CN109225146A - Chitosan-based compound emergency material of one kind and its preparation method and application - Google Patents
Chitosan-based compound emergency material of one kind and its preparation method and application Download PDFInfo
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- CN109225146A CN109225146A CN201811031185.7A CN201811031185A CN109225146A CN 109225146 A CN109225146 A CN 109225146A CN 201811031185 A CN201811031185 A CN 201811031185A CN 109225146 A CN109225146 A CN 109225146A
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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
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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
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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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
Abstract
The invention discloses a kind of chitosan-based compound emergency materials and its preparation method and application, are related to environmental technology field, the preparation method includes the following steps: (1) that cotton fiber is placed in sodium periodate solution, under the conditions of being protected from light, concussion 2h is carried out, takes out, obtains product A；The product A is dipped in ethylene glycol solution by step 2, is shaken, obtains product B；Step 3, by after the product B ethanol washing, be dipped in tetraethylenepentamine solution, shaken, obtain product C；Step 4, by after the product C ethanol washing, be placed in glutaraldehyde solution, shaken, obtain product D；The product D is placed in chitosan acetic acid solution by step 5, is shaken, obtains product E；Step 6 carries out vacuum drying treatment to the product E using vacuum desiccator, obtains chitosan-based compound emergency material.Emergency material of the invention has preferable adsorption capacity, and preparation process is simple, and cost is relatively low.
Description
Technical field
The present invention relates to environmental technology field, more particularly to a kind of chitosan-based compound emergency material and preparation method thereof with
Using.
Background technique
Water is the source of all life, is the important physical resources that the mankind depend on for existence and development.In recent years, with urbanization
With the quickening of process of industrialization, water body environment is by increasingly severe destruction, especially heavy metal in water suddenly accident
It is commonplace.At present in water the minimizing technology of heavy metal mainly have chemical precipitation method, ion-exchange, coacervation, membrane separation process,
Electrochemical process, oxidation-reduction method, ferrite process and absorption method etc., wherein absorption method is due to easy to operate, high-efficient etc. excellent
It puts and is concerned.
Currently, common adsorbent material is mainly absorbent charcoal material, but problems faced is most of absorbent charcoal material
It is at high cost, production technology is complicated and is difficult to recycle.Particularly, for the burst heavy metal pollution accident such as river water, nothing
The active carbon of method recycling often results in water body environment secondary pollution.
In recent years, the method for biological adsorption heavy metal advantage efficient with its, cheap is shown one's talent gradually, to this method
Research also makes great progress.But biosorption technology is mostly at the experimental stage, from it is industrialized application there is also compared with
Big gap.Main reason is that selecting desorption appropriate how under the premise of not influencing biomaterial quality and adsorption capacity
Heavy metal is recycled in agent, how more efficient and inexpensive adsorbed water body heavy metal, be all urgently to be resolved to ask at present
Topic.
Therefore, those skilled in the art be dedicated to developing a kind of chitosan-based compound emergency material and preparation method thereof with
Using method to obtain a kind of efficient, recyclable and environmentally friendly adsorption cleaning heavy metal in water ion, to effectively control
Heavy metal pollution of water body processed.
Summary of the invention
In view of the above drawbacks of the prior art, the technical problem to be solved by the present invention is to how to provide it is a kind of efficiently,
The method of recyclable and environmentally friendly adsorption cleaning heavy metal in water ion, effectively to control the heavy metal pollution of water body.
To achieve the above object, the present invention provides a kind of preparation methods of chitosan-based compound emergency material, including such as
Lower step: cotton fiber is placed in sodium periodate solution by step 1, under the conditions of being protected from light, carries out first time concussion, the first time
The time of concussion is 2h, takes out, obtains product A；The product A is dipped in ethylene glycol solution by step 2, is carried out second and is shaken
It swings, obtains product B；Step 3, by after the product B ethanol washing, be dipped in tetraethylenepentamine solution, carry out third time shake
It swings, obtains product C；Step 4, by after the product C ethanol washing, be placed in glutaraldehyde solution, carry out the 4th time concussion, obtain
To product D；The product D is placed in chitosan acetic acid solution by step 5, is carried out the 5th concussion, is obtained product E；Step 6,
Vacuum drying treatment is carried out to the product E using vacuum desiccator, obtains chitosan-based compound emergency material.
Further, in the step 1, the concentration of the sodium periodate solution is 20~30mmol/L, the cotton fiber
Bath raio between the sodium metaperiodate is 20:1, and the weight of the cotton fiber is 2g, and the temperature for being protected from light condition is 40 DEG C.
Further, in the step 2, the volume fraction of the ethylene glycol solution is 2~3%, second of concussion
Time be 20~30min, bath raio between the product A and the ethylene glycol solution is 30:1.
Further, in the step 3, the volume fraction of the tetraethylenepentamine solution is 20%, volume 50mL, institute
The time for stating third time concussion is 10~12h, and the environment temperature when third time is shaken is 60 DEG C.
Further, in the step 4, the volume fraction of the glutaraldehyde solution is 1~2%, the 4th concussion
Time be 30min, described 4th time concussion when environment temperature be 30 DEG C.
Further, in the step 5, the time of the 5th concussion is 10~30min, when the 5th concussion
Environment temperature be 30 DEG C, the volume fraction of the chitosan acetic acid solution is 2%.
Further, sodium periodate solution described in the step 1 is 30mmol/L, ethylene glycol described in the step 2
The volume fraction of solution is 2%, the time of second of concussion is 30min, shaken for the third time described in the step 3 when
Between be 12h, the volume fraction of glutaraldehyde solution described in the step 4 is 1%, the 5th concussion described in the step 5
Time is 30min.
The present invention also provides a kind of chitosan-based compound emergency materials, and the chitosan-based compound emergency material is by above-mentioned
The preparation method of chitosan-based compound emergency material be prepared.
The present invention also provides a kind of application of chitosan-based compound emergency material in water body purification or reparation, the applications
For the application using the chitosan-based compound emergency material in water body Adsorption heavy metal.
Further, the chitosan-based compound emergency material is fixed on water body ring in the form of adsorbing sphere or adsorption column
In border.
Compared with prior art, beneficial effects of the present invention include following three aspect: first, shell provided by the invention
The preparation method of the compound emergency material of glycan base, preparation process is simple, is not required to that energy consumption can be greatly reduced using complicated technique
And human cost, cost is relatively low, meanwhile, cotton fiber used in preparation method is cheap and easy to get, biodegradable environment friend
Good profile material；Second, chitosan-based compound emergency material provided by the invention, property is stablized, and has preferable adsorptivity ability,
It is recycled convenient for separation from water body, secondary pollution can be avoided；Third, the present invention provides a kind of compound to be answered chitosan-based
Application of the anxious material in water pollution control and reparation, chitosan-based compound emergency material are consolidated in the form of adsorption column and adsorbing sphere
It is scheduled in water body environment, while the material after use can effectively avoid secondary pollution convenient for recycling.
It is described further below with reference to technical effect of the attached drawing to design of the invention, specific structure and generation, with
It is fully understood from the purpose of the present invention, feature and effect.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of the original cotton fiber of a preferred embodiment of the invention；
Fig. 2 is the stereoscan photograph of the chitosan-based compound emergency material of a preferred embodiment of the invention.
Specific embodiment
Multiple preferred embodiments of the invention are introduced below with reference to Figure of description, keep its technology contents more clear and just
In understanding.The present invention can be emerged from by many various forms of embodiments, and protection scope of the present invention not only limits
The embodiment that Yu Wenzhong is mentioned.
Embodiment one:
The present embodiment illustrates a kind of preparation method of chitosan-based compound emergency material, includes the following steps:
A certain amount of cotton fiber is placed in sodium periodate solution by step 1, and 2h is shaken under the conditions of being protected from light, and is taken out, is produced
Object A；
Product A is dipped in certain density ethylene glycol solution by step 2, is shaken certain time, is obtained product B；
Step 3, by after product B ethanol washing, be dipped in certain density tetraethylenepentamine solution, concussion one timing
Between, obtain product C；
Step 4, by after product C ethanol washing, be placed in glutaraldehyde solution, shake certain time, obtain product D；
Product D is placed in certain density chitosan acetic acid solution by step 5, is shaken certain time, is obtained product E；
Step 6 carries out vacuum drying treatment to product E using vacuum desiccator, obtains chitosan-based compound emergency material.
Wherein, in step 1, the concentration of sodium periodate solution is 20~30mmol/L, between cotton fiber and sodium metaperiodate
Bath raio is 20:1, and the weight of cotton fiber is 2g, and the temperature for being protected from light condition is 40 DEG C.
In step 2, the volume fraction of ethylene glycol solution is 2~3%, and the concussion time is 20~30min, product A and second two
Bath raio between alcoholic solution is 30:1.
In step 3, the volume fraction of tetraethylenepentamine solution is 20%, volume 50mL, and the concussion time is 10~12h,
Environment temperature when concussion is 60 DEG C.
In step 4, the volume fraction of glutaraldehyde solution is 1~2%, and the concussion time is 30min, environment temperature when concussion
It is 30 DEG C.
In step 5, the concussion time is 10~30min, and environment temperature when concussion is 30 DEG C, the body of chitosan acetic acid solution
Fraction is 2%, the crosslinking time of concussion time namely chitosan and fiber in the step.
Embodiment two:
The present embodiment illustrates a kind of preparation method of chitosan-based compound emergency material, includes the following steps:
The cotton fiber of 2g is placed in 30mmol/L sodium periodate solution, the bath between cotton fiber and sodium metaperiodate by step 1
Than shaking 2h under the conditions of being protected from light, at a temperature of 40 DEG C for 20:1, takes out, obtain product A；
Product A is dipped in the ethylene glycol solution that concentration is 2%, the bath raio between product A and ethylene glycol solution by step 2
For 30:1,30min is shaken, product B is obtained；
Step 3, by after product B ethanol washing, it is molten to be dipped in the tetraethylenepentamine that volume fraction is 20%, volume is 50mL
In liquid, 12h is shaken at a temperature of 60 DEG C, obtains product C；
Step 4 after product C ethanol washing, will be placed in the glutaraldehyde solution that volume fraction is 1%, in 30 DEG C of temperature
Lower concussion 30min, obtains product D；
Product D is placed in the chitosan acetic acid solution that concentration is 2% by step 5, is shaken 30min at a temperature of 30 DEG C, is obtained
To product E；
Step 6 is dried product E using vacuum desiccator, obtains chitosan-based compound emergency material.
Wherein, the crosslinking time of the concussion time namely chitosan and fiber in step 5.
Fig. 1 is the stereoscan photograph of original cotton fiber used in the present embodiment, and Fig. 2 is to utilize the present embodiment preparation side
The stereoscan photograph of the finally obtained chitosan-based compound emergency material of method.From Fig. 1 and Fig. 2 as can be seen that compared to original
Beginning cotton fiber, the surface using the obtained chitosan-based compound emergency material of the present embodiment preparation method is more coarse, and thick
Rough surface is more conducive to adsorbing heavy metal in water.
Embodiment three:
The present embodiment illustrates a kind of preparation method of chitosan-based compound emergency material, includes the following steps:
The cotton fiber of 2g is placed in 20mmol/L sodium periodate solution, the bath between cotton fiber and sodium metaperiodate by step 1
Than shaking 2h under the conditions of being protected from light, at a temperature of 40 DEG C for 20:1, takes out, obtain product A；
Product A is dipped in the ethylene glycol solution that concentration is 2.5%, the bath between product A and ethylene glycol solution by step 2
Than obtaining product B for 30:1, concussion 20min；
Step 3, by after product B ethanol washing, it is molten to be dipped in the tetraethylenepentamine that volume fraction is 20%, volume is 50mL
In liquid, 10h is shaken at a temperature of 60 DEG C, obtains product C；
Step 4 after product C ethanol washing, will be placed in the glutaraldehyde solution that volume fraction is 1.5%, in 30 DEG C of temperature
Degree is lower to shake 30min, obtains product D；
Product D is placed in the chitosan acetic acid solution that concentration is 2% by step 5, is shaken 10min at a temperature of 30 DEG C, is obtained
To product E；
Step 6 is dried product E using vacuum desiccator, obtains chitosan-based compound emergency material.
Wherein, the crosslinking time of the concussion time namely chitosan and fiber in step 5.
Example IV:
The present embodiment illustrates a kind of preparation method of chitosan-based compound emergency material, includes the following steps:
The cotton fiber of 2g is placed in 25mmol/L sodium periodate solution, the bath between cotton fiber and sodium metaperiodate by step 1
Than shaking 2h under the conditions of being protected from light, at a temperature of 40 DEG C for 20:1, takes out, obtain product A；
Product A is dipped in the ethylene glycol solution that concentration is 3%, the bath raio between product A and ethylene glycol solution by step 2
For 30:1,25min is shaken, product B is obtained；
Step 3, by after product B ethanol washing, it is molten to be dipped in the tetraethylenepentamine that volume fraction is 20%, volume is 50mL
In liquid, 11h is shaken at a temperature of 60 DEG C, obtains product C；
Step 4 after product C ethanol washing, will be placed in the glutaraldehyde solution that volume fraction is 2%, in 30 DEG C of temperature
Lower concussion 30min, obtains product D；
Product D is placed in the chitosan acetic acid solution that concentration is 2% by step 5, is shaken 20min at a temperature of 30 DEG C, is obtained
To product E；
Step 6 is dried product E using vacuum desiccator, obtains chitosan-based compound emergency material.
Wherein, the crosslinking time of the concussion time namely chitosan and fiber in step 5.
Embodiment five:
The present embodiment illustrates a kind of chitosan-based compound emergency material that the preparation method by embodiment one obtains, this is answered
Anxious material is prepared by sodium periodate oxidation and two step of glutaraldehyde cross-linking.
Specifically using modified cheap cotton fiber as base material, by tetraethylenepentamine and chitosan material penta
It is integrated on cotton fiber under dialdehyde effect, the chitosan-based compound emergency material of acquisition.
Specifically being obtained using modified cheap cotton fiber as base material by sodium periodate solution oxidized cotton fiber
To aldehyde radical cotton, then tetraethylenepentamine and aldehyde radical cotton are acted on, then under glutaraldehyde effect by chitosan crosslinked on fiber,
The chitosan-based compound emergency material obtained.
Embodiment six:
The present embodiment illustrates a kind of chitosan-based compound emergency material of preparation method acquisition by embodiment one in water
Application in body purification or reparation.Chitosan-based compound emergency material is fixed on river etc. in the form of adsorbing sphere or adsorption column
In water body environment, the heavy metal in absorption polluted-water is carried out.
Specifically, the dirt containing copper nitrate is added according to the ratio that mass ratio is 2% in chitosan-based compound emergency material
In water, when the copper ion concentration in copper nitrate sewage is 5000 μ g/L, the removal rate of copper ion is more than 90%.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be within the scope of protection determined by the claims.
Claims (10)
1. a kind of preparation method of chitosan-based compound emergency material, which comprises the steps of:
Cotton fiber is placed in sodium periodate solution by step 1, under the conditions of being protected from light, carries out first time concussion, the first time concussion
Time be 2h, take out, obtain product A；
The product A is dipped in ethylene glycol solution by step 2, is carried out second and is shaken, obtains product B；
Step 3, by after the product B ethanol washing, be dipped in tetraethylenepentamine solution, carry out third time concussion, produced
Object C；
Step 4, by after the product C ethanol washing, be placed in glutaraldehyde solution, carry out the 4th time concussion, obtain product D；
The product D is placed in chitosan acetic acid solution by step 5, is carried out the 5th concussion, is obtained product E；
Step 6 carries out vacuum drying treatment to the product E using vacuum desiccator, obtains chitosan-based compound emergency material.
2. the preparation method of chitosan-based compound emergency material as described in claim 1, which is characterized in that in the step 1,
The concentration of the sodium periodate solution is 20~30mmol/L, and the bath raio between the cotton fiber and the sodium metaperiodate is 20:
1, the weight of the cotton fiber is 2g, and the temperature for being protected from light condition is 40 DEG C.
3. the preparation method of chitosan-based compound emergency material as described in claim 1, which is characterized in that in the step 2,
The volume fraction of the ethylene glycol solution is 2~3%, and the time of second concussion is 20~30min, the product A with
Bath raio between the ethylene glycol solution is 30:1.
4. the preparation method of chitosan-based compound emergency material as described in claim 1, which is characterized in that in the step 3,
The volume fraction of the tetraethylenepentamine solution is 20%, volume 50mL, and the time of the third time concussion is 10~12h,
The environment temperature when third time is shaken is 60 DEG C.
5. the preparation method of chitosan-based compound emergency material as described in claim 1, which is characterized in that in the step 4,
The volume fraction of the glutaraldehyde solution is 1~2%, and the time of the 4th concussion is 30min, when the 4th concussion
Environment temperature be 30 DEG C.
6. the preparation method of chitosan-based compound emergency material as described in claim 1, which is characterized in that in the step 5,
It is described 5th time concussion time be 10~30min, described 5th time concussion when environment temperature be 30 DEG C, the chitosan second
The volume fraction of acid solution is 2%.
7. such as the preparation method of chitosan-based compound emergency material described in any one of claims 1 to 6, which is characterized in that
Sodium periodate solution described in the step 1 is 30mmol/L, and the volume fraction of ethylene glycol solution described in the step 2 is
2%, the time of second of concussion is 30min, and the time shaken for the third time described in the step 3 is 12h, the step
The volume fraction of glutaraldehyde solution described in 4 is 1%, and the time of the 5th concussion described in the step 5 is 30min.
8. a kind of chitosan-based compound emergency material, which is characterized in that the chitosan-based compound emergency material is wanted by right
The preparation method of chitosan-based compound emergency material described in asking any one of 1 to 7 is prepared.
9. a kind of application of compound emergency material chitosan-based as described in claim 8 in water body purification or reparation,
It is characterized in that, the application is the application using the chitosan-based compound emergency material in water body Adsorption heavy metal.
10. application of the chitosan-based compound emergency material as claimed in claim 9 in water body purification or reparation, feature exist
In the chitosan-based compound emergency material is fixed in water body environment in the form of adsorbing sphere or adsorption column.
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