CN107684904A - A kind of chitose magnetic fluid water quality purification material, preparation method and applications - Google Patents
A kind of chitose magnetic fluid water quality purification material, preparation method and applications Download PDFInfo
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- CN107684904A CN107684904A CN201711056774.6A CN201711056774A CN107684904A CN 107684904 A CN107684904 A CN 107684904A CN 201711056774 A CN201711056774 A CN 201711056774A CN 107684904 A CN107684904 A CN 107684904A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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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- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The present invention relates to natural polymer nano composite material and purification of water quality process field, disclose a kind of chitose magnetic fluid water quality purification material, preparation method and applications, the preparation method of chitose magnetic fluid water quality purification material its be included in the solution dissolved with chitosan and add Fe2+、Fe3+Ion；It is being mixed with chitosan and Fe2+、Fe3+Add excessive water in the solution of ion to be diluted, the volume of the water added is 3~4 times of blend step resulting solution volume；And stir the solution for diluting gained under alkaline environment, more than 4h is then aged, obtains ferrofluid suspension.This method is simple, and cost is cheap, the nanometer Fe in gained chitose magnetic fluid3O4Uniform particle diameter, dispersiveness preferably, can effectively purified industrial waste water, such as dyestuff, heavy metal.
Description
Technical field
The present invention relates to natural polymer nano composite material and field of industrial waste water treatment, in particular to one kind
Chitose magnetic fluid water quality purification material, preparation method and applications.
Background technology
The processing method of industrial wastewater has a lot, and conventional processes include precipitation/flocculation, biodegradation, activated carbon suction
It is attached etc.；Emerging handling process has oxidizing process, electrochemical process, membrane separation process, absorption method, ion-exchange etc..Wherein, absorption method
The advantages that its is easy to operate, equipment is cheap, removal effect is high, is widely used in water treatment field.Acticarbon is as one
Kind of conventional industrial adsorbents, it is versatile, removal efficiency is high, but its regeneration is difficult, and it is expensive, it is extensive to limit its
Use.It is safe and non-toxic because chitosan is cheap, good biocompatibility, substantial amounts of active group be present in its molecular structure
Group --- free amino group and hydroxyl, meanwhile, the hydrogen bond of skeleton interchain forms secondary structure, particularity in this structure and
The physical characteristic of high-molecular compound so that chitosan has ion exchange, chela to many ions, organic matter, biomolecule etc.
The effects such as conjunction, absorption, can be used as sorbent treatment industrial wastewater in several ways with the pollutant in waste water.
The existing technology for preparing chitose magnetic fluid mainly has two kinds, when coprecipitation, second, reversed-phase emulsion cross-linking method,
Wherein emulsion-crosslinking method is most widely used.The experiment condition requirement multipair greatly of these methods is more harsh, and these were prepared
Journey is mostly by Fe3O4The preparation of nano-particle separates with overall preparation process, adds the difficulty in experiment implementation process.
Nanometer Fe3O4Preparation method mainly have micro emulsion method, hydro-thermal method, thermal decomposition method and chemical coprecipitation, nanometer made from micro emulsion method
Fe3O4Uniform particle sizes, but wherein surfactant is difficult to remove, and nano-particle yield is relatively low；Nanoparticle seed prepared by hydro-thermal method
Degree is evenly distributed, and crystal formation is good, but requires higher to preparation condition, need to be carried out in sealed high-pressure vessel, and different temperatures
Directly affect particle size；Nano-particle purity made from thermal decomposition method is high, but pyroreaction easily induces nucleation, makes cluster of grains
It is poly-；Chemical precipitation method is simple to operate, but gained nano-particle is easily reunited, and particle diameter is difficult homogeneous.
The content of the invention
It is an object of the invention to provide a kind of preparation method of chitose magnetic fluid water quality purification material, it passes through original position
The step of coprecipitation one is made, and method is simple, and cost is cheap, the nanometer Fe in products therefrom3O4Uniform particle diameter, dispersiveness preferably, are inhaled
Attached amount is big.
It is still another object of the present invention to provide a kind of chitose magnetic fluid water quality purification material in absorption azo dyes
And the application gone in removing heavy metals.
What embodiments of the invention were realized in：
A kind of preparation method of chitose magnetic fluid water quality purification material, it includes：
Blend step：Fe is added in the solution dissolved with chitosan2+、Fe3+Ion；
Dilution step：It is being mixed with chitosan and Fe2+、Fe3+Excessive water is added in the solution of ion, the water added
Volume be 3~4 times of blend step resulting solution volume；And
Settling step：Solution obtained by dilution step is stirred under alkaline environment, is then aged more than 4h.
In an embodiment of the present invention, the dilution step of the preparation method of above-mentioned chitose magnetic fluid water quality purification material
In rapid, add after excessive water, to the chitosan and Fe after dilution2+、Fe3+The mixed solution of ion is stirred, stirring
Time is 20~30min.
In an embodiment of the present invention, in the preparation method of above-mentioned chitose magnetic fluid water quality purification material, precipitation
The alkaline environment of step is realized by adding 1~1.5mol/L NaOH solution.
In an embodiment of the present invention, in the preparation method of above-mentioned chitose magnetic fluid water quality purification material, dilution
The temperature control of step is at 40~80 DEG C.
In an embodiment of the present invention, the preparation method blend step of above-mentioned chitose magnetic fluid water quality purification material
In, Fe2+、Fe3+The mol ratio of ion is 1:2.
In an embodiment of the present invention, the mixing step of the preparation method of above-mentioned chitose magnetic fluid water quality purification material
The solution dissolved with chitosan in rapid is obtained by the way that chitosan is dissolved under sour environment；Fe2+、Fe3+It is first dissolved in water shape
Into containing Fe2+、Fe3+Solution, then mixed with the solution dissolved with chitosan.
In an embodiment of the present invention, the mixing step of the preparation method of above-mentioned chitose magnetic fluid water quality purification material
Solution temperature in rapid is controlled at 40~80 DEG C.
In an embodiment of the present invention, the precipitation step of the preparation method of above-mentioned chitose magnetic fluid water quality purification material
Whipping temp in rapid is 40~80 DEG C, and the disperse system after stirring is aged at room temperature.
A kind of chitose magnetic fluid water quality purification material, its by above-mentioned chitose magnetic fluid water quality purification material preparation
Method is made.
Above-mentioned chitose magnetic fluid water quality purification material is in absorption azo dyes or the application gone in removing heavy metals.
The beneficial effect of the embodiment of the present invention is：
Chitose magnetic fluid water quality purification material provided by the invention is made by the step of coprecipitation one in situ, including
It is blended with chitosan and Fe2+、Fe3+Excessive water is added in the solution of ion, the volume of the water added is blend step institute
Obtain 3~4 times of liquor capacity；And stir the solution obtained by dilution step under alkaline environment, to form chitosan magnetic current
Body, then it is aged more than 4h.This method is simple, and cost is cheap, the nanometer Fe in products therefrom3O4Uniform particle diameter, dispersiveness compared with
It is good, it can effectively purify azo dyes and heavy metal.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the chitose magnetic fluid water quality purification material in the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope picture of the chitose magnetic fluid water quality purification material in the embodiment of the present invention 1；
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.
Main agents：Chitosan (deacetylation 80-95%, viscosity average molecular weigh are 3.0 × 105g/mol), glacial acetic acid, hydrogen
Sodium oxide molybdena, concentrated hydrochloric acid, FeCl3·6H2O and FeCl2·4H2O, section's dragon chemical reagent factory (Chinese Chengdu).All compounds are
Commercially available chemicals, without being further purified.Ultra-pure water used in all experiments is Milli-Q water purification systems (Ulupure
Company) produce.
Key instrument:PHS-320 acidometers (Chengdu ShiJiFangZhou Science and Technology Ltd.), SHZ-82 water-baths vibration case (river
Revive Jintan City Jin Cheng Guo Sheng laboratory apparatus factory), BSA224S-CW electronic balances (Sai Duolisi scientific instrument Co., Ltd).
A kind of preparation method of chitose magnetic fluid water quality purification material of the present invention comprises the following steps：
First, blend step.
0.5~1g chitosans are added in 50mL acid solutions, alternatively, the concentration that acid solution selection is 50mL is 2~
4% acetum.In order that chitosan preferably dissolves, 20~30min stirring is carried out in embodiment to chitosan solution,
Mixing speed is 200~300r/min, and it is 40~80 DEG C to control solution temperature.
Fe will be contained2+、Fe3+The mixed solution of ion is slowly added into the solution dissolved with chitosan, alternatively, Fe2+
With Fe3+The mol ratio of ion is 1:2.In an embodiment of the present invention, containing Fe2+、Fe3+The mode of the mixed solution of ion is,
By 0.81g FeCl3·6H2O and 0.2891gFeCl2·4H2O is added in 100mL ultra-pure waters, is obtained containing Fe2+、Fe3+Ion
Mixed solution.Water used in embodiments of the invention uses ultra-pure water, to reduce influence of the Impurities In Solvents to product, because super
The oxygen content of pure water is seldom, therefore can prevent ferrous oxidising.In the case where not influenceing product effect, can also use purity compared with
Low water.
To being mixed with chitosan and Fe2+、Fe3+The solution of ion carries out 40~80 DEG C of constant temperature stirring, and mixing speed is
200~300r/min, 30~50min of duration, solution are changed into orange red.Stop stirring afterwards, stand 10~20min, make
Solution is fully aged.
2nd, dilution step.
450~600mL ultra-pure waters are added in the solution obtained by blend step, and stir 20~30min, then stand 10
~20min so that solution is scattered more uniform.
3rd, settling step.
Aqueous slkali is added in the mixed solution obtained by dilution step, in an embodiment of the present invention, is slowly added to
40mL 1~1.5mol/L NaOH solutions, are stirred vigorously, and it is 40~80 DEG C to control temperature, mixing speed 600-800r/
Min, mixing time are 40~60min, obtain suspension；After stopping reaction, suspension is aged more than 4 hours at room temperature,
Cleaned again with ultra-pure water to neutrality and obtain chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
It should be noted that in addition to room temperature is carried out, it is related to except by the operation of suspension ageing more than 4 hours containing Fe2+、Fe3+
Stirring, the reaction of ion all should carry out in 40~80 DEG C of water bath with thermostatic control, and be passed through protective gas to prevent ferrous ion
Oxidation, optional protective gas are nitrogen, argon gas etc..
Embodiment 1
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：0.5g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is extremely
It is completely dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
500mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 25min.15min is stood again；
S3, settling step
40mL 1.25mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min,
Mixing time is 40min；Stop reaction after, suspension is aged at room temperature 4 hours, using ultra-pure water by suspension clean to
Neutrality obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 80 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 59%.
Embodiment 2
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：0.7g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is extremely
It is completely dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
500mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 25min.15min is stood again；
S3, settling step
40mL 1.25mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min,
Mixing time is 40min；Stop reaction after, suspension is aged at room temperature 4 hours, using ultra-pure water by suspension clean to
Neutrality obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 80 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 82.6%.
Embodiment 3
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：1g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is to complete
Fully dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
500mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 25min.15min is stood again；
S3, settling step
40mL 1.25mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min,
Mixing time is 40min；Stop reaction after, suspension is aged at room temperature 4 hours, using ultra-pure water by suspension clean to
Neutrality obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 80 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 118%.
Embodiment 4
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：0.5g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is extremely
It is completely dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
400mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 20min.15min is stood again；
S3, settling step
40mL 1.25mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min,
Mixing time is 40min；Stop reaction after, suspension is aged at room temperature 4 hours, using ultra-pure water by suspension clean to
Neutrality obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 60 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 59%.
Embodiment 5
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：0.7g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is extremely
It is completely dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
400mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 20min.15min is stood again；
S3, settling step
40mL 1.25mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min,
Mixing time is 40min；Stop reaction after, suspension is aged at room temperature 4 hours, using ultra-pure water by suspension clean to
Neutrality obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 60 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 82.6%.
Embodiment 6
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：1g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is to complete
Fully dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
400mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 30min.15min is stood again；
S3, settling step
40mL 1.25mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min,
Mixing time is 40min；Stop reaction after, suspension is aged at room temperature 4 hours, using ultra-pure water by suspension clean to
Neutrality obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 60 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 118%.
Embodiment 7
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：0.5g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is extremely
It is completely dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
600mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 30min.15min is stood again；
S3, settling step
40mL 1.5mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min, are stirred
It is 40min to mix the time；After stopping reaction, suspension is aged at room temperature 4 hours, cleaned suspension into using ultra-pure water
Property obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 40 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 59%.
Embodiment 8
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：0.7g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is extremely
It is completely dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
600mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 30min.15min is stood again；
S3, settling step
40mL 1.5mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min, are stirred
It is 40min to mix the time；After stopping reaction, suspension is aged at room temperature 4 hours, cleaned suspension into using ultra-pure water
Property obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 40 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 82.6%.
Embodiment 9
The present embodiment provides a kind of preparation method of chitose magnetic fluid water quality purification material, and it comprises the following steps：
S1, blend step
Dissolve chitosan：1g chitosans are added in three-neck flask, add the acetums of 50mL 2%, mechanical agitation is to complete
Fully dissolved, mixing speed 200r/min, mixing time 20min；
The preparation of chitosan and Fe (II, III) mixed solution：Weigh 0.81g FeCl3·6H2O and 0.2891g FeCl2·
4H2O, add 100mL ultra-pure waters to dissolve, and mixed solution is poured slowly into flask, it is orange red, stirring speed that constant temperature, which is stirred to solution,
Spend for 200r/min, time 30min.Agitator is closed, stands 15min；
S2, dilution step
600mL ultra-pure waters are first added into flask, then open agitator, mixing speed 200r/min, mixing time
For 30min.15min is stood again；
S3, settling step
40mL 1.5mol/L NaOH solutions are poured slowly into flask, are stirred vigorously, mixing speed 600r/min, are stirred
It is 40min to mix the time；After stopping reaction, suspension is aged at room temperature 4 hours, cleaned suspension into using ultra-pure water
Property obtains chitosan magnetic nanometer suspension, i.e. chitose magnetic fluid water quality purification material.
Above step except suspension is aged 4 hours and operation afterwards in addition to, enter in 40 DEG C of waters bath with thermostatic control
OK, and be passed through nitrogen with evacuation of air, prevent it is ferrous oxidising, beneficial to the generation of ferroso-ferric oxide.Obtained chitosan magnetic current
The duty factor of body water quality purification material is 118%.
It is below the operating parameter of each embodiment and adsorbs Congo red adsorbance.
The operating parameter of 1 each embodiment of table and the adsorbance to wastewater treatment
It should be noted that adsorbance here is the adsorbance of the chitose magnetic fluid of unit quality, the shell in each embodiment gathers
The quality of sugared magnetic fluid water quality purification material is to calculate gained after drying.
Electron microscopic observation will be done after the chitose magnetic fluid water quality purification material drying of embodiment 1.Fig. 1 is the embodiment of the present invention
The scanning electron microscope (SEM) photograph of chitose magnetic fluid water quality purification material in 1；Fig. 2 is chitose magnetic fluid water quality in the embodiment of the present invention 1
The transmission electron microscope picture of scavenging material.As seen from the figure, torispherical and the nanometer Fe of ellipse3O4Particle is well dispersed, particle size compared with
Homogeneous, average grain diameter is about 8nm, and the grain shape of chitosan magnetic is irregular, but mostly ball-type, and average grain diameter is about 19nm,
It is uniformly dispersed, is not easy to reunite.Coprecipitation in situ is by Chitosan-coated in Fe3O4Particle surface so that magnetic particle it is skin-deep from
By that can decline, magnetic particle particle aggregation and sedimentation because caused by closing to mutually is stopped, has played dispersant and stabilizer
Function.On the other hand, due to the restriction effect of chitosan, the chitose magnetic fluid nano-particle average grain diameter formed is less than phase
Like the Fe obtained under reaction condition3O4The average grain diameter of nano-particle.The chitose magnetic fluid water of the embodiment of the present invention 1 after tested
Matter scavenging material can reach more than 1700mg/g to Congo red adsorbance, and heavy metal ion also has preferable treatment effect.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
- A kind of 1. preparation method of chitose magnetic fluid water quality purification material, it is characterised in that the chitose magnetic fluid water quality The preparation method of scavenging material includes：Blend step：Fe is added in the solution dissolved with chitosan2+、Fe3+Ion；Dilution step：It is being mixed with the chitosan and the Fe2+、Fe3+Excessive water is added in the solution of ion, is added The volume of water is 3~4 times of the blend step resulting solution volume；AndSettling step：Solution obtained by the dilution step is stirred under alkaline environment, is then aged more than 4h.
- 2. the preparation method of chitose magnetic fluid water quality purification material according to claim 1, it is characterised in that described dilute Release in step, add after excessive water, to the chitosan after dilution and the Fe2+、Fe3+The mixed solution of ion enters Row stirring, the time of stirring is 20~30min.
- 3. the preparation method of chitose magnetic fluid water quality purification material according to claim 1, it is characterised in that described heavy The alkaline environment of shallow lake step is realized by adding 1~1.5mol/L NaOH solution.
- 4. the preparation method of chitose magnetic fluid water quality purification material according to claim 1, it is characterised in that described dilute The temperature control of step is released at 40~80 DEG C.
- 5. the preparation method of chitose magnetic fluid water quality purification material according to claim 1, it is characterised in that described mixed Close the Fe in step2+、Fe3+The mol ratio of ion is 1:2.
- 6. the preparation method of chitose magnetic fluid water quality purification material according to claim 1, it is characterised in that described mixed The solution dissolved with chitosan closed in step is obtained by the way that the chitosan is dissolved under sour environment；The Fe2+、 Fe3+It is first dissolved in water formation and contains Fe2+、Fe3+Solution, then mixed with the solution dissolved with chitosan.
- 7. the preparation method of chitose magnetic fluid water quality purification material according to claim 1, it is characterised in that described mixed The solution temperature closed in step is controlled at 40~80 DEG C.
- 8. the preparation method of chitose magnetic fluid water quality purification material according to claim 1, it is characterised in that described heavy Whipping temp in the step of shallow lake is 40~80 DEG C, and the disperse system after the stirring is aged at room temperature.
- A kind of 9. chitose magnetic fluid water quality purification material, it is characterised in that the chitose magnetic fluid water quality purification material by The preparation method of chitose magnetic fluid water quality purification material any one of claim 1 to 8 is made.
- 10. chitose magnetic fluid water quality purification material as claimed in claim 9 is in absorption azo dyes or removes removing heavy metals In application.
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| CN115215422A (en) * | 2022-05-19 | 2022-10-21 | 成都理工大学 | Method for remedying underground water organic pollution by in-situ reaction zone |
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