CN107262061A - A kind of heavy metal ion adsorbing material based on graphene and preparation method thereof - Google Patents
A kind of heavy metal ion adsorbing material based on graphene and preparation method thereof Download PDFInfo
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- CN107262061A CN107262061A CN201710540032.4A CN201710540032A CN107262061A CN 107262061 A CN107262061 A CN 107262061A CN 201710540032 A CN201710540032 A CN 201710540032A CN 107262061 A CN107262061 A CN 107262061A
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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
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention belongs to environment-friendly materials field, more particularly to a kind of heavy metal ion adsorbing material based on graphene and preparation method thereof；The heavy metal ion adsorbing material of the present invention mixes nitrogen-doped graphene, is crosslinked using polyvinyl alcohol, lignin sulfonic acid and carboxymethyl chitosan as raw material, is made using high polymer material as skeleton, and nitrogen-doped graphene is enhanced heavy metal ion adsorbing material；The heavy metal ion adsorbing material rate of adsorption is fast, and adsorbance is big, can rapid regeneration；The present invention is aided with after nitrogen-doped graphene, cross-linking reaction and activated using alkalinity potassium permanganate using polyvinyl alcohol, lignin sulfonic acid and carboxymethyl chitosan as primary raw material, and preparation process is simple, it is easy to operate, it is adaptable to industrialization production；The primary raw material that the present invention is used is cheap and easy to get, it is possible to decrease production cost；Advantages of nontoxic raw materials of the present invention is harmless, and poisonous and harmful substance will not be also produced in preparation process, and reaction condition is gentle, and energy consumption is low, environmental protection.
Description
Technical field
The invention belongs to environment-friendly materials field, more particularly to a kind of heavy metal ion adsorbing material based on graphene and its
Preparation method.
Background technology
In recent years, environmental pollution is of increasing concern, and the removing of heavy metal ions in sewage turns into hot research, mainly
Processing method includes absorption method, chemical precipitation method, ion-exchange, membrane separation process, bio-flocculation process etc., wherein, absorption method tool
Have simple to operate, the advantages of heavy metal treatment effect is preferable.
Absorption method is the avtive spot surface for making heavy metal ion stick to adsorbent by physics or chemical method, is entered
And the method for heavy-metal ion removal purpose is reached, conventional adsorbent includes two kinds of natural material and artificial material, natural material
Material includes activated carbon, mineral matter, agriculture and forestry organic waste material, silt etc., artificial material including nano material etc. in general, natural material
Material be easier to obtain, cost is relatively low, but adsorption effect is poor, artificial material prepare cost be higher than natural material, but adsorption effect compared with
It is good.
Chinese patent 201410104126.3 discloses a kind of N, N- bis- (phosphine methyl) disubstituted aminodithioformic acid official
The preparation method and its adsorption effect to heavy metal ion such as cadmium, copper, nickel, lead of the silica gel absorber of energy dough；But its cost
It is higher, and the rate of adsorption is slow；Chinese patent 201010161774.4 disclose it is a kind of go water removal in heavy metal adsorbent and its
Preparation method, this goes heavy metal absorbent in water removal to be made up of high polymer material, metal oxide and pore creating material, heavy metal
Adsorption capacity is big, and adsorption rate is fast；But there is the problem of regeneration is difficult in it.
The content of the invention
The present invention for above-mentioned technical problem in the prior art there is provided one kind is with low cost, the rate of adsorption is fast,
Adsorption capacity is big, the reproducible heavy metal ion adsorbing material based on graphene and preparation method thereof.
To solve the above problems, technical scheme is as follows：
A kind of heavy metal ion adsorbing material based on graphene, includes the raw material of following parts by weight：
Nitrogen-doped graphene：4-6 parts；
Lignin sulfonic acid：30-45 parts；
Polyvinyl alcohol：10-50 parts；
Carboxymethyl chitosan：20-35 parts；
Initiator：5-9 parts；
Crosslinking agent：12-19 parts.
Graphene be one kind by carbon atom with sp2The hexangle type of hybridized orbit composition is in the flat film of honeycomb lattice, tool
There are unique performances such as specific surface area is big, carrier mobility is high, excellent in mechanical performance；Adulterated in graphene lattice other
Hetero atom such as nitrogen, sulphur, boron etc., can produce chelation, so as to increase the adsorption rate of heavy metal ion with heavy metal ion；It is wooden
Plain sulfonic acid is the accessory substance of wood pulp papermaking, there is good diffusivity；Polyvinyl alcohol is that a kind of purposes is quite extensive water-soluble high
Molecularly Imprinted Polymer, strong adherence, epithelium pliability, flatness, oil resistivity, solvent resistance, protecting colloid with uniqueness,
Gas barrier performance, wearability and the specially treated water resistance having；Carboxymethyl chitosan is that a kind of water soluble chitosan spreads out
Biology, with a variety of functional groups such as amino, carboxyl, hydroxyl.
Preferably, described heavy metal ion adsorbing material, includes the raw material of following parts by weight：
Nitrogen-doped graphene：5 parts；
Lignin sulfonic acid：35 parts；
Polyvinyl alcohol：21 parts；
Carboxymethyl chitosan：28 parts；
Initiator：7 parts；
Crosslinking agent：15 parts.
Preferably, the initiator is any one in benzoyl peroxide and lauroyl peroxide, and the crosslinking agent is
Any one in ethyleneglycol dimethyacrylate and divinylbenzene.
One kind prepares heavy metal ion adsorbing material method, comprises the following steps：
The lignin sulfonic acid that poly-vinyl alcohol solution that S1, configuration quality fraction are 2%-7%, mass fraction are 4%-6%
Solution and the carboxymethyl chitosan solution that mass fraction is 2.5%-3.5%；The property of the control influence final product of solution concentration
Energy：Solution concentration is too high, and reaction system viscosity is excessive, the cross-linking reaction that is unfavorable in subsequent process and graphene it is scattered, and
Influence final product structure is so as to influence absorption property；
S2, by nitrogen-doped graphene and water according to 1:49-99 mass ratio mixing, ultrasonic disperse is added after 30-60 minutes
The poly-vinyl alcohol solution, is uniformly mixed；
S3, under condition of heating and stirring, the sulfomethylated lignin acid solution, carboxylic first are sequentially added into step 2 resulting solution
Base chitosan solution, is passed through inert gas deoxygenation, and stir；
S4, the initiator and crosslinking agent, heating stirring are added into step 3 resulting solution；
S5, by step 4 products therefrom carry out suction filtration, washing, 60-70 DEG C drying；
S6, by step 5 products therefrom be placed in alkaline permanganate solution soak a period of time after, suction filtration, washing, dry
To constant weight, heavy metal ion adsorbing material is made.
Preferably, step 1 poly-vinyl alcohol solution and sulfomethylated lignin acid solution are 90-100 DEG C, mixing speed in temperature
Configuration is obtained under the conditions of 80-90rpm；Solubility is preferable at high temperature for poly-vinyl alcohol solution and sulfomethylated lignin acid solution.
Preferably, the heating-up temperature of the step 3 is 75-85 DEG C, and mixing speed is 60-70rpm；Temperature and mixing speed
Influence is produced on final product performance.
Preferably, the step 3 is added after sulfomethylated lignin acid solution and carboxymethyl chitosan solution and stirred 2-3 hours；It is suitable
It is necessary to carry out mixing and deoxygenation when the long time.
Preferably, step 4 heating-up temperature is 85-95 DEG C, and mixing time is 4-6 hours, and mixing speed is 55-
65rpm。
Preferably, the collocation method of the alkalinity potassium permanganate of the step 6 is：The collocation method of alkalinity potassium permanganate is：
To 1L mass fractions to add 0.05-0.1mol sodium hydroxide in 5-10% liquor potassic permanganate, alkalinity potassium permanganate is used
In activation sorbing material, controlled concentration keeps appropriate oxidisability.
Preferably, the nitrogen-doped graphene is porous graphene nano-particle；Porous graphene nano-particle has more
Big reference area, further enhances the adsorbance and the rate of adsorption of heavy metal ion.
Relative to prior art, advantages of the present invention is as follows,
The present invention heavy metal ion adsorbing material using polyvinyl alcohol, lignin sulfonic acid and carboxymethyl chitosan as raw material,
Mix nitrogen-doped graphene, be crosslinked, be made using high polymer material as skeleton, nitrogen-doped graphene be enhanced heavy metal from
Sub- sorbing material；The crosslinking of polyvinyl alcohol, lignin sulfonic acid and carboxymethyl chitosan builds material stiffness skeleton, thus heavy metal
The ion adsorbing material rate of adsorption is fast；And there is the functional groups such as a large amount of amino, hydroxyl, carboxyl in skeleton surface, be different metal from
Son provides a large amount of binding sites, and adsorbance is big；Nitrogen-doped graphene is evenly distributed in rigid backbone as reinforcing material, a side
Face can strengthen sorbing material mechanical property, on the other hand, exist because nitrogen-doped graphene specific surface area is big with heteroatomic, greatly
The rate of adsorption and adsorbance of big enhancing heavy metal ion adsorbing material；The heavy metal ion adsorbing material of the present invention can also pass through
Alkalinity potassium permanganate carries out rapid regeneration；
The present invention is aided with nitrogen-doped graphene using polyvinyl alcohol, lignin sulfonic acid and carboxymethyl chitosan as primary raw material,
Activated after cross-linking reaction using alkalinity potassium permanganate, preparation process is simple, it is easy to operate, it is adaptable to industrialization production；The present invention
The primary raw material of use is cheap and easy to get, it is possible to decrease production cost；Advantages of nontoxic raw materials of the present invention is harmless, will not also be produced in preparation process
Poisonous and harmful substance, reaction condition is gentle, and energy consumption is low, environmental protection.
Embodiment
Embodiment 1：
A kind of preparation method of heavy metal ion adsorbing material, includes the raw material of following parts by weight：
Nitrogen-doped graphene：5 parts；
Lignin sulfonic acid：35 parts；
Polyvinyl alcohol：21 parts；
Carboxymethyl chitosan：28 parts；
Initiator：7 parts；
Crosslinking agent：15 parts.
Wherein, initiator is benzoyl peroxide, and crosslinking agent is ethyleneglycol dimethyacrylate.
Preparation process comprises the following steps：
S1, in the polyvinyl alcohol that temperature is 90-100 DEG C, configuration quality fraction is 4% under the conditions of mixing speed 80-90rpm
Solution, mass fraction are 5% sulfomethylated lignin acid solution；Configuration quality fraction is 3% carboxymethyl chitosan solution；
S2, selection nitrogen-doped graphene porous nano particle, by the nitrogen-doped graphene and water according to 1:99 quality
Than mixing, ultrasonic disperse adds the poly-vinyl alcohol solution, is uniformly mixed after 30-60 minutes；
S3, heating-up temperature be 75-85 DEG C, mixing speed be 60-70rpm under the conditions of, into step 2 resulting solution successively plus
Enter the sulfomethylated lignin acid solution, carboxymethyl chitosan solution, be passed through nitrogen deoxygenation, continue to stir 2-3 hours.；
S4, the initiator and crosslinking agent, heating stirring are added into step 3 resulting solution；Heating-up temperature is 85-95
DEG C, mixing time is 4-6 hours, and mixing speed is 55-65rpm；
S5, by step 4 products therefrom carry out suction filtration, washing, 60-70 DEG C drying；
S6, the sodium hydroxide configuration for adding into 1L 8% liquor potassic permanganate 0.08mol obtain 8% alkaline permanganic acid
Potassium solution；Step 5 products therefrom is immersed in the alkaline permanganate solution after immersion a period of time, suction filtration, washing, drying
To constant weight, heavy metal ion adsorbing material is made.
Embodiment 2：
Keep the other conditions of embodiment 1 constant, heavy metal ion adsorbing material is prepared according to the raw material proportioning of table one：
Table one, different ratios of raw materials prepare heavy metal ion adsorbing material
| Raw material | A groups | B groups | C groups | D groups | E groups | F groups | G groups | H groups |
| Nitrogen-doped graphene | 4 | 6 | 0 | 3 | 10 | 5 | 5 | 5 |
| Lignin sulfonic acid | 30 | 45 | 35 | 35 | 35 | 0 | 35 | 35 |
| Polyvinyl alcohol | 10 | 50 | 21 | 21 | 21 | 21 | 0 | 21 |
| Carboxymethyl chitosan | 20 | 35 | 28 | 28 | 28 | 28 | 28 | 0 |
| Initiator | 5 | 9 | 7 | 7 | 7 | 7 | 7 | 7 |
| Crosslinking agent | 12 | 19 | 15 | 15 | 15 | 15 | 15 | 15 |
Wherein, the initiator of A, B group is lauroyl peroxide, and crosslinking agent is divinylbenzene；
The initiator of C-H groups is benzoyl peroxide, and crosslinking agent is ethyleneglycol dimethyacrylate.
Embodiment 3：
Keep the other conditions of embodiment 1 constant, according to poly-vinyl alcohol solution, the sulfomethylated lignin of different quality containing in table two
Acid solution, carboxymethyl chitosan solution prepare heavy metal ion adsorbing material：
Table two, the raw material of different quality containing prepare heavy metal ion adsorbing material
| Raw material | A groups | B groups | C groups |
| Poly-vinyl alcohol solution | 2% | 7% | 8% |
| Sulfomethylated lignin acid solution | 6% | 4% | 10% |
| Carboxymethyl chitosan solution | 3.5% | 2.5% | 6% |
Embodiment 4：
Keep the other conditions of embodiment 1 constant, the alkalinity potassium permanganate of selection different quality point fraction：2% (A groups), 5%
(B groups), 10% (C groups), 15% (D groups)；Activate heavy metal ion adsorbing material.
The collocation method of alkalinity potassium permanganate is：It is addition in 2-15% liquor potassic permanganate to 1L mass fractions
0.02-0.15mol sodium hydroxide.
Embodiment 5：
Keep the other conditions of embodiment 1 constant, graphene of the selection undoped with nitrogen prepares heavy metal ion adsorbing material.
Embodiment 6：
Heavy metal ion adsorbing material made from testing example 1-5 is in 15min, the removal to 0.1mol/L copper ions
Rate：
The clearance of copper ion=(C0-C15min)/C0× 100%
It the results are shown in Table three：
Clearance of the heavy metal ion adsorbing material to copper ion made from the embodiment 1-5 of table three
| Group | Clearance % | Group | Clearance % |
| Embodiment 1 | 96.2 | Embodiment 3 (A groups) | 94.7 |
| Embodiment 2 (A groups) | 94.3 | Embodiment 3 (B groups) | 93.2 |
| Embodiment 2 (B groups) | 95.1 | Embodiment 3 (C groups) | 69.8 |
| Embodiment 2 (C groups) | 46.2 | Embodiment 4 (A groups) | 78.1 |
| Embodiment 2 (D groups) | 69.8 | Embodiment 4 (B groups) | 94.7 |
| Embodiment 2 (E groups) | 92.1 | Embodiment 4 (C groups) | 93.5 |
| Embodiment 2 (F groups) | 29.8 | Embodiment 4 (D groups) | 66.5 |
| Embodiment 2 (G groups) | 37.6 | Embodiment 5 | 83.2 |
| Embodiment 2 (H groups) | 62.9 |
It can be seen from above-described embodiment 1, the test experiments result of embodiment 2, following each component interaction, by handing over
The heavy metal ion adsorbing material performance that connection reaction is made is more excellent：
Nitrogen-doped graphene：4-6 parts；
Lignin sulfonic acid：30-45 parts；
Polyvinyl alcohol：10-50 parts；
Carboxymethyl chitosan：20-35 parts；
Initiator：5-9 parts；
Crosslinking agent：12-19 parts.
Wherein sorbing material effect is optimal made from embodiment 1；The absorption of the addition enhancing sorbing material of doped graphene
Performance, but absorption property is not directly proportional to raw material addition, and addition excessively increases cost on the contrary.
It can be seen from the test experiments result of embodiment 3, the performance of the influence final product of reactant solution concentration：Quality
The sulfomethylated lignin acid solution and mass fraction that poly-vinyl alcohol solution that fraction is 2%-7%, mass fraction are 4%-6% be
2.5%-3.5% carboxymethyl chitosan solution is optium concentration.
It can be seen from the test experiments result of embodiment 4, the concentration influence activation effect of alkalinity potassium permanganate, mass fraction
It is optium concentration for 5-10% liquor potassic permanganate.
It can be seen from the test experiments result of embodiment 5, inhaled undoped with heavy metal ion made from the grapheme material of nitrogen
Enclosure material adsorption capacity is relatively weak.
Embodiment 7：
Heavy metal ion adsorbing material made from testing example 1 is in 15min, heavy metal ion different to 0.1mol/L
Clearance：
The clearance of heavy metal ion=(C0-C15min)/C0× 100%
It the results are shown in Table four：
The clearance of table four, heavy metal ion adsorbing material to different heavy metal ion
| Heavy metal ion | Clearance % |
| Copper ion | 96.2 |
| Lead ion | 95.1 |
| Cadmium ion | 96.5 |
| Nickel ion | 94.9 |
| Cobalt ions | 93.6 |
Embodiment 8：
By heavy metal ion adsorbing material made from embodiment 1 carry out it is heavy metal ion adsorbed after, the alkalescence for being placed in 4% is high
It is stirred continuously, soaks 4-6 hours, suction filtration in potassium manganate solution, is washed with deionized to neutrality, drying to constant weight can be sharp again
With, be reused for test 15min in, to the clearance of 0.1mol/L copper ions, clearance is up to 95.1%.
It should be noted that above-described embodiment is only presently preferred embodiments of the present invention, not for limiting the present invention's
Protection domain, the equivalent substitution or replacement made on the basis of the above belongs to protection scope of the present invention.
Claims (10)
1. a kind of heavy metal ion adsorbing material based on graphene, it is characterised in that include the raw material of following parts by weight：
Nitrogen-doped graphene：5-9 parts；
Lignin sulfonic acid：30-45 parts；
Polyvinyl alcohol：10-50 parts；
Carboxymethyl chitosan：20-35 parts；
Initiator：5-9 parts；
Crosslinking agent：12-19 parts.
2. heavy metal ion adsorbing material as claimed in claim 1, it is characterised in that include the raw material of following parts by weight：
Nitrogen-doped graphene：7 parts；
Lignin sulfonic acid：35 parts；
Polyvinyl alcohol：21 parts；
Carboxymethyl chitosan：28 parts；
Initiator：7 parts；
Crosslinking agent：15 parts.
3. heavy metal ion adsorbing material as claimed in claim 2, it is characterised in that the initiator is benzoyl peroxide
With any one in lauroyl peroxide, the crosslinking agent is any one in ethyleneglycol dimethyacrylate and divinylbenzene
Kind.
4. one kind prepares the heavy metal ion adsorbing material method as described in claim 1-3 any one, it is characterised in that including
Following steps：
The sulfomethylated lignin acid solution that poly-vinyl alcohol solution that S1, configuration quality fraction are 2%-7%, mass fraction are 4%-6%
With the carboxymethyl chitosan solution that mass fraction is 2.5%-3.5%；
S2, by nitrogen-doped graphene and water according to 1:49-99 mass ratio mixing, ultrasonic disperse is added described after 30-60 minutes
Poly-vinyl alcohol solution, is uniformly mixed；
S3, under condition of heating and stirring, the sulfomethylated lignin acid solution, carboxymethyl shell are sequentially added into step 2 resulting solution
Glycan solution, is passed through inert gas deoxygenation, and stir；
S4, the initiator and crosslinking agent, heating stirring are added into step 3 resulting solution；
S5, by step 4 products therefrom carry out suction filtration, washing, 60-70 DEG C drying；
S6, step 5 products therefrom is placed in alkaline permanganate solution and soaked after a period of time, suction filtration, washing are dried to perseverance
Weight, is made heavy metal ion adsorbing material.
5. preparation method as claimed in claim 4, it is characterised in that step 1 poly-vinyl alcohol solution and lignin sulfonic acid
Solution is 90-100 DEG C, configures under the conditions of mixing speed 80-90rpm and obtain in temperature.
6. preparation method as claimed in claim 4, it is characterised in that the heating-up temperature of the step 3 is 75-85 DEG C, stirring
Speed is 60-70rpm.
7. preparation method as claimed in claim 4, it is characterised in that the step 3 adds sulfomethylated lignin acid solution and carboxylic first
Stirred 2-3 hours after base chitosan solution.
8. preparation method as claimed in claim 4, it is characterised in that step 4 heating-up temperature is 85-95 DEG C, during stirring
Between be 4-6 hours, mixing speed is 55-65rpm.
9. preparation method as claimed in claim 4, it is characterised in that the collocation method of the alkalinity potassium permanganate of the step 6
For：To sodium hydroxide of the 1L mass fractions for addition 0.05-0.1mol in 5-10% liquor potassic permanganate.
10. preparation method as claimed in claim 4, it is characterised in that the nitrogen-doped graphene is porous graphene nanometer
Particle.
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