CN110368916A - One heavy metal species composite adsorbing material and the preparation method and application thereof - Google Patents
One heavy metal species composite adsorbing material and the preparation method and application thereof Download PDFInfo
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- CN110368916A CN110368916A CN201910811216.9A CN201910811216A CN110368916A CN 110368916 A CN110368916 A CN 110368916A CN 201910811216 A CN201910811216 A CN 201910811216A CN 110368916 A CN110368916 A CN 110368916A
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- heavy metal
- cyclodextrin
- beta
- artificial zeolite
- acrylic acid
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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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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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
- B01J20/28047—Gels
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3028—Granulating, agglomerating or aggregating
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a kind of novel heavy metal composite adsorbing materials and preparation method thereof, the heavy metal composite adsorbing material is using beta-cyclodextrin and acrylic monomers as raw material, artificial zeolite is as filler, N, N'- methylene-bisacrylamide is crosslinking agent, and potassium peroxydisulfate is beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel made from initiator.The composite hydrogel can effectively adsorb the heavy metal ion such as uranium, and to achieve the purpose that rationally to administer sewage, and its synthesis technology is simple, low raw-material cost, adsorption operations step is simple, has wide application prospect, can satisfy the demand of the sewage treatment of rapid development.
Description
Technical field
The present invention relates to biological chemical fields, and in particular to a kind of beta-cyclodextrin/acrylic acid/artificial zeolite compound water congealing
The preparation of glue and its application in absorption heavy metal.
Background technique
In recent years, with the rapid development of industry, the use of heavy metal increases, but its unconfined discharge leads to environment
In metallics increase.Uranium is the main fuel of current most of commercial reactors, and largely the waste water containing radioactive uranium is arranged
It is put into environment, the mankind and environment can be caused to threaten for a long time, therefore, remove and recycle uranium from waste water and extremely compel as one
The problem of cutting.
Have the multiple technologies such as ion exchange, solvent extraction, reverse osmosis, film filtering and chemical precipitation method at present from aqueous solution
With uranium is removed in waste water.The wherein absorption method physico-chemical process important as one kind in heavy metal industrial effluent processing application,
It is widely used due to its is at low cost, effect is good, adsorption rate is fast, the advantages that can be recycled in adsorbent.
Composite gel material solves the defect of natural material itself, has key for Cheap highly effective absorption for realizing
Effect, provide feasible thinking and research direction to new material is prepared.In addition, a variety of group collective effects, inorganic material
The structure of material can be used as physical absorption binding site, greatly improve the adsorption capacity of material.Thus, by natural material and synthesis
High molecular material combines, and exploitation composite high-molecular gel rubber material has important research significance and market prospects.
Summary of the invention
The object of the present invention is to provide heavy metal species composite adsorbing material and preparation method thereof, the heavy-metal adsorption materials
The heavy metal ion such as the uranium that can be used in absorption effluent.
To achieve the above object, the present invention adopts the following technical scheme:
One heavy metal species composite adsorbing material is using beta-cyclodextrin and acrylic monomers as raw material, and artificial zeolite is as filling
Agent, N, N'- methylene-bisacrylamide are crosslinking agent, and potassium peroxydisulfate is initiator, the water-insoluble beta-cyclodextrin of rapid synthesis/
Acrylic acid/artificial zeolite composite hydrogel.
The preparation method of the heavy metal composite adsorbing material be beta-cyclodextrin is dissolved in 10mol/L sodium hydroxide it is molten
In liquid, and artificial zeolite stirring 1h is added, is added contains acrylic monomers and N, the mixing of N'- methylene-bisacrylamide later
Solution reacts 1h in 50 DEG C of water-bath after mixing evenly, adds potassium peroxydisulfate and stirs evenly, in 50-70 DEG C of water-bath
React 2-3h, product is freeze-dried to obtain the final product.
Each raw material percentage used are as follows: beta-cyclodextrin 14-18%, sodium hydroxide 10%, artificial zeolite 1-20%,
Acrylic monomers 60-70%, N, N'- methylene-bisacrylamide 1.5-3.0%, potassium peroxydisulfate 0.1-0.5%, each raw material weight hundred
The sum of score is 100%.
In polymerization reaction, C -- C single bond can be formed between acrylic monomers, and the hydroxyl of beta-cyclodextrin can be with the carboxyl of acrylic acid
Ester bond is formed, makes to contain a large amount of carboxyl and hydroxyl on gained heavy metal composite adsorbing material.Carboxyl and hydroxyl reactive group
In the presence of ion exchange or chelation can be passed through, heavy metal ion is effectively combined on active group, good adsorption is reached
The effect of heavy metal ion.
The preparation method of heavy metal composite adsorbing material of the present invention is simple, and strong operability, raw material is easy to buy, and price
Cheap, the hydrogel adsorption activity of formation is high, can quickly and effectively remove the heavy metal in sewage, therefore can satisfy rapidly
The demand of the sewage treatment of development.
Detailed description of the invention
Fig. 1 be different materials XRD crystal structure analysis figure, wherein a be beta-cyclodextrin/acrylic acid, b be beta-cyclodextrin/
Acrylic acid/artificial zeolite, c are artificial zeolite.
Fig. 2 is the thermogravimetric analysis figure of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is β-ring paste
Essence/acrylic acid/artificial zeolite-uranium compound.
Fig. 3 is the FTIR spectrum figure of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite-uranium compound, b
For beta-cyclodextrin/acrylic acid/artificial zeolite, c is beta-cyclodextrin/acrylic acid, and d is artificial zeolite.
Fig. 4 is the SEM shape appearance figure of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is β-ring paste
Essence/acrylic acid/artificial zeolite-uranium compound.
Fig. 5 is the EDX surface-element analysis chart of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is
Beta-cyclodextrin/acrylic acid/artificial zeolite-uranium compound.
Fig. 6 is influence situation map of the pH to absorption.
Fig. 7 is influence situation map of the different materials under different initial concentrations to absorption, wherein a is beta-cyclodextrin/propylene
Acid/artificial zeolite, b are beta-cyclodextrin/acrylic acid.
Fig. 8 is influence situation map of the temperature to absorption.
Specific embodiment
The present invention is to provide the preparation method of a heavy metal species composite adsorbing material, this method, which is mainly used for synthesis, to go
Except beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel of heavy metal ions in sewage, specific preparation step are as follows: will
1.5g beta-cyclodextrin is dissolved in the 10mol/L solution of the sodium hydroxide containing 1.0g, and 1.0g artificial zeolite stirring 1h is added, it
The mixed solution for containing 6.3g acrylic monomers and 0.18g N, N'- methylene-bisacrylamide is added afterwards, exists after mixing evenly
1h is reacted in 50 DEG C of water-bath, 0.02g potassium peroxydisulfate is added and stirs evenly, 2-3h is reacted in 50-70 DEG C of water-bath, is polymerize
After the reaction was completed, drying in freeze drier is placed on after hydrogel being shredded for 24 hours, to be then put in 50 DEG C of baking ovens and save.
Using Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), energy dispersion X-ray (EDX) and
X-ray diffraction (XRD) has carried out table to beta-cyclodextrin/acrylic acid/artificial zeolite composite material microstructure and chemical component
Sign.
Fig. 1 be different materials XRD crystal structure analysis figure, wherein a be beta-cyclodextrin/acrylic acid, b be beta-cyclodextrin/
Acrylic acid/artificial zeolite, c are artificial zeolite.Compare beta-cyclodextrin/acrylic acid and beta-cyclodextrin/acrylic acid/artificial zeolite figure
Shape, which can be seen that in beta-cyclodextrin/acrylic acid/artificial zeolite, there is the characteristic diffraction peak of artificial zeolite, this shows successfully to prepare
Hydrogel material is obtained.
Fig. 2 is the thermogravimetric analysis figure of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is β-ring paste
Essence/acrylic acid.It can be seen that the thermal stability of hydrogel adsorbent material significantly improves after artificial zeolite is added.
Fig. 3 is the FTIR spectrum figure of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite-uranium compound, b
For beta-cyclodextrin/acrylic acid/artificial zeolite, c is beta-cyclodextrin/acrylic acid, and d is artificial zeolite.It can be seen that β-ring paste
Essence/acrylic acid is in 1658 and 1254 cm-1The peak at place is C=O and the C-O-C slip key of ester group；After introducing artificial zeolite, gained β-
Cyclodextrin/acrylic acid/artificial zeolite is in 1030 cm-1There is new peak in place, this may be (Si, Al)-O of artificial zeolite not
Symmetrical stretching vibration；After adsorbing uranium ion, there is O=U=O group in beta-cyclodextrin/acrylic acid/artificial zeolite-uranium compound
Characteristic peak.
Fig. 4 is the SEM shape appearance figure of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is β-ring paste
Essence/acrylic acid/artificial zeolite-uranium compound.It is not advised it can be seen that beta-cyclodextrin/acrylic acid/artificial zeolite surface is presented
Shape then, and full of many holes；And after adsorbing uranium ion, surface becomes smooth, and coarse hole is filled out by flocculent substance
It is full.
Fig. 5 is the EDX surface-element analysis chart of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is
Beta-cyclodextrin/acrylic acid/artificial zeolite-uranium compound.It can be seen that being shown in beta-cyclodextrin/acrylic acid/artificial zeolite
The characteristic element (Si, Al and Mg) of artificial zeolite；After adsorption uranium, surface increases U element, this shows that uranium ion is adsorbed
On the surface of CAP hydrogel, it was demonstrated that CAP has good adsorption effect to uranium ion.
Several specific examples of the invention below, further describe the present invention, but the present invention is not limited only to this.
Embodiment 1
Beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel after taking 10mg dry is put into the uranyl of different pH, 500mg/L
Absorption research is carried out in solion.Using arsenazo Ⅲ as complexing agent, it is measured at 650nm wavelength with ultraviolet specrophotometer
Concentration.
,
Wherein, qeRepresent adsorption capacity, ceAnd c0Balance and initial concentration are respectively represented, m represents the quality of adsorbent material, and V is represented
The volume of adsorbent solution.
As shown in fig. 6, pH value increases to 3.5 from 2, beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel to uranyl from
The adsorption capacity of son gradually increases.When pH value increases to 4.5, the adsorbance of uranyl ion is kept approximately constant and reaches flat
Weighing apparatus, when pH value is greater than 4.5, the adsorbance of uranyl ion is reduced rapidly.Adsorbance is different under the conditions of different pH, maximum
Adsorbance is 730.26mg/g.
Embodiment 2
It is operated as described in Example 1, under the conditions of research pH is 4.0-4.5, temperature is 25 DEG C, different initial concentrations
Influence of the uranyl ion solution of 20mL to adsorption process.
As shown in fig. 7, when initial concentration is greater than 800mg/L, beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel
Maximum value can reach to uranyl ion adsorbance, be 797.37mg/g, and be higher than beta-cyclodextrin/acrylic acid, it was demonstrated that it can be effective
Remove the uranyl ion in solution.
Embodiment 3
Using the uranyl ion solution of 500mg/L, 1 method of embodiment is pressed under conditions of pH is 4.0-4.5 with different temperature
It is operated, studies influence of the temperature to adsorption process.
As shown in figure 8, as the temperature rises, adsorbent increases the adsorbance of uranyl ion, therefore adsorbent is to uranium
The adsorption process of acyl ion is heat absorption.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (4)
1. a heavy metal species composite adsorbing material, it is characterised in that: the heavy metal composite adsorbing material is with beta-cyclodextrin and third
Acrylic monomer is raw material, and artificial zeolite is crosslinking agent as filler, N, N'- methylene-bisacrylamide, and potassium peroxydisulfate is to draw
Send out agent, beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel of rapid synthesis.
2. a kind of preparation method of heavy metal composite adsorbing material as described in claim 1, it is characterised in that: beta-cyclodextrin is molten
Artificial zeolite stirring 1h is added in the sodium hydroxide solution of 10mol/L in solution, is added contains acrylic monomers and N later,
The mixed solution of N'- methylene-bisacrylamide reacts 1h in 50 DEG C of water-bath after mixing evenly, adds potassium peroxydisulfate and stirs
It mixes uniformly, 2-3h is reacted in 50-70 DEG C of water-bath, product is freeze-dried to obtain the final product.
3. the preparation method of heavy metal composite adsorbing material according to claim 2, it is characterised in that: each raw material used is by weight
Amount percentage is calculated as: beta-cyclodextrin 14-18%, sodium hydroxide 10%, artificial zeolite 1-20%, acrylic monomers 60-70%, N, N'-
Methylene-bisacrylamide 1.5-3.0%, potassium peroxydisulfate 0.1-0.5%, the sum of each raw material weight percentage are 100%.
4. the purposes that a kind of heavy metal composite adsorbing material as described in claim 1 is used as heavy metal ions in sewage adsorbent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112934189A (en) * | 2021-02-08 | 2021-06-11 | 华南理工大学 | Peanut shell lignocellulose/beta-cyclodextrin composite hydrogel adsorbent for heavy metal wastewater treatment, and preparation method and application thereof |
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