CN106179272A - A kind of novel porous nano carbon microsphere composite aquogel and preparation method thereof - Google Patents
A kind of novel porous nano carbon microsphere composite aquogel and preparation method thereof Download PDFInfo
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- 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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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0056—Preparation of gels containing inorganic material and water
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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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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- 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
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- 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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- 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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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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 present invention relates to a kind of novel porous nano carbon microsphere composite aquogel, composition is polysaccharide/anion polysaccharide poly-dopamine porous carbon nanosphere composite aquogel, the intervention of the most poly-dopamine porous carbon nanosphere improves the stability of hydrogel, and improves the absorbability of hydrogel；Its principle is the avtive spot that poly-dopamine provides the electrostatic interaction of a large amount of contacting metal ions and organic pollution, can form stable chelate with metal ion；The porous carbon nanosphere specific surface area of functionalization is relatively big, the offer spaces such as the hole on its surface is metal ion；And polysaccharide/anionic polysaccharides has the advantages that to combine closely with metal ion, it is not easy to fall off absorption behavior.Therefore the porous nano carbon ball composite aquogel of the present invention in ionic adsorption field, Industrial Waste Water Treatments field, biochemistry and pharmaceutical engineering field there is bigger application prospect.
Description
Technical field
The present invention relates to the preparation method of a kind of hydrogel, refer more particularly to a kind of novel porous nano carbon microsphere compound water congealing
Glue and preparation method thereof, belongs to environmental technology field.
Technical background
Porous nano carbon ball is three-dimensional carbon nano material, because of its porous surface, has than Two-dimensional Carbon nano material (graphite
Alkene, CNT etc.) surface area is less, catalysis is active, absorbability is higher.
Because of most natural polymer water absorption, water-retaining property preferably, natural macromolecule modification hydrogel obtains in every field
Extensive application.Wherein chitosan is one of them, and chitosan is that the chitin being widely present by nature is through deacetylated
Effect obtains, in medicine, food, chemical industry, cosmetics, water process, METAL EXTRACTION and recovery, biochemistry and biomedical engineering etc.
The applied research of numerous areas achieves major progress.Carboxymethyl chitosan be chitosan in the basic conditions with chloroacetate reaction
A kind of water-solubility chitosan derivative prepared, because the introducing of carboxyl, improves its dissolubility in water.Additionally, introduce
Carboxyl can be with the metallic ion coordination in solution, the metal ion in adsorbent solution, thus reach purify sewage purpose.
Hydrogel is because of the tridimensional network of its uniqueness, higher adsorbance, the preferable rate of adsorption, good renewable
Property causes the extensive concern of people in adsorption of metal ions field.The application of hydrogel and composite aquogel is more and more extensive.
China Patent No. 201210378225.1 discloses the tool sulfydryl magnetic hydrogel of a kind of Adsorption of Heavy Metal Ions
Preparation method, polyalcohol hydrogel is mixed irradiated polymerization by 2-(Acryloyloxy)ethanol, two kinds of monomers of Cys and distilled water
Obtain, and with this polyalcohol hydrogel for template carried magnetic nano ferrum in situ；This invention carried magnetic nano ferrum, method in situ
Simply, obtained tool sulfydryl magnetic hydrogel is applied to the absorption of heavy metal ion, can effective heavy-metal ion removal.
China Patent No. 201210332089.2 discloses a kind of metal ion print with interpenetrating polymer networks structure
Mark hydrogel adsorbing material and preparation method thereof, by acrylic monomer, acrylic crosslinking agent and radical initiator, and second
After alkene ethers cross-linking agent, cationic initiator, and dissolving metal salts mix homogeneously in a solvent, inject mould, through a step ultraviolet
Photoirradiation solidifies 5 minutes～1 hour, is extracted by resulting materials in hydrochloric acid solution, removes template ion, obtains metal ion print
Mark hydrogel adsorbing material.This invention has mechanical property, higher adsorption capacity and the stronger Selective adsorption of excellence.
Summary of the invention
For the adsorption of metal ions amount minor defect overcoming prior art to exist, the primary and foremost purpose of the present invention aims to provide one
Novel porous nano carbon microsphere composite aquogel.
The one novel porous nano carbon microsphere composite aquogel of the present invention, it is characterised in that composition is that polysaccharide/anion is many
Sugar-poly-dopamine-porous carbon nanosphere composite aquogel, the intervention of the most poly-dopamine-porous carbon nanosphere improves water-setting
The stability of glue, and improve the absorbability of hydrogel.The raising of absorbability is that poly-dopamine provides a large amount of contact
The avtive spot of the electrostatic interaction of metal ion and organic pollution, can form stable chelate with metal ion；Function
Change porous carbon nanosphere specific surface area relatively big, the offer spaces such as the hole on its surface is metal ion；Polysaccharide/anionic polysaccharides,
Such as carboxymethyl chitosan also can be combined closely with metal ion, it is not easy to De contamination behavior occurs.
The one novel porous nano carbon microsphere composite aquogel of the present invention, its preparation method is as follows:
A) preparation of active porous carbon nanometer micro ball: successively by 40～50 parts of dense strong acid, strong acid in 5～10 parts, 3～6 parts
Oxidant, 1～3 part of porous nano carbon ball add in enamel still, stir 12h, be cooled to room temperature at 40～60 DEG C, add 40～
50 portions of frozen water, then with 30～50nm osmosis membrane filters, obtain active porous nano carbon microsphere；
B) preparation of poly-dopamine modified lithium porous carbon nanosphere dispersion liquid: porous nano carbon ball is added to the water ultrasonic point
Dissipating, make the porous nano carbon ball dispersion liquid that concentration is 0.5～2.0mg/mL, it is 0.5～1.0mg/mL many for being subsequently adding concentration
Bar amine aqueous solution is mixed with and stirs, by alkali or buffer regulation system pH to about 8.0, under agitation and be heated to 50
～70 DEG C, react 6～8h, cooling obtains poly-dopamine modified lithium porous carbon nanosphere dispersion liquid；
C) preparation of composite aquogel: weigh 8～10 parts of polysaccharide or anionic polysaccharides, stir at 80～100 DEG C to
Being uniformly dissolved, add the dopamine modified porous Nano carbon balls dispersion liquid of 30～50 parts of steps b, ultrasonic disperse is uniform, with injection
Mixed liquor is added drop-wise to, among 3% calcium chloride-saturated boric acid aqueous solution, be cross-linked into the composite aquogel of a diameter of 1～5mm by device.
Described porous carbon nanosphere be chemical vapour deposition technique, solvent-thermal method, template, ultrasonic spray pyrolysis,
Porous carbon nanosphere prepared by supercritical methanol technology, impact compress method, arc discharge method, laser ablation method or plasma method is at least
A kind of.
Described dense strong acid is the combination of one or more in concentrated sulphuric acid, concentrated nitric acid, dense perchloric acid；Further, excellent
Elect the mixture of concentrated sulphuric acid and concentrated nitric acid as.
Described middle strong acid is in phosphoric acid, tartaric acid, sulfurous acid, acetone acid, oxalic acid, nitrous acid, Fluohydric acid., formic acid
Kind or several combinations；Further, preferably phosphoric acid.
Described oxidant is one or more in hydrogen peroxide, potassium dichromate, potassium permanganate, sodium hypochlorite, nitrate
Combination；Further, preferably potassium permanganate.
Described polysaccharide or anionic polysaccharides be starch, cellulose, glycogen, chitosan, agar, carboxymethyl cellulose,
The combination of one or more in carboxymethyl starch, carboxymethyl chitosan, sodium alginate；Further, preferably chitosan, carboxylic
One or both combination in methyl chitosan, sodium alginate.
Detailed description of the invention
Below in conjunction with embodiment, the application is described in further detail.It is understood that tool described herein
Body embodiment is used only for explaining related invention, rather than the restriction to this invention.
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can phases
Combination mutually.
Embodiment 1
A kind of novel porous nano carbon microsphere composite aquogel, its preparation method is as follows:
A) preparation of active porous carbon nanometer micro ball: successively by 45 parts of concentrated sulphuric acids and the mixture of concentrated nitric acid, 5 parts of phosphoric acid, 4
Part potassium permanganate, 2 parts of porous nano carbon balls add in enamel stills, stir 12h, are cooled to room temperature, add 44 at 50～60 DEG C
Part frozen water, then with 30～50nm osmosis membrane filters, obtains active porous nano carbon microsphere；
B) preparation of poly-dopamine modified lithium porous carbon nanosphere dispersion liquid: 5mg porous nano carbon ball is added in 500mL water
Ultrasonic disperse, makes the porous nano carbon ball dispersion liquid that concentration is 1.0mg/mL, and being subsequently adding 500mL concentration is that 1.0mg/mL is many
Bar amine aqueous solution is mixed with and stirs, by sodium bicarbonate buffer liquid regulation system pH to about 8.0, under agitation and heat
To 50～70 DEG C, reacting 6～8h, cooling obtains poly-dopamine modified lithium porous carbon nanosphere dispersion liquid；
C) preparation of composite aquogel: weigh 8 parts of carboxymethyl chitosans, 80～100 DEG C of stirrings down to being uniformly dissolved, adds
Entering the dopamine modified porous Nano carbon balls dispersion liquid of 40 parts of steps b, ultrasonic disperse is uniform, is added drop-wise to by mixed liquor with syringe
Among 3% calcium chloride-saturated boric acid aqueous solution, it is cross-linked into the composite aquogel of a diameter of 2.5～4mm.
Embodiment 2
A kind of novel porous nano carbon microsphere composite aquogel, its preparation method is as follows:
Step a, step b are with embodiment 1；
C) preparation of composite aquogel: weigh 10 parts of chitosans, 80～100 DEG C of stirrings down to being uniformly dissolved, adds 45
The dopamine modified porous Nano carbon balls dispersion liquid of part step b, ultrasonic disperse is uniform, with syringe, mixed liquor is added drop-wise to 3%
Among calcium chloride-saturated boric acid aqueous solution, it is cross-linked into the composite aquogel of a diameter of 2～4mm.
Embodiment 3
A kind of novel porous nano carbon microsphere composite aquogel, its preparation method is as follows:
A) preparation of active porous carbon nanometer micro ball: successively by 45 parts of concentrated sulphuric acids and the mixture of concentrated nitric acid, 6 parts of oxalic acid, 4
Part potassium dichromate, 2 parts of porous nano carbon balls add in enamel stills, stir 12h, are cooled to room temperature, add 43 at 50～60 DEG C
Part frozen water, then with 30～50nm osmosis membrane filters, obtains active porous nano carbon microsphere；
B) preparation of poly-dopamine modified lithium porous carbon nanosphere dispersion liquid: 7.5mg porous nano carbon ball is added 500mL water
Middle ultrasonic disperse, makes the porous nano carbon ball dispersion liquid that concentration is 1.5mg/mL, and being subsequently adding 500mL concentration is 1.5mg/mL
Dopamine solution is mixed with and stirs, by sodium bicarbonate buffer liquid regulation system pH to about 8.0, under agitation and add
Heat, to 50～70 DEG C, reacts 6～8h, and cooling obtains poly-dopamine modified lithium porous carbon nanosphere dispersion liquid；
C) preparation of composite aquogel: weigh 10 parts of chitosans and the mixture of sodium alginate, under stirring at 80～100 DEG C
To being uniformly dissolved, adding the dopamine modified porous Nano carbon balls dispersion liquid of 40 parts of steps b, ultrasonic disperse is uniform, uses syringe
It is added drop-wise to mixed liquor, among 3% calcium chloride-saturated boric acid aqueous solution, be cross-linked into the composite aquogel of a diameter of 3～5mm.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to the technology of the particular combination of above-mentioned technical characteristic
Scheme, also should contain in the case of without departing from described inventive concept simultaneously, above-mentioned technical characteristic or its equivalent feature carry out
Combination in any and other technical scheme of being formed.Such as features described above has similar merit with (but not limited to) disclosed herein
The technical scheme that the technical characteristic of energy is replaced mutually and formed.
Claims (10)
1. a novel porous nano carbon microsphere composite aquogel, it is characterised in that: described porous nano carbon ball composite aquogel,
Composition is polysaccharide/anion polysaccharide-poly-dopamine-porous carbon nanosphere composite aquogel；Its preparation method is as follows:
A) preparation of active porous carbon nanometer micro ball: successively by 40～50 parts of dense strong acid, strong acid, 3～6 parts of oxidations in 5～10 parts
Agent, 1～3 part of porous nano carbon ball add in enamel still, stir 12h, be cooled to room temperature, add 40～50 parts at 40～60 DEG C
Frozen water, then with 30～50nm osmosis membrane filters, obtains active porous nano carbon microsphere；
B) preparation of poly-dopamine modified lithium porous carbon nanosphere dispersion liquid: porous nano carbon ball is added to the water ultrasonic disperse, system
The porous nano carbon ball dispersion liquid becoming concentration to be 0.5～2.0mg/mL, being subsequently adding concentration is that 0.5～1.0mg/mL dopamine is molten
Liquid is mixed with and stirs, by alkali or buffer regulation system pH to about 8.0, under agitation and be heated to 50～70
DEG C, react 6～8h, cooling obtains poly-dopamine modified lithium porous carbon nanosphere dispersion liquid；
C) preparation of composite aquogel: weigh 8～10 parts of polysaccharide or anionic polysaccharides, at 80～100 DEG C, stirring is to dissolving
Uniformly, adding the dopamine modified porous Nano carbon balls dispersion liquid of 30～50 parts of steps b, ultrasonic disperse is uniform, will with syringe
Mixed liquor is added drop-wise to, among 3% calcium chloride-saturated boric acid aqueous solution, be cross-linked into the composite aquogel of a diameter of 1～5mm.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described porous carbon
Nanosphere be chemical vapour deposition technique, solvent-thermal method, template, ultrasonic spray pyrolysis, supercritical methanol technology, impact compress method,
At least one of porous carbon nanosphere prepared by arc discharge method, laser ablation method, plasma method.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described dense strong acid
For the combination of one or more in concentrated sulphuric acid, concentrated nitric acid, dense perchloric acid.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described dense strong acid
Mixture for concentrated sulphuric acid Yu concentrated nitric acid.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described middle strong acid
For the combination of one or more in phosphoric acid, tartaric acid, sulfurous acid, acetone acid, oxalic acid, nitrous acid, Fluohydric acid., formic acid.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described middle strong acid
For phosphoric acid.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described oxidant
For the combination of one or more in hydrogen peroxide, potassium dichromate, potassium permanganate, sodium hypochlorite, nitrate.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described oxidant
For potassium permanganate.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described polysaccharide or
Anionic polysaccharides is starch, cellulose, glycogen, chitosan, agar, carboxymethyl cellulose, carboxymethyl starch, carboxymethyl chitosan
The combination of one or more in sugar, sodium alginate.
A kind of novel porous nano carbon microsphere composite aquogel the most as claimed in claim 1, it is characterised in that: described polysaccharide
Or anionic polysaccharides is one or both the combination in chitosan, carboxymethyl chitosan, sodium alginate.
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| CN107375196A (en) * | 2017-07-26 | 2017-11-24 | 暨南大学 | A kind of natural polysaccharide composite aquogel carrier of phenolic group containing catechu and preparation method thereof |
| CN107808955A (en) * | 2017-10-27 | 2018-03-16 | 湖南工业大学 | A kind of absorbent charcoal material with spherical structure and its preparation method and application |
| CN109266463A (en) * | 2018-09-27 | 2019-01-25 | 镇江奥视达光学有限公司 | A kind of cleaning agent of concave lens and preparation method thereof |
| CN109908876A (en) * | 2019-04-22 | 2019-06-21 | 盐城工学院 | A kind of preparation method and application of the chitosan-based bionical attractive gel of polysaccharide nano microcrystalline doping |
| CN110746516A (en) * | 2019-10-29 | 2020-02-04 | 无锡贝迪生物工程股份有限公司 | Natural polymer hydrogel based on collagen and preparation method thereof |
| CN110871054A (en) * | 2018-08-31 | 2020-03-10 | 侯梦斌 | Preparation process of activated carbon water slurry agent |
| CN111330970A (en) * | 2020-03-18 | 2020-06-26 | 西南林业大学 | Method for reducing bioavailability of heavy metal composite contaminated soil in agricultural land |
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| CN113512208A (en) * | 2021-08-04 | 2021-10-19 | 哈尔滨工业大学 | Preparation method of sodium alginate-based photothermal distillation hydrogel |
| CN114832773A (en) * | 2022-03-08 | 2022-08-02 | 湖北工业大学 | Composite hollow carbon sphere ion adsorption material and preparation method and application thereof |
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