room temperature, and extruding filters out more
Remaining moisture, carboxymethyl chitosan/oxidized graphene composite aquogel is made.
Using test：
The carboxymethyl chitosan/oxidized graphene composite aquogel processing metal plating waste water that embodiment 1~3 is prepared
Performance detected respectively, specific testing procedure is as follows：
The above-mentioned carboxymethyl chitosan/oxidized graphene composite aquogel 2.0g prepared is taken respectively, is added to 200mL and is contained
The metal plating waste water of heavy metal ion, adjust the pH=5.7 of solution, room temperature condition oscillation treatment 12h., will after the completion of processing
Carboxymethyl chitosan/oxidized graphene composite aquogel takes out, electroplating industry before and after being adsorbed by atomic radiations spectrographic determination
The change of heavy metal ions in wastewater (Pb2+, Ni2+, Cd2+) concentration.
The effect of heavy metal ion in the carboxymethyl chitosan/oxidized graphene composite aquogel absorption metal plating waste water
Much better than carboxymethyl chitosan effect of fruit, in preferred embodiment 2, to the metal ion species of Pb2+, Ni2+, Cd2+ tri- most
Big adsorbance is respectively 471.12mg/g, 197.54mg/g, 97.47mg/g, and the adsorbance compared with carboxymethyl chitosan improves successively
115.96%th, 144.66%, 49.17%.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, letter
Change, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel, it is characterised in that including following step
Suddenly：Graphene oxide water solution is added into carboxymethyl chitosan sugar aqueous solution and stirred, obtains carboxymethyl chitosan and oxidation
Graphene dispersing solution；Be added dropwise under the conditions of being kept stirring for a certain amount of 4,4 '-dimethyl triphenyl methane -2,2 ', 5,5 '-four is different
Cyanate, ultrasonic deaeration, at room temperature reaction a period of time, extruding filtering, carboxymethyl chitosan/oxidized graphene is made and answers
Heshui gel, described carboxymethyl chitosan sugar aqueous solution mass concentration are 10%.
2. the preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel according to claim 1, its feature
It is, contained graphene oxide in the carboxymethyl chitosan and graphene oxide water solution in the carboxymethyl chitosan solution
Mass ratio be (30~40):1.
3. the preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel according to claim 1, its feature
It is, contained graphene oxide in the carboxymethyl chitosan and graphene oxide water solution in the carboxymethyl chitosan solution
Mass ratio be 35:1.
4. the preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel according to claim 1, its feature
It is, the time of the room temperature reaction is 3~4h.
5. the preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel according to claim 1, its feature
It is, the content of graphene oxide is 5.0mg/mL in graphene oxide water solution used.
6. the preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel according to claim 1, its feature
It is, described 4,4 '-dimethyl triphenyl methane -2,2 ', 5,5 '-tetraisocyanate addition is the matter of carboxymethyl chitosan
The 1.5~2.0% of amount.
7. the preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel according to claim 1, its feature
It is, the rotating speed of the stirring is 300~350r/min；The ultrasonic power of the ultrasonic deaeration is 300~400w, the time 15
~20min.
8. a kind of carboxymethyl chitosan/oxidized graphene composite aquogel, it is characterised in that it is any by claim 1 to 8
The preparation method of carboxymethyl chitosan/oxidized graphene composite aquogel described in is made.
9. the carboxymethyl chitosan/oxidized graphene composite aquogel described in claim 9 adsorbs as metal plating waste water
Application of the agent in metal plating waste water heavy metal ion is removed.
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| CN201711270786.9A CN107868261A (en) | 2017-12-05 | 2017-12-05 | A kind of carboxymethyl chitosan/oxidized graphene composite aquogel and its preparation and application |
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| CN201711270786.9A CN107868261A (en) | 2017-12-05 | 2017-12-05 | A kind of carboxymethyl chitosan/oxidized graphene composite aquogel and its preparation and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108728929A (en) * | 2018-05-28 | 2018-11-02 | 泽塔纳米科技（苏州）有限公司 | A kind of nano-fiber material and preparation method thereof of filtering heavy metal ion |
| CN113683786A (en) * | 2021-08-03 | 2021-11-23 | 武汉理工大学 | Dual self-healing antibacterial hydrogel and preparation method and application thereof |
| CN114307980A (en) * | 2021-12-27 | 2022-04-12 | 中国人民解放军火箭军工程大学 | Composite material and composition for treating unsymmetrical dimethylhydrazine pollutants, and treatment method and experimental method thereof |
-
2017
- 2017-12-05 CN CN201711270786.9A patent/CN107868261A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108728929A (en) * | 2018-05-28 | 2018-11-02 | 泽塔纳米科技（苏州）有限公司 | A kind of nano-fiber material and preparation method thereof of filtering heavy metal ion |
| CN108728929B (en) * | 2018-05-28 | 2021-06-11 | 泽塔纳米科技（苏州）有限公司 | Nanofiber material for filtering heavy metal ions and preparation method thereof |
| CN113683786A (en) * | 2021-08-03 | 2021-11-23 | 武汉理工大学 | Dual self-healing antibacterial hydrogel and preparation method and application thereof |
| CN113683786B (en) * | 2021-08-03 | 2023-12-12 | 武汉理工大学 | Double self-healing antibacterial hydrogel and preparation method and application thereof |
| CN114307980A (en) * | 2021-12-27 | 2022-04-12 | 中国人民解放军火箭军工程大学 | Composite material and composition for treating unsymmetrical dimethylhydrazine pollutants, and treatment method and experimental method thereof |
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Application publication date: 20180403 |