CN106237998B - A kind of al deposition chitosan non-woven fabrics adsorbent and its preparation and application - Google Patents

A kind of al deposition chitosan non-woven fabrics adsorbent and its preparation and application Download PDF

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CN106237998B
CN106237998B CN201610606983.2A CN201610606983A CN106237998B CN 106237998 B CN106237998 B CN 106237998B CN 201610606983 A CN201610606983 A CN 201610606983A CN 106237998 B CN106237998 B CN 106237998B
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woven fabrics
adsorbent
chitosan non
deposition
dyestuff
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CN106237998A (en
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沈忱思
李素
陈彦红
柳建设
张奇
郜艳
沈晓凤
齐晓宝
张庆云
潘玉婷
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Donghua University
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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
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • 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
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/16—Regeneration of sorbents, filters

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The present invention provides a kind of al deposition chitosan non-woven fabrics adsorbent and its preparations and application.The al deposition chitosan non-woven fabrics adsorbent, which is characterized in that including chitosan non-woven fabrics, be deposited with aluminium salt on the chitosan non-woven fabrics.Preparation method includes: to impregnate chitosan non-woven fabrics with aluminum salt solution, is stirred at room temperature, and is taken out, and obtains al deposition chitosan non-woven fabrics adsorbent after washed, drying.Al deposition chitosan non-woven fabrics adsorbent material preparation method of the present invention is simple, low in cost；It is good for the removal effect of dyestuff contaminant in water, and lye can be used to be desorbed, regenerating easily reuse is a kind of dye waste water treatment method of green high-efficient.

Description

A kind of al deposition chitosan non-woven fabrics adsorbent and its preparation and application
Technical field
The present invention relates to a kind of al deposition chitosan non-woven fabrics adsorbent and preparation method thereof and its to dye discoloration in water The application of object removal.
Background technique
Chitosan macromolecular is that there are most commonly used alkaline polysaccharides in nature, extensively from shell-fish such as shrimp, crabs Animal is a kind of resourceful agriculture low value product.It is due to including active amino abundant and hydroxyl, Neng Gouyou in structure Effect chelating heavy metal ion and adsorpting anion pollutant, the application in water process have obtained extensive research.Chitosan is inhaled Attached dose is prepared to the variforms such as powder, microballoon, fiber and flaky material, and improves adsorptivity by chemical modification Energy.Wherein, chitosan metal complexes adsorbent is due to having merged metal ion outstanding electronic conduction ability and polymer Good plasticity and mechanical performance of fine quality have outstanding pollutant adsorption capacity.However, such material be still limited by it is cumbersome Separation process limits their practical application, needs to effectively improve separating and recovering performance to meet FUTURE ENVIRONMENT and energy skill The needs of art.
Increasingly mature with non-woven fabrics weaving technology, chitosan macromolecular non-woven fabrics has been successfully applied to the row such as medicine Industry produces good commercial value.Nonwoven cloth material is similar to the characteristic of woven fabric because of it, can easily divide in current water From and easily replace, be highly suitable for water treatment procedure.
Summary of the invention
The absorption property and large area non-woven fabrics that the purpose of the present invention is combine chitosan metal complexes adsorbent outstanding The excellent release energy of material proposes a kind of al deposition chitosan non-woven fabrics adsorbent material for having efficient absorption ability and its system Preparation Method and the application in absorption dyestuff contaminant.
In order to achieve the above object, the present invention provides a kind of al deposition chitosan non-woven fabrics adsorbents, which is characterized in that Including chitosan non-woven fabrics, aluminium salt is deposited on the chitosan non-woven fabrics.
Further, the chitosan and aluminium salt form complex.
The present invention also provides the preparation methods of above-mentioned al deposition chitosan non-woven fabrics adsorbent, which is characterized in that packet It includes: impregnating chitosan non-woven fabrics with aluminum salt solution, be stirred at room temperature, take out, obtain al deposition chitosan nonwoven after washed, drying Cloth adsorbent.
Preferably, the aluminum salt solution is the aluminum nitrate solution that concentration is 0.3~1mmol/L.
Preferably, the time being stirred at room temperature is 6~12h.
Preferably, the temperature of the drying is 40~80 DEG C.
Preferably, the pH of the solution is 3~5.
The present invention also provides above-mentioned al deposition chitosan non-woven fabrics adsorbents in the wastewater treatment containing dyestuff Using.
Further, the specific steps of the application include: to add above-mentioned al deposition chitosan non-woven fabrics adsorbent Enter in the waste water containing dyestuff, room temperature absorption a period of time, take out, obtains the waste water of removal dyestuff and the aluminium for having adsorbed dyestuff is heavy Product chitosan non-woven fabrics washs the al deposition chitosan non-woven fabrics for having adsorbed dyestuff, drying, and it is de- to put into stirring in desorbing agent Attached, activation obtains regenerated al deposition chitosan non-woven fabrics adsorbent.
Further, the desorbing agent is the Na of NaOH, 0.05mol/L of 0.05mol/L2CO3Or 0.05mol/L NaHCO3Solution.
Due to chitosan monomer in chitosan non-woven fabrics metal complex and metal ion (Al3+) can be carried out with certain proportion Coordination, therefore the concentration of aqueous metallic ions cannot be too high, excessive concentration then extra metal ion cannot in conjunction with chitosan, It causes to waste.The concentration of aqueous metallic ions can not be too low simultaneously, the too low progress for being unfavorable for reaction of concentration, so that big portion Divide chitosan that cannot influence the using effect of chitosan non-woven fabrics metal complex adsorbent with metallic ion coordination.Al3+With shell The combination of glycan increases chitosan material to the adsorption site of anionic dye.Chitosan non-woven fabrics-aluminum complex structure It is formed, has ensured the high efficiency of additive capability of chitosan material, provide the effect of enrichment method for the degradation of dyestuff on the surface of the material, Meanwhile chitosan large area non-woven fabrics is easily recycled and replaces.
The al deposition chitosan non-woven fabrics adsorbent that the above method is prepared when dyestuff contaminant, operates in going water removal Simply, non-woven fabrics need to be only directly thrown into waste water from dyestuff, the efficient absorption of dyestuff, absorption dye can be completed in stirring at room temperature Al deposition chitosan non-woven fabrics adsorbent after material can use base extraction, destroy the interaction between adsorbent and dye molecule Power and be desorbed, realize the recycling of dyestuff and the regeneration of al deposition chitosan non-woven fabrics adsorbent.It is poly- that al deposition shell is added The amount of sugared nonwoven cloth material can be adjusted according to dye strength in actual waste water.
Compared with prior art, the beneficial effects of the present invention are:
(1) al deposition chitosan non-woven fabrics adsorbent material preparation method of the present invention is simple, low in cost；For in water The removal effect of dyestuff contaminant is good, and lye can be used to be desorbed, and regenerating easily reuse is a kind of green high-efficient Dye waste water treatment method.
(2) al deposition chitosan non-woven fabrics adsorbent material of the present invention is easy to separate and replace from water body, compared with powder Chitosan adsorbent material is more suitable for large-scale practical application.
(3) the al deposition chitosan non-woven fabrics adsorbent that is prepared of the present invention, suitable for the waste water from dyestuff of a variety of concentration, The processing in waste water from dyestuff can be used directly, it is easy to operate；
(4) the al deposition chitosan non-woven fabrics that the present invention is prepared, stability is stronger, reusable, adsorbs dyestuff Lye can be used to be desorbed after diluted acid activates afterwards, regenerating easily reuse.
Detailed description of the invention
Fig. 1 is scanning electron microscope-energy spectrum diagram of al deposition chitosan non-woven fabrics adsorbent surface form prepared by the present invention；It should Adsorbent is smooth by many surfaces and the fiber of uniform diameter forms, meanwhile, aluminium ion is uniformly deposited on chitosan nonwoven On cloth.
Fig. 2 is reuse and the regeneration figure of al deposition chitosan non-woven fabrics adsorbent；Al deposition chitosan non-woven fabrics adsorbent After 5 times, through 0.05mol/L NaHCO3Desorption, 2.5mmol/L HCl activation after regeneration, be recycled efficiency compared with Height is easy to regenerate, and reuse is convenient.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Range.
Embodiment 1
A kind of al deposition chitosan non-woven fabrics adsorbent, including chitosan non-woven fabrics sink on the chitosan non-woven fabrics Product has aluminium salt, and the chitosan and aluminium salt form complex.The preparation side of the al deposition chitosan non-woven fabrics adsorbent Method are as follows: 0.5g chitosan non-woven fabrics is immersed in 0.3mmol/L aluminum nitrate solution, the pH value of solution is 4.36, and room temperature is lasting 12h is stirred, is taken out, is washed with water, obtains al deposition chitosan non-woven fabrics adsorbent after 40 DEG C of drying, as shown in Figure 1.
Embodiment 2
A kind of al deposition chitosan non-woven fabrics adsorbent, including chitosan non-woven fabrics sink on the chitosan non-woven fabrics Product has aluminium salt, and the chitosan and aluminium salt form complex.The preparation side of the al deposition chitosan non-woven fabrics adsorbent Method are as follows: 0.5g chitosan non-woven fabrics is immersed in 0.5mmol/L aluminum nitrate solution, the pH value of solution is 4.21, and room temperature is lasting 12h is stirred, is taken out, is washed with water, obtains al deposition chitosan non-woven fabrics adsorbent after 40 DEG C of drying.
Embodiment 3
A kind of al deposition chitosan non-woven fabrics adsorbent, including chitosan non-woven fabrics sink on the chitosan non-woven fabrics Product has aluminium salt, and the chitosan and aluminium salt form complex.The preparation side of the al deposition chitosan non-woven fabrics adsorbent Method are as follows: 0.5g chitosan non-woven fabrics is immersed in 0.8mmol/L aluminum nitrate solution, the pH value of solution is 4.10, and room temperature is lasting 12h is stirred, is taken out, is washed with water, obtains al deposition chitosan non-woven fabrics adsorbent after 40 DEG C of drying.
Comparative example 1
Taking 0.5g chitosan non-woven fabrics is sorbent material.
Comparative example 2
0.5g chitosan non-woven fabrics is immersed in 0.05mmol/L aluminum nitrate solution, room temperature persistently stirs 12h, it takes out, Al deposition chitosan non-woven fabrics adsorbent is obtained after washed, drying.
Comparative example 3
0.5g chitosan non-woven fabrics is immersed in 0.5mmol/L aluminum nitrate solution, room temperature persistently stirs 6h, takes out, warp Al deposition chitosan non-woven fabrics adsorbent is obtained after washing, drying.
Test one: it takes added by the modification of chitosan nonwoven cloth material 0.5g of Examples 1 to 3 and the preparation of comparative example 1~3 respectively Enter 200mL concentration be 100mg/L 73 dye solution of acid red in, be stirred at room temperature 90 minutes, take supernatant, using it is ultraviolet-can See that spectrophotometer measures dyestuff residual concentration in dyestuff maximum absorption wave strong point.The results are shown in Table 1 for dyestuff removal.
Table 1
As shown in Table 1, chitosan plays a very important role the efficient removal of dyestuff with aluminum ions combination, in aluminium Solution concentration, which prepares resulting al deposition chitosan non-woven fabrics adsorbent when being 0.3~1mmol/L, has 73 dyestuff of acid red Good removal effect, removal rate are greater than 90%.When aluminium ion solution solubility is lower than 0.05mmol/L, the shell prepared is poly- Sugared non-woven fabrics adsorbent declines the adsorption capacity of dyestuff obvious.
Test two: it takes respectively and 200mL concentration difference is added by sorbent material 0.5g prepared by embodiment 2 and comparative example 1 To be stirred at room temperature 90 minutes, taking supernatant in 73 dye solution of acid red of 20mg/L, 50mg/L, 150mg/L, 200mg/L, Dyestuff residual concentration is measured in dyestuff maximum absorption wave strong point using ultraviolet-visible spectrophotometer.Dyestuff removes division result such as table 2 It is shown.
Table 2
Chitosan-aluminium adsorbent Dyestuff initial concentration (mg/L) Dyestuff removal rate (%)
Embodiment 2 20 99.9
Embodiment 2 50 99.9
Embodiment 2 150 96.2
Embodiment 2 200 80
Comparative example 1 20 92.5
Comparative example 1 50 82.4
Comparative example 1 150 68.5
Comparative example 1 200 54.2
As shown in Table 2, resulting al deposition chitosan non-woven fabrics is prepared in the aluminum solutions that concentration is 0.3~1mmol/L Material is wider to the adaptation range of dye strength, can reach 80% or more removal efficiency between 20~200mg/L.
Test three: it takes respectively and 200mL concentration difference is added by sorbent material 0.5g prepared by embodiment 2 and comparative example 1 To be stirred at room temperature 90 minutes in 73 dye solution of acid red of 100mg/L.Adsorbent is reused 5 times by the above process, is taken Supernatant measures dyestuff residual concentration.The results are shown in Table 3 for dyestuff removal.
Table 3
As shown in Table 3, al deposition chitosan nonwoven cloth material still keeps good dyestuff removal effect after reusing 5 times Fruit；On the contrary, the chitosan nonwoven cloth material without containing aluminium is lower to the removal efficiency of dyestuff.
Test four: by same preparation method in embodiment 2, al deposition chitosan nonwoven cloth material is prepared.System is taken respectively It is the different types of dye solution of 100mg/L that 200mL concentration, which is added, in the adsorbent 0.5g obtained, is stirred at room temperature 90 minutes, takes supernatant Liquid measures dyestuff residual concentration.The results are shown in Table 4 for dyestuff removal.
Table 4
Serial number Dyestuff Dyestuff removal rate (%)
Application examples 1 Reactive black 5 99.0
Application examples 2 Active blue 19 99.9
Application examples 3 Directly Huang 12 98.4
Application examples 4 Directly Huang 18 94.1
Application examples 5 Acid blue 113 96.3
Embodiment 4
Application of the al deposition chitosan non-woven fabrics adsorbent in the wastewater treatment containing dyestuff, specific steps are as follows:
The 0.5g al deposition chitosan non-woven fabrics adsorbent that will be prepared according to method in embodiment 2 is added to 200mL concentration It in 73 dye solution of acid red of 200mg/L, room temperature is adsorbed 90 minutes, takes out, obtains waste water and the absorption of removal dyestuff The al deposition chitosan non-woven fabrics for having adsorbed dyestuff is washed with water the al deposition chitosan non-woven fabrics of dyestuff, dries at 40 DEG C, Put into the NaHCO of 200mL 0.05mol/L3In aqueous solution, 2h is stirred so that the acid of al deposition chitosan non-woven fabrics absorption is desorbed Property red 73, then using 2.5mmol/L HCl activate, regenerated al deposition chitosan non-woven fabrics adsorbent is obtained, such as Fig. 2 institute Show, reuse.
Embodiment 5
Application of the al deposition chitosan non-woven fabrics adsorbent in the wastewater treatment containing dyestuff, specific steps are as follows:
The 0.5g al deposition chitosan non-woven fabrics adsorbent that will be prepared according to method in embodiment 2 is added to 200mL concentration It in 73 dye solution of acid red of 200mg/L, room temperature is adsorbed 90 minutes, takes out, obtains waste water and the absorption of removal dyestuff The al deposition chitosan non-woven fabrics for having adsorbed dyestuff is washed with water the al deposition chitosan non-woven fabrics of dyestuff, dries at 40 DEG C, It puts into the NaOH aqueous solution of 200mL 0.05mol/L, stirs 2h so that the acidity of al deposition chitosan non-woven fabrics absorption is desorbed Red 73, it is then activated using the HCl of 2.5mmol/L, obtains regenerated al deposition chitosan non-woven fabrics adsorbent, reuse.
Embodiment 6
Application of the al deposition chitosan non-woven fabrics adsorbent in the wastewater treatment containing dyestuff, specific steps are as follows:
The 0.5g al deposition chitosan non-woven fabrics adsorbent that will be prepared according to method in embodiment 2 is added to 200mL concentration It in 73 dye solution of acid red of 200mg/L, room temperature is adsorbed 90 minutes, takes out, obtains waste water and the absorption of removal dyestuff The al deposition chitosan non-woven fabrics for having adsorbed dyestuff is washed with water the al deposition chitosan non-woven fabrics of dyestuff, dries at 40 DEG C, Put into the Na of 200mL 0.05mol/L2CO3In aqueous solution, 2h is stirred so that the acidity of al deposition chitosan non-woven fabrics absorption is desorbed Red 73, it is then activated using the HCl of 2.5mmol/L, obtains regenerated al deposition chitosan non-woven fabrics adsorbent, reuse.
Comparative example 4
Application of the al deposition chitosan non-woven fabrics adsorbent in the wastewater treatment containing dyestuff, specific steps are as follows:
The 0.5g al deposition chitosan non-woven fabrics adsorbent that will be prepared according to method in embodiment 2 is added to 200mL concentration It in 73 dye solution of acid red of 200mg/L, room temperature is adsorbed 90 minutes, takes out, obtains waste water and the absorption of removal dyestuff The al deposition chitosan non-woven fabrics for having adsorbed dyestuff is washed with water the al deposition chitosan non-woven fabrics of dyestuff, dries at 40 DEG C, It puts into the NaAc aqueous solution of 200mL 0.05mol/L, stirs, stir 2h so that the absorption of al deposition chitosan non-woven fabrics is desorbed Then acid red 73 is activated using the HCl of 2.5mmol/L, obtains regenerated al deposition chitosan non-woven fabrics adsorbent, reuse.
Test five: the desorption liquid that Example 4~6, comparative example 4 are selected respectively is to accordingly having adsorbed 73 dyestuff of acid red Adsorbent be desorbed, then using 2.5mmol/L HCl activation after regeneration.The results are shown in Table 5 for desorption.
Table 5
As shown in Table 5, the chitosan absorbent after absorption passes through NaHCO3、NaOH、Na2CO3The desorption of aqueous solution, then make It is activated with the HCl of 2.5mmol/L, so that it may reach desorption and activation effect well, be conducive to recycle.

Claims (7)

1. application of the al deposition chitosan non-woven fabrics adsorbent in the wastewater treatment containing dyestuff, the al deposition chitosan Non-woven fabrics adsorbent includes chitosan non-woven fabrics, is deposited with aluminium salt on the chitosan non-woven fabrics；The chitosan and aluminium Salt forms complex.
2. application of the al deposition chitosan non-woven fabrics adsorbent as described in claim 1 in the wastewater treatment containing dyestuff, It is characterized in that, the preparation method of the al deposition chitosan non-woven fabrics adsorbent includes: to impregnate chitosan with aluminum salt solution Non-woven fabrics is stirred at room temperature, and takes out, and obtains al deposition chitosan non-woven fabrics adsorbent after washed, drying.
3. application of the al deposition chitosan non-woven fabrics adsorbent as claimed in claim 2 in the wastewater treatment containing dyestuff, It is characterized in that, the aluminum salt solution is the aluminum nitrate solution that concentration is 0.3~1mmol/L.
4. application of the al deposition chitosan non-woven fabrics adsorbent as claimed in claim 2 in the wastewater treatment containing dyestuff, It is characterized in that, the time being stirred at room temperature is 6~12h.
5. application of the al deposition chitosan non-woven fabrics adsorbent as claimed in claim 2 in the wastewater treatment containing dyestuff, It is characterized in that, the temperature of the drying is 40~80 DEG C.
6. application of the al deposition chitosan non-woven fabrics adsorbent as described in claim 1 in the wastewater treatment containing dyestuff, It is characterized in that, specific steps include: that above-mentioned al deposition chitosan non-woven fabrics adsorbent is added in the waste water containing dyestuff, It room temperature absorption a period of time, takes out, obtain the waste water of removal dyestuff and has adsorbed the al deposition chitosan non-woven fabrics of dyestuff, will inhale The al deposition chitosan non-woven fabrics washing of attached dyestuff, drying put into and stir desorption in desorbing agent, and activation obtains regenerated aluminium Deposit chitosan non-woven fabrics adsorbent.
7. application of the al deposition chitosan non-woven fabrics adsorbent as claimed in claim 6 in the wastewater treatment containing dyestuff, It is characterized in that, the desorbing agent is the Na of NaOH, 0.05mol/L of 0.05mol/L2CO3Or the NaHCO of 0.05mol/L3 Solution.
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CN110485180A (en) * 2019-08-09 2019-11-22 山西大学 One kind is anti-to dye cloth and preparation method thereof
CN113731373A (en) * 2021-09-17 2021-12-03 东华大学 Chitosan non-woven fabric adsorbent with fluorescence indication function and application thereof

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Inventor before: Li Su

Inventor before: Chen Yanhong

Inventor before: Liu Jianshe

Inventor before: Zhang Qi

Inventor before: Gao Yan

Inventor before: Shen Xiaofeng

Inventor before: Qi Xiaobao

Inventor before: Zhang Qingyun

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