CN110433771A - A kind of pair of Co (II) has the functionalized carbon nano material and preparation method thereof of absorption property - Google Patents
A kind of pair of Co (II) has the functionalized carbon nano material and preparation method thereof of absorption property Download PDFInfo
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- CN110433771A CN110433771A CN201910660828.2A CN201910660828A CN110433771A CN 110433771 A CN110433771 A CN 110433771A CN 201910660828 A CN201910660828 A CN 201910660828A CN 110433771 A CN110433771 A CN 110433771A
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- carbon nano
- nano material
- functionalized carbon
- absorption property
- graphene oxide
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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
- B01J20/0203—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
- B01J20/0274—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 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
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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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
-
- 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
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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 the functionalized carbon nano materials and preparation method thereof that a kind of pair of Co (II) has absorption property.The present invention is the PO using graphene oxide as matrix, in phosphoric acid4 3‑Group is supported on the surface of graphene oxide composite material by covalent bond P-C-；The mass ratio of P element and graphene oxide is 1:2-1:7.Carbon material prepared by the present invention has remarkable result, and the low raw-material cost that the present invention uses for the absorption property of cobalt ions, easy to operate, and environmental-friendly, used raw material is the advantages that nature enriches.
Description
Technical field
The invention belongs to inorganic adsorbing material fabricating technology fields, are related to a kind of pair of Co (II) with absorption property
A kind of preparation method of functionalized carbon nano material, and in particular to carbon nanomaterial for heavy metal ion with absorption property
Preparation method.
Background technique
In recent years, with the high speed development of modern industry, a large amount of unprocessed or sewage direct emission that processing is below standard,
Violent destruction is caused to water environment, leads to water quality deterioration, and water quality type water shortage problem becomes increasingly conspicuous.It shows according to investigations, Chinatown
City's wastewater treatment rate only has 36%, and a large amount of raw sewerage direct emissions become the pollution source of urban environment.With this
Meanwhile industrialized development increases the discharge amount of industrial wastewater, including acidic and alkaline waste water, paper waste, effluent containing heavy metal ions
And waste water from dyestuff etc., wherein heavy metal wastewater thereby be environmental pollution most serious and to the mankind endanger maximum industrial wastewater it
One.Common heavy metal wastewater thereby includes the sewage containing metal ions such as lead, cadmium, chromium, mercury, nickel, cobalts, results from smelting, electrolysis
With plating etc. industrial process.Discharge of wastewater containing plurality of heavy metal is formed heavy metal pollution into natural water.With much money
Belong to pollution the characteristics of be it is difficult to degrade, have enriching and high toxicity.With heavy metal existing for various chemical states or chemical form,
It will retain, accumulate and migrate after entering environment or the ecosystem, can also be accumulated in algae and bed mud, by fish and shellfish
Body surface absorption generates food chain concentration, to cause public hazards.
In numerous heavy metal elements, do not have an effect with water under Co (II) room temperature, stability is also higher in air, is
A kind of amphoteric metal.Cobalt is chiefly used in manufacturing alloy in the industry and produces pigment, and Long Term Contact easily causes anaphylaxis or irritation
Dermatitis.Cobalt dirt can also cause the diseases such as respiratory disease and pneumonia, acute gastritis, and the serious gene for also resulting in living cells is prominent
Become, greatly endangers the health of the mankind.
Up to the present, the method for removing Heavy Metals in Waters has ion-exchange, membrane filter method, coagulant sedimentation
And absorption method.Wherein absorption method has the characteristics that safety and low cost, and this method does not generate harmful side product, can be effectively
Remove the pollutant in various water bodys.
Summary of the invention
It is an object of the invention in view of the shortcomings of the prior art, providing a kind of pair of heavy metal ion with absorption property
Functionalized carbon nano material, loads PO on the carbon material4 3-Group realizes it to the metal Co in water body2+The selectivity of ion is inhaled
It is attached.
It is the phosphorus using graphene oxide as matrix that the present invention, which has the functionalized carbon nano material of absorption property to Co (II),
PO in acid4 3-Group is supported on the surface of graphene oxide composite material by covalent bond P-C-；The matter of P element and graphene oxide
Amount is than being 1:2-1:7.
It is a further object to provide the preparation methods of above-mentioned functionalized carbon nano material, specifically include following step
It is rapid:
Step 1) electrolysis: connecing graphite rod for DC stable power supply anode, and cathode connects graphite plate, with test tube clamp by graphite rod and
Graphite plate, which is fixed to, to be placed in the container that 250-1000mL concentration is 0.5-1.0mol/L phosphoric acid electrolyte.
It after being put into magnetic stir bar in a reservoir, places it on magnetic stirring apparatus, powers on, adjust DC stabilization electricity
Source, starting voltage 5.0-8.0V.When graphite rod is consumed to total length 1/5, power off and magnetic stirring apparatus.
Step 2) filtering: step 1) acquired solution is staticly settled, is rinsed after removing supernatant with distilled water, is stood again
Afterwards, it rinses again, by rinsing repeatedly, solution acid-basicity is measured when it is close neutral with pH test paper, by neutral solution
Filtering moves into filter residue in evaporating dish.
Step 3) is dry: filter residue obtained by step 2) being put into vacuum oven, 60-90 DEG C of temperature is adjusted, in vacuum item
It takes out under part after dry 5-8h to get to Co2+Functionalized carbon nano material with absorption property.
Beneficial effects of the present invention:
Functionalized carbon nano material of the present invention is to Co2+Absorption property it is significant, having for cobalt ions waste water adsorbing domain
Good application prospect.The present invention have method is simple, preparation reaction rate is fast, can carry out at normal temperatures and pressures, is at low cost,
Yield height and environmental-friendly advantage are expected to carry out industrialized production.
Detailed description of the invention
Fig. 1 is to load PO obtained by embodiment 14 3--Infrared spectroscopy (IR) figure of group carbon nanomaterial；
Fig. 2 is to load PO obtained by embodiment 14 3-Group carbon nanomaterial, unsupported PO4 3-Group carbon nanomaterial and powder
The absorption property comparison diagram that last absorbent charcoal material adsorbs cobalt ions.
Specific embodiment
Below according to specific embodiment, the present invention will be described in detail, and the objects and effects of the present invention will be more apparent.
Comparative example 1
1) anodic oxidation of carbon nanomaterial: the 6.94mL concentrated sulfuric acid is dissolved in the distilled water of 50mL, and is added a certain amount of
Distilled water be settled in the volumetric flask of 250mL, obtain clear electrolyte；With graphite rod (5 × 100mm of dimension D) for anode,
Graphite flake (10 × 2 × 100mm of size) is cathode, is fixed to and is placed in the beaker of sulfuric acid electrolyte with test tube clamp, is put into magnetic force
It is placed on magnetic stirring apparatus after stirrer, opening magnetic stirring apparatus is uniformly mixed solution, DC stable power supply is connected and adjusts,
Starting voltage is 5.0-8.0V.
2) it filters: when graphite rod is consumed to residue 1/5, the solution left standstill for dissolving graphite powder being precipitated, after removing supernatant
It is rinsed with distilled water, after standing again, is rinsed again, by rinsing repeatedly, with pH test paper measurement solution acid-basicity until it
Close to neutrality.
3) it is dried in vacuo: neutral solution obtained by step 2) is filtered, be put into vacuum oven after filter residue is moved into evaporating dish
In, 60-80 DEG C of temperature is adjusted, is taken out after drying 5-8 hour under vacuum conditions to get the carbon nanometer with absorption property is arrived
Material.Obtained carbon nanomaterial is put into spare in the drier for fill silica gel.
Embodiment 1
1) anodic oxidation of carbon nanomaterial: 8.22mL concentrated phosphoric acid is dissolved in the distilled water of 50mL, and is added a certain amount of
Distilled water be settled in the volumetric flask of 500mL, obtain clear concentration be 0.5-1.0mol/L electrolyte；With graphite rod (ruler
Very little D5 × 100mm) it is anode, graphite flake (10 × 2 × 100mm of size) is cathode, is fixed to test tube clamp and is placed with 250mL phosphoric acid
In the beaker of electrolyte, it is placed on magnetic stirring apparatus after being put into magnetic stir bar, opening magnetic stirring apparatus is uniformly mixed solution,
Connect and adjust DC stable power supply, starting voltage 5.0V.
2) it filters: when graphite rod is consumed to residue 1/5, the solution left standstill for dissolving graphite powder being precipitated, after removing supernatant
It is rinsed with distilled water, after standing again, is rinsed again, by rinsing repeatedly, with pH test paper measurement solution acid-basicity until it
Close to neutrality.
3) it is dried in vacuo: neutral solution obtained by step 2) is filtered, be put into vacuum oven after filter residue is moved into evaporating dish
In, temperature 60 C is adjusted, is taken out after drying 5 hours under vacuum conditions to get the carbon nanomaterial with absorption property is arrived
(mass ratio of P element and nano-carbon material is 1:2-1:7).Obtained carbon nanomaterial is put into the drier for filling silica gel
In it is spare.Fig. 1 is to load PO obtained by embodiment 14 3--Infrared spectroscopy (IR) figure of group carbon nanomaterial.
Embodiment 2
1) anodic oxidation of carbon nanomaterial: 16.44mL concentrated phosphoric acid is dissolved in the distilled water of 50mL, and is added a certain amount of
Distilled water be settled in the volumetric flask of 250mL, obtain clear concentration be 0.5-1.0mol/L electrolyte；With graphite rod (ruler
Very little D5 × 100mm) it is anode, graphite flake (10 × 2 × 100mm of size) is cathode, is fixed to test tube clamp and is placed with 250mL phosphoric acid
In the beaker of electrolyte, it is placed on magnetic stirring apparatus after being put into magnetic stir bar, opening magnetic stirring apparatus is uniformly mixed solution,
Connect and adjust DC stable power supply, starting voltage 5V.
2) it filters: when graphite rod is consumed to residue 1/5, the solution left standstill for dissolving graphite powder being precipitated, after removing supernatant
It is rinsed with distilled water, after standing again, is rinsed again, by rinsing repeatedly, with pH test paper measurement solution acid-basicity until it
Close to neutrality.
3) it is dried in vacuo: neutral solution obtained by step 2) is filtered, be put into vacuum oven after filter residue is moved into evaporating dish
In, temperature 60 C is adjusted, is taken out after drying 5 hours under vacuum conditions to get the carbon nanomaterial with absorption property is arrived
(mass ratio of P element and nano-carbon material is 1:2-1:7).Obtained carbon nanomaterial is put into the drier for filling silica gel
In it is spare.
Embodiment 3
1) anodic oxidation of carbon nanomaterial: 8.22mL concentrated phosphoric acid is dissolved in the distilled water of 50mL, and is added a certain amount of
Distilled water be settled in the volumetric flask of 250mL, obtain clear concentration be 0.5-1.0mol/L electrolyte；With graphite rod (ruler
Very little D5 × 100mm) it is anode, graphite flake (10 × 2 × 100mm of size) is cathode, is fixed to test tube clamp and is placed with 250mL phosphoric acid
In the beaker of electrolyte, it is placed on magnetic stirring apparatus after being put into magnetic stir bar, opening magnetic stirring apparatus is uniformly mixed solution,
Connect and adjust DC stable power supply, starting voltage 5.0V.
2) it filters: when graphite rod is consumed to residue 1/5, the solution left standstill for dissolving graphite powder being precipitated, after removing supernatant
It is rinsed with distilled water, after standing again, is rinsed again, by rinsing repeatedly, with pH test paper measurement solution acid-basicity until it
Close to neutrality.
3) it is dried in vacuo: neutral solution obtained by step 2) is filtered, be put into vacuum oven after filter residue is moved into evaporating dish
In, temperature 60 C is adjusted, is taken out after drying 5 hours under vacuum conditions to get the carbon nanomaterial with absorption property is arrived
(mass ratio of P element and nano-carbon material is 1:2-1:7).Obtained carbon nanomaterial is put into the drier for filling silica gel
In it is spare.
Embodiment 4
1) anodic oxidation of carbon nanomaterial: 8.22mL concentrated phosphoric acid is dissolved in the distilled water of 50mL, and is added a certain amount of
Distilled water be settled in the volumetric flask of 250mL, obtain clear concentration be 0.5-1.0mol/L electrolyte；With graphite rod (ruler
Very little D5 × 100mm) it is anode, graphite flake (10 × 2 × 100mm of size) is cathode, is fixed to test tube clamp and is placed with 250mL phosphoric acid
In the beaker of electrolyte, it is placed on magnetic stirring apparatus after being put into magnetic stir bar, opening magnetic stirring apparatus is uniformly mixed solution,
Connect and adjust DC stable power supply, starting voltage 7.0V.
2) it filters: when graphite rod is consumed to residue 1/5, the solution left standstill for dissolving graphite powder being precipitated, after removing supernatant
It is rinsed with distilled water, after standing again, is rinsed again, by rinsing repeatedly, with pH test paper measurement solution acid-basicity until it
Close to neutrality.
3) it is dried in vacuo: neutral solution obtained by step 2) is filtered, be put into vacuum oven after filter residue is moved into evaporating dish
In, temperature 60 C is adjusted, is taken out after drying 8 hours under vacuum conditions to get the carbon nanomaterial with absorption property is arrived
(mass ratio of P element and nano-carbon material is 1:2-1:7).Obtained carbon nanomaterial is put into the drier for filling silica gel
In it is spare.
Embodiment 5
1) anodic oxidation of carbon nanomaterial: 8.22mL concentrated phosphoric acid is dissolved in the distilled water of 50mL, and is added a certain amount of
Distilled water be settled in the volumetric flask of 250mL, obtain clear concentration be 0.5-1.0mol/L electrolyte；With graphite rod (ruler
Very little D5 × 100mm) it is anode, graphite flake (10 × 2 × 100mm of size) is cathode, is fixed to test tube clamp and is placed with 250mL phosphoric acid
In the beaker of electrolyte, it is placed on magnetic stirring apparatus after being put into magnetic stir bar, opening magnetic stirring apparatus is uniformly mixed solution,
Connect and adjust DC stable power supply, starting voltage 8.0V.
2) it filters: when graphite rod is consumed to residue 1/5, the solution left standstill for dissolving graphite powder being precipitated, after removing supernatant
It is rinsed with distilled water, after standing again, is rinsed again, by rinsing repeatedly, with pH test paper measurement solution acid-basicity until it
Close to neutrality.
3) it is dried in vacuo: neutral solution obtained by step 2) is filtered, be put into vacuum oven after filter residue is moved into evaporating dish
In, temperature 70 C is adjusted, is taken out after drying 8 hours under vacuum conditions to get the carbon nanomaterial with absorption property is arrived
(mass ratio of P element and nano-carbon material is 1:2-1:7).Obtained carbon nanomaterial is put into the drier for filling silica gel
In it is spare.
Adsorption experiment of the invention: in order to prove load PO4 3-The absorption property of group carbon nanomaterial, the present invention carry out
To the adsorption experiment for the simulation cobalt chloride waste water that concentration is 0.01mg/mL, the load PO of preparation is weighed respectively4 3-The carbon of group
Nano material, unsupported PO4 3-Group carbon nanomaterial and absorbent charcoal material (BET specific surface area 750m2/ g, 70 DEG C of dryings
5 hours) each 0.05g, loaded in 250mL ground conical flask.The configured cobalt chloride solution of 50mL is respectively added in four bottles,
It is put into constant-temperature table, shaking table set temperature is 25 degree, revolving speed 150rpm.
Entire reaction lasts two hours, has therefrom intercepted 8 time points.It is inhaled by the uv-vis spectra of divalent cobalt ion
The variation of receipts value comes and passes through standard curve and be converted to concentration to characterize its absorption property, and experimental result is shown in Fig. 2.It can be with from Fig. 2
Find out: load PO4 3-Group carbon nanomaterial absorption property is best, to the removal rate of cobalt ions in solution up to 84.11%, with not
Load PO4 3-The carbon nanomaterial of group improves 68.7%.Powder activated carbon is 19.32% to the removal rate that cobalt ions adsorbs.
It can be seen that loading PO as made from electrochemistry anodic oxidation by raw material of graphite4 3-The carbon nanomaterial pair of group
Cobalt ions in solution has good absorption property, has certain practical extending application value.
Claims (4)
1. the functionalized carbon nano material that a kind of pair of Co (II) has absorption property, it is characterised in that using graphene oxide as base
Body, the PO in phosphoric acid4 3-Group is supported on the surface of graphene oxide composite material by covalent bond P-C-.
2. functionalized carbon nano material as described in claim 1, it is characterised in that the mass ratio of P element and graphene oxide is
1:2-1:7.
3. the preparation method of functionalized carbon nano material as claimed in claim 1 or 2, it is characterised in that this method includes following
Step:
Step 1) electrolysis: connecing graphite rod for DC stable power supply anode, and cathode connects graphite plate, with test tube clamp by graphite rod and graphite
Plate, which is fixed to, to be placed in the container that 250-1000mL concentration is 0.5-1.0mol/L phosphoric acid electrolyte；
It after being put into magnetic stir bar in a reservoir, places it on magnetic stirring apparatus, powers on, adjust DC stable power supply,
Starting voltage is 5.0-8.0V；When graphite rod is consumed to total length 1/5, power off and magnetic stirring apparatus；
Step 2) filtering: step 1) acquired solution being staticly settled, is rinsed after removing supernatant with distilled water, after standing again,
It rinses again, by rinsing repeatedly, until when solution acid-basicity is neutral, filtering；
Step 3) is dry: filter residue obtained by step 2) being put into vacuum oven, adjusts 60-90 DEG C of temperature, under vacuum conditions
Taken out after dry 5-8h to get.
4. application of the functionalized carbon nano material as claimed in claim 1 or 2 in cobalt-containing wastewater absorption.
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| CN201910660828.2A CN110433771A (en) | 2019-07-22 | 2019-07-22 | A kind of pair of Co (II) has the functionalized carbon nano material and preparation method thereof of absorption property |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN105478074A (en) * | 2015-12-23 | 2016-04-13 | 中国科学院烟台海岸带研究所 | Preparation method and application of heavy metal ion remover |
| CN108502874A (en) * | 2017-02-28 | 2018-09-07 | 上海华明高技术（集团）有限公司 | A kind of method that electrochemistry assisting ultrasonic method prepares graphene dispersing solution |
-
2019
- 2019-07-22 CN CN201910660828.2A patent/CN110433771A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN105478074A (en) * | 2015-12-23 | 2016-04-13 | 中国科学院烟台海岸带研究所 | Preparation method and application of heavy metal ion remover |
| CN108502874A (en) * | 2017-02-28 | 2018-09-07 | 上海华明高技术（集团）有限公司 | A kind of method that electrochemistry assisting ultrasonic method prepares graphene dispersing solution |
Non-Patent Citations (3)
| Title |
|---|
| NAVNEET KUMAR: "Simple Synthesis of Large Graphene Oxide Sheets via Electrochemical Method Coupled with Oxidation Process", 《ACS OMEGA》 * |
| 李宏伟: "石墨烯的电化学方法制备及其对重金属离子的吸附研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 邓佳等: "磁性氧化石墨烯的制备及其对Co(Ⅱ)的吸附", 《核化学与放射化学》 * |
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Application publication date: 20191112 |