CN106237998A - A kind of al deposition chitosan non-woven fabrics adsorbent and preparation thereof and application - Google Patents

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

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Publication number
CN106237998A
CN106237998A CN201610606983.2A CN201610606983A CN106237998A CN 106237998 A CN106237998 A CN 106237998A CN 201610606983 A CN201610606983 A CN 201610606983A CN 106237998 A CN106237998 A CN 106237998A
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woven fabrics
adsorbent
deposition
chitosan non
chitosan
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CN106237998B (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
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Donghua University
National Dong Hwa 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 invention provides a kind of al deposition chitosan non-woven fabrics adsorbent and preparation thereof and application.Described al deposition chitosan non-woven fabrics adsorbent, it is characterised in that include chitosan non-woven fabrics, on described chitosan non-woven fabrics, deposition has aluminium salt.Its preparation method includes: with aluminum salt solution soak chitosan non-woven fabrics, be stirred at room temperature, take out, scrubbed, dry after obtain al deposition chitosan non-woven fabrics adsorbent.Al deposition chitosan non-woven fabrics adsorbing material preparation method of the present invention is simple, with low cost；Good for the removal effect of dyestuff contaminant in water, and alkali liquor can be used to be desorbed, regenerating easily reuse, is the dye waste water treatment method of a kind of green high-efficient.

Description

A kind of al deposition chitosan non-woven fabrics adsorbent and preparation thereof and application
Technical field
The present invention relates to a kind of al deposition chitosan non-woven fabrics adsorbent and preparation method thereof and to dye discoloration in water The application that thing is removed.
Background technology
Chitosan macromole is to there is most commonly used alkaline polysaccharide in nature, extensively derives from the shell-fish such as shrimp, Eriocheir sinensis Animal, is a class resourceful agricultural low value product.It is owing to comprising abundant active amino and hydroxyl in structure, it is possible to have Effect chelating heavy metal ion and adsorpting anion pollutant, the application in water processes has obtained studying widely.Chitosan is inhaled Attached dose is prepared to the variforms such as powder, microsphere, fiber and flaky material, and improves adsorptivity by chemical modification Energy.Wherein, chitosan metal complexes adsorbent is owing to having merged the outstanding electronic conduction ability of metal ion and polymer Good plasticity of fine quality and mechanical performance, have outstanding pollutant absorbability.But, this type of material is still limited by loaded down with trivial details Separation process, limits their actual application, it is desirable to have effect improves separating and recovering performance to meet FUTURE ENVIRONMENT and energy skill The needs of art.
Increasingly mature along with non-woven fabrics weaving technology, chitosan macromole non-woven fabrics has been successfully applied to the row such as medicine Industry, creates good commercial value.Nonwoven cloth material is similar to, because of it, the characteristic weaved cotton cloth, can easily divide in current water From and change easily, be highly suitable for water treatment procedure.
Summary of the invention
It is an object of the invention to combine the outstanding absorption property of chitosan metal complexes adsorbent and large area non-woven fabrics The excellent release energy of material, proposes a kind of al deposition chitosan non-woven fabrics adsorbing material possessing efficient absorption ability and system thereof Preparation Method and the application in absorbing dye pollutant.
In order to achieve the above object, the invention provides a kind of al deposition chitosan non-woven fabrics adsorbent, it is characterised in that Including chitosan non-woven fabrics, on described chitosan non-woven fabrics, deposition has aluminium salt.
Further, described chitosan forms coordination compound with aluminium salt.
Present invention also offers the preparation method of above-mentioned al deposition chitosan non-woven fabrics adsorbent, it is characterised in that bag Include: with aluminum salt solution soak chitosan non-woven fabrics, be stirred at room temperature, take out, scrubbed, dry after obtain al deposition chitosan nonwoven Cloth adsorbent.
Preferably, described aluminum salt solution be concentration be the aluminum nitrate solution of 0.3～1mmol/L.
Preferably, the described time being stirred at room temperature is 6～12h.
Preferably, the temperature of described drying is 40～80 DEG C.
Preferably, the pH of described solution is 3～5.
Present invention also offers above-mentioned al deposition chitosan non-woven fabrics adsorbent in the waste water containing dyestuff processes Application.
Further, the concrete steps of described application include: added by above-mentioned al deposition chitosan non-woven fabrics adsorbent Entering in the waste water containing dyestuff, room temperature is adsorbed a period of time, takes out, and obtains the waste water removing dyestuff and the aluminum having adsorbed dyestuff sinks Fructus Aurantii polysaccharide non-woven fabrics, washs the al deposition chitosan non-woven fabrics having adsorbed dyestuff, dries, and puts into stirring in desorbing agent de- Attached, activation, obtain the al deposition chitosan non-woven fabrics adsorbent of regeneration.
Further, described desorbing agent is the Na of NaOH, 0.05mol/L of 0.05mol/L2CO3Or 0.05mol/L NaHCO3Solution.
Due to chitosan monomer and metal ion (Al in chitosan non-woven fabrics metal complex3+) can carry out with certain proportion Coordination, therefore the concentration of aqueous metallic ions can not be the highest, and the most unnecessary metal ion of excessive concentration can not be combined with chitosan, Cause waste.The concentration of aqueous metallic ions can not be too low simultaneously, the lowest the carrying out being unfavorable for reaction of concentration so that big portion Divide chitosan that the using effect of chitosan non-woven fabrics metal complex adsorbent with metallic ion coordination, can not be affected.Al3+With shell The combination of polysaccharide adds the chitosan material adsorption site to anionic dye.Chitosan non-woven fabrics-aluminum complex structure Formed, ensured the high efficiency of additive capability of chitosan material, provide the effect of enrichment method for dyestuff degrading of material surface, Meanwhile, chitosan large area non-woven fabrics is easily recycled and changes.
The al deposition chitosan non-woven fabrics adsorbent that said method prepares during dyestuff contaminant, operates in removing water Simply, only need to be directly thrown in waste water from dyestuff by non-woven fabrics, under room temperature, stirring can complete the efficient absorption of dyestuff, absorption dye Al deposition chitosan non-woven fabrics adsorbent after material can use base extraction, destroys the interaction between adsorbent and dye molecule Power and be desorbed, it is achieved the recovery of dyestuff and the regeneration of al deposition chitosan non-woven fabrics adsorbent.Add al deposition shell to gather The amount of sugar 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 is:
(1) al deposition chitosan non-woven fabrics adsorbing material preparation method of the present invention is simple, with low cost；For in water The removal effect of dyestuff contaminant is good, and alkali liquor 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 adsorbing material of the present invention is prone to separate from water body and change, relatively powder Chitosan adsorbing material is more suitable for large-scale practical application.
(3) the al deposition chitosan non-woven fabrics adsorbent that the present invention prepares, it is adaptable to the waste water from dyestuff of multiple concentration, Process in waste water from dyestuff be can be used directly, easy to operate；
(4) the al deposition chitosan non-woven fabrics that the present invention prepares, stability is relatively strong, reusable, absorbing dye After alkali liquor can be used to carry out being desorbed after diluted acid activates, regenerating easily reuse.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope-energy spectrogram of al deposition chitosan non-woven fabrics adsorbent surface form prepared by the present invention；Should Adsorbent is made up of a lot of smooth surfaces and the fiber of uniform diameter, and meanwhile, aluminium ion is deposited on chitosan nonwoven uniformly 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 using 5 times, through 0.05mol/L NaHCO3Desorption, regeneration after 2.5mmol/L HCl activation, recycle efficiency relatively High, it is easy to regeneration, reuse is convenient.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited Scope.
Embodiment 1
A kind of al deposition chitosan non-woven fabrics adsorbent is including chitosan non-woven fabrics, heavy on described chitosan non-woven fabrics Long-pending have aluminium salt, and described chitosan forms coordination compound with aluminium salt.The preparation side of described al deposition chitosan non-woven fabrics adsorbent Method is: being immersed in 0.3mmol/L aluminum nitrate solution by 0.5g chitosan non-woven fabrics, described pH value of solution is 4.36, and room temperature is lasting Stirring 12h, take out, wash with water, 40 DEG C dry after obtain al deposition chitosan non-woven fabrics adsorbent, as shown in Figure 1.
Embodiment 2
A kind of al deposition chitosan non-woven fabrics adsorbent is including chitosan non-woven fabrics, heavy on described chitosan non-woven fabrics Long-pending have aluminium salt, and described chitosan forms coordination compound with aluminium salt.The preparation side of described al deposition chitosan non-woven fabrics adsorbent Method is: being immersed in 0.5mmol/L aluminum nitrate solution by 0.5g chitosan non-woven fabrics, described pH value of solution is 4.21, and room temperature is lasting Stirring 12h, take out, wash with water, 40 DEG C dry after obtain al deposition chitosan non-woven fabrics adsorbent.
Embodiment 3
A kind of al deposition chitosan non-woven fabrics adsorbent is including chitosan non-woven fabrics, heavy on described chitosan non-woven fabrics Long-pending have aluminium salt, and described chitosan forms coordination compound with aluminium salt.The preparation side of described al deposition chitosan non-woven fabrics adsorbent Method is: being immersed in 0.8mmol/L aluminum nitrate solution by 0.5g chitosan non-woven fabrics, described pH value of solution is 4.10, and room temperature is lasting Stirring 12h, take out, wash with water, 40 DEG C dry after obtain al deposition chitosan non-woven fabrics adsorbent.
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, the continuously stirred 12h of room temperature, takes out, Scrubbed, dry after obtain al deposition chitosan non-woven fabrics adsorbent.
Comparative example 3
0.5g chitosan non-woven fabrics is immersed in 0.5mmol/L aluminum nitrate solution, the continuously stirred 6h of room temperature, takes out, warp Al deposition chitosan non-woven fabrics adsorbent is obtained after washing, drying.
Test one: take respectively and added by embodiment 1～3 and the modification of chitosan nonwoven cloth material 0.5g of comparative example 1～3 preparation Enter in Xylene Red 73 dye solution that 200mL concentration is 100mg/L, be stirred at room temperature 90 minutes, take supernatant, use ultraviolet-can See that spectrophotometer measures dyestuff residual concentration in dyestuff maximum absorption wave strong point.Dyestuff goes division result as shown in table 1.
Table 1
As shown in Table 1, efficiently removing of dyestuff is played a very important role, at aluminum by chitosan with aluminum ions combination Solution concentration is that Xylene Red 73 dyestuff is had by the al deposition chitosan non-woven fabrics adsorbent preparing gained when 0.3～1mmol/L Good removal effect, clearance is more than 90%.When aluminium ion solution solubility is less than 0.05mmol/L, the shell prepared gathers The absorbability of dyestuff is declined substantially by sugar non-woven fabrics adsorbent.
Test two: take the sorbent material 0.5g prepared by embodiment 2 and comparative example 1 respectively and add 200mL concentration respectively For in Xylene Red 73 dye solution of 20mg/L, 50mg/L, 150mg/L, 200mg/L, it is stirred at room temperature 90 minutes, takes supernatant, Ultraviolet-visible spectrophotometer is used to measure dyestuff residual concentration in dyestuff maximum absorption wave strong point.Dyestuff removes division result such as table 2 Shown in.
Table 2
Chitosan-aluminum adsorbent Dyestuff initial concentration (mg/L) Dyestuff clearance (%)
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, in the aluminum solutions that concentration is 0.3～1mmol/L, prepare the al deposition chitosan non-woven fabrics of gained Material is relatively wide to the subject range of dye strength, all can reach the removal efficiency of more than 80% between 20～200mg/L.
Test three: take the sorbent material 0.5g prepared by embodiment 2 and comparative example 1 respectively and add 200mL concentration respectively For, in Xylene Red 73 dye solution of 100mg/L, being stirred at room temperature 90 minutes.By the above process adsorbent is reused 5 times, take Supernatant measures dyestuff residual concentration.Dyestuff goes division result as shown in table 3.
Table 3
As shown in Table 3, effect removed by the dyestuff still keeping good after al deposition chitosan nonwoven cloth material reuses 5 times Really；On the contrary, the chitosan nonwoven cloth material not containing aluminum is relatively low to the removal efficiency of dyestuff.
Test four: by preparation method same in embodiment 2, prepare al deposition chitosan nonwoven cloth material.Take system respectively It is the different types of dye solution of 100mg/L that the adsorbent 0.5g obtained adds 200mL concentration, is stirred at room temperature 90 minutes, takes supernatant Liquid measures dyestuff residual concentration.Dyestuff goes division result as shown in table 4.
Table 4
Sequence number Dyestuff Dyestuff clearance (%)
Application examples 1 Reactive black 5 99.0
Application examples 2 Active blue 19 99.9
Application examples 3 The most yellow 12 98.4
Application examples 4 The most yellow 18 94.1
Application examples 5 Acid blue 113 96.3
Embodiment 4
The application in the waste water containing dyestuff processes of the al deposition chitosan non-woven fabrics adsorbent, concretely comprises the following steps:
The 0.5g al deposition chitosan non-woven fabrics adsorbent will prepared according to method in embodiment 2, adds to 200mL concentration For in Xylene Red 73 dye solution of 200mg/L, room temperature is adsorbed 90 minutes, takes out, and obtains removing the waste water of dyestuff and absorption The al deposition chitosan non-woven fabrics of dyestuff, washes with water the al deposition chitosan non-woven fabrics having adsorbed dyestuff, 40 DEG C of drying, Put into the NaHCO of 200mL 0.05mol/L3In aqueous solution, stirring 2h is with the acid of desorption al deposition chitosan non-woven fabrics absorption Property red 73, then use the HCl of 2.5mmol/L to activate, obtain regeneration al deposition chitosan non-woven fabrics adsorbent, such as Fig. 2 institute Show, reuse.
Embodiment 5
The application in the waste water containing dyestuff processes of the al deposition chitosan non-woven fabrics adsorbent, concretely comprises the following steps:
The 0.5g al deposition chitosan non-woven fabrics adsorbent will prepared according to method in embodiment 2, adds to 200mL concentration For in Xylene Red 73 dye solution of 200mg/L, room temperature is adsorbed 90 minutes, takes out, and obtains removing the waste water of dyestuff and absorption The al deposition chitosan non-woven fabrics of dyestuff, washes with water the al deposition chitosan non-woven fabrics having adsorbed dyestuff, 40 DEG C of drying, Putting in the NaOH aqueous solution of 200mL 0.05mol/L, stirring 2h is with the acidity of desorption al deposition chitosan non-woven fabrics absorption Red 73, then use the HCl of 2.5mmol/L to activate, obtain the al deposition chitosan non-woven fabrics adsorbent of regeneration, reuse.
Embodiment 6
The application in the waste water containing dyestuff processes of the al deposition chitosan non-woven fabrics adsorbent, concretely comprises the following steps:
The 0.5g al deposition chitosan non-woven fabrics adsorbent will prepared according to method in embodiment 2, adds to 200mL concentration For in Xylene Red 73 dye solution of 200mg/L, room temperature is adsorbed 90 minutes, takes out, and obtains removing the waste water of dyestuff and absorption The al deposition chitosan non-woven fabrics of dyestuff, washes with water the al deposition chitosan non-woven fabrics having adsorbed dyestuff, 40 DEG C of drying, Put into the Na of 200mL 0.05mol/L2CO3In aqueous solution, stirring 2h is with the acidity of desorption al deposition chitosan non-woven fabrics absorption Red 73, then use the HCl of 2.5mmol/L to activate, obtain the al deposition chitosan non-woven fabrics adsorbent of regeneration, reuse.
Comparative example 4
The application in the waste water containing dyestuff processes of the al deposition chitosan non-woven fabrics adsorbent, concretely comprises the following steps:
The 0.5g al deposition chitosan non-woven fabrics adsorbent will prepared according to method in embodiment 2, adds to 200mL concentration For in Xylene Red 73 dye solution of 200mg/L, room temperature is adsorbed 90 minutes, takes out, and obtains removing the waste water of dyestuff and absorption The al deposition chitosan non-woven fabrics of dyestuff, washes with water the al deposition chitosan non-woven fabrics having adsorbed dyestuff, 40 DEG C of drying, Putting in the NaAc aqueous solution of 200mL 0.05mol/L, stirring, stirring 2h is with desorption al deposition chitosan non-woven fabrics absorption Xylene Red 73, then uses the HCl of 2.5mmol/L to activate, and obtains the al deposition chitosan non-woven fabrics adsorbent of regeneration, reuse.
Test five: the desorption liquid that Example 4～6, comparative example 4 are selected respectively is to having adsorbed Xylene Red 73 dyestuff accordingly Adsorbent be desorbed, then use 2.5mmol/L HCl activation after regeneration.Desorption result is as shown in table 5.
Table 5
As shown in Table 5, the chitosan absorbent after absorption is through NaHCO3、NaOH、Na2CO3The desorption of aqueous solution, then make By the HCl activation processing of 2.5mmol/L, so that it may reach well to be desorbed and activation effect, be conducive to recycling.

Claims (9)

1. an al deposition chitosan non-woven fabrics adsorbent, it is characterised in that include chitosan non-woven fabrics, described chitosan without Spin deposition on cloth and have aluminium salt.
2. al deposition chitosan non-woven fabrics adsorbent as claimed in claim 1, it is characterised in that described chitosan and aluminium salt Form coordination compound.
3. the preparation method of the al deposition chitosan non-woven fabrics adsorbent described in claim 1 or 2, it is characterised in that including: use Aluminum salt solution soak chitosan non-woven fabrics, be stirred at room temperature, take out, scrubbed, dry after obtain al deposition chitosan non-woven fabrics inhale Attached dose.
4. the preparation method of al deposition chitosan non-woven fabrics adsorbent as claimed in claim 3, it is characterised in that described aluminum Saline solution be concentration be the aluminum nitrate solution of 0.3～1mmol/L.
5. the preparation method of al deposition chitosan non-woven fabrics adsorbent as claimed in claim 3, it is characterised in that described room The time of temperature stirring is 6～12h.
6. the preparation method of al deposition chitosan non-woven fabrics adsorbent as claimed in claim 3, it is characterised in that described baking Dry temperature is 40～80 DEG C.
7. the application in the waste water containing dyestuff processes of the al deposition chitosan non-woven fabrics adsorbent described in claim 1 or 2.
8. the al deposition chitosan non-woven fabrics adsorbent as claimed in claim 7 application in the waste water containing dyestuff processes, It is characterized in that, concrete steps include: added by above-mentioned al deposition chitosan non-woven fabrics adsorbent in the waste water containing dyestuff, Room temperature is adsorbed a period of time, takes out, and obtains removing the waste water of dyestuff and having adsorbed the al deposition chitosan non-woven fabrics of dyestuff, will inhale The al deposition chitosan non-woven fabrics washing of attached dyestuff, dries, and puts into stirring desorption in desorbing agent, activation, obtains the aluminum of regeneration Deposition shell polysaccharide non-woven fabrics adsorbent.
9. the al deposition chitosan non-woven fabrics adsorbent as claimed in claim 8 application in the waste water containing dyestuff processes, It is characterized in that, described 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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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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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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