CN108793308A - A kind of method of efficient removal heavy metal in waste water nickel ion - Google Patents
A kind of method of efficient removal heavy metal in waste water nickel ion Download PDFInfo
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- CN108793308A CN108793308A CN201810710866.XA CN201810710866A CN108793308A CN 108793308 A CN108793308 A CN 108793308A CN 201810710866 A CN201810710866 A CN 201810710866A CN 108793308 A CN108793308 A CN 108793308A
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- Prior art keywords
- nickel ion
- waste water
- heavy metal
- efficient removal
- removal heavy
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
-
- 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
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention relates to a kind of method of efficient removal heavy metal in waste water nickel ion, step includes:(1) preparation of graphene microballoon;(2)Nickel ion is adsorbed from waste water using graphene microballoon, the elution of nickel ion after absorption;(3)Before and after test absorption, the adsorbance of nickel ion.This method is simple, efficiently, can Reusability, be suitable for scale detection and efficiently remove the heavy metal nickel ion waste water.
Description
Technical field
The invention belongs to the application fields of Environmental Chemistry, the more particularly to efficient minimizing technology of heavy metal ions in wastewater.
Background technology
Graphene is as a kind of carbonaceous new material, since being found, due to its unique two-dimentional monoatomic layer structure,
Receive the extensive concern of people.Since graphene has big specific surface area and big pi-conjugated structure, so that it is had and inhaled as height
The potentiality of attached capacity sorbent agent can be applied to the heavy metal ion in absorption waste water.But Sheet Graphite alkene is easy in solid-state
It stacks, and is easy to reunite in the solution, this not only makes the reduction of its stability of solution, while also reducing its effective specific surface
Product, reduces its adsorption capacity.Simultaneously as Sheet Graphite alkene is not of uniform size, although under high speed centrifugation, the graphite of small lamella
Alkene also is difficult to separate from solution, thus causes it and applies obstacle as adsorbent.In contrast, graphene is micro-
Ball has better crushing resistance and anti-agglomeration, but still remains the advantage of its large specific surface area, is more suitable for adsorbing
The use of agent.
Heavy metal ion form stable, toxicity in water environment are big and can in vivo be accumulated by food chain,
It seriously endangers ecological environment and human health, heavy metal pollution has become the important environmental problem of facing mankind.Chemical nickel plating is useless
The traditional processing method of liquid mainly has ion-exchange, the precipitation method and electrolysis etc., but these methods are of high cost, complicated for operation
And often cause secondary pollution, it is difficult to achieve the effect that satisfied.And absorption method has at low cost, operation relative to these methods
Simply, it can be recycled and do not easily cause the advantages that secondary pollution, to be widely used in the processing of nickel-containing waste water.
Invention content
Technical problem to be solved by the invention is to provide a kind of method of efficient removal heavy metal in waste water nickel ion, this method
Using graphene microballoon as adsorbent, using the method for Static Adsorption, take it is less, can efficiently, in the slave waste water of high dose
Adsorb heavy metal nickel ion;The prices of raw materials used in the present invention are cheap, and obtained graphene microballoon has preferable anti-
Pressure property and anti-agglomeration, and specific surface area is larger, the potentiality with follow-up related application.
A kind of method of adsorbent absorption heavy metal in waste water nickel ion of the present invention, including:
(1)Graphene oxide is dissolved in the water, with ultrasonic atomizer by solution atomization, then by tube furnace, is used in combination poly- four
Vinyl fluoride PTFE filter membranes are collected, dry to get graphene microsphere adsorbing agent;
(2)Graphene microballoon is added in certain density nickel-containing waste water, in room temperature, the condition of certain rotating speed and certain pH value
Under, certain time is reacted, then solution is centrifuged under conditions of room temperature, certain rotating speed, ultraviolet specrophotometer is used in combination
The absorbance of supernatant after test centrifugation, for calculating adsorption capacity of the adsorbent to nickel ion.
The step(1)The mass concentration of middle graphene oxide solution is 7-10 wt.%.
The step(1)Ultrasonic frequency is 1.0 ~ 2.0 MHz in middle ultrasonic atomization process.
The step(1)The temperature of middle tube furnace is 350~450 DEG C.
The step(1)The middle aperture for collecting the PTFE filter membranes used is 0.20 ~ 0.45 μm.
The step(1)In at room temperature drying time be 8 ~ 15 h.
The step(2)Middle nickel ion solution concentration is 10 ~ 1000 mg/L.
The step(2)Middle rotating speed is 50 ~ 150 rpm.
The step(2)The pH value of middle solution is 2-10, and the reaction time is 0 ~ 300 min.
The step(2)Middle centrifugal rotational speed is 8000 ~ 12000 rpm, and centrifugation time is 3 ~ 10 min.
Advantageous effect
(1)The present invention utilizes graphene microballoon prepared by ultrasonic atomizatio method, easy to operate, is easy to industrial amplification;
(2)The graphene microballoon of the present invention has crushing resistance and anti-agglomeration, and is inhaled with preferable with larger specific surface area
Attached performance can adsorb heavy metal nickel ion in efficient, high dose slave waste water.
Description of the drawings
Fig. 1 is influence of the adsorption time to nickel ion adsorbance.
Fig. 2 is adsorption isotherm of the graphene microsphere adsorbing agent to nickel ion.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
The preparation of graphene microsphere adsorbing agent, includes the following steps:
Ultra-pure water is added into graphene oxide, prepares the graphene oxide solution that mass concentration is 8 wt.%, solution is placed in
It is connected in the ultrasonic atomizer of tube furnace, ultrasonic frequency 1.5MHz.It is set to be atomized into aerosol droplets, in N2 and suction filtration
It is slow transitted through under vacuum pump driving and is heated to 400 DEG C of tube furnace, end is collected with 0.22 um PTFE filter membranes.It dries at room temperature
8 h are to get graphene microsphere adsorbing agent, and graphene microspherulite diameter prepared by the present invention is in 5 um or so.
Embodiment 2
Graphene microsphere adsorbing agent includes the following steps the adsorption experiment of nickel ion under different time
10 mg graphene microsphere adsorbing agents are accurately weighed with electronic balance, be added to the nickel of a concentration of 400 mg/L of 20 mL from
In sub- solution.Under conditions of room temperature, 100 rpm and pH=8.0, the different time is adsorbed, then 10000 rpm centrifuge 8 points
Clock,
It is used in combination ultraviolet specrophotometer to test the variation front and back in absorption of its absorbance, calculates adsorbent according to the following formula when different
Between under adsorbance.
q(t)=(C0-Ct)V/m
In formula, q (t) indicates the adsorbance (mg/g) of t moment;C0, Ct indicate nickel ion concentration in initial soln (mg/L) respectively,
Nickel ion concentration (mg/L) in solution after nickel ion concentration (mg/L) in t moment solution, and absorption;V and m indicate nickel respectively
The quality (g) of volume (L) and adsorbent of solion.
Fig. 1 is shown in influence of the graphene ball to the adsorbance of nickel ion under different time.It can be seen from figure 1 that graphene microballoon is inhaled
Attached dose very fast to the adsorption rate of nickel ion, just reaches 70% or more of adsorbance saturation value within 5 minutes, illustrates the suction of the present invention
Attached dose is a kind of efficient, efficient adsorbent.
Embodiment 3
The test of adsorption isotherm, includes the following steps:
10 mg graphene microsphere adsorbing agents are accurately weighed with electronic balance, the concentration range for being added to 20 mL is 40-800 mg/
In the nickel ion solution of L.Under conditions of room temperature, 100 rpm and pH=8.0,120 min are adsorbed, ultraviolet specrophotometer is used in combination
The variation front and back in absorption of its absorbance is tested, the concentration of remaining nickel ion in each solution is calculated with this, draws adsorption isotherm
Line tests the maximal absorptive capacity of graphene microballoon, sees Fig. 2.It can be seen from the figure that the adsorbance of adsorbent is with nickel in solution
The increase of ion concentration and increase, until absorption reach balance.When nickel ion concentration is relatively low, the adsorbance of adsorbent is less,
This may be because at low concentrations, the adsorption site on adsorbent is not fully utilized;And with the increase of nickel ion concentration,
The adsorption site of unsaturated state on adsorbent continues and nickel ion combines, to make adsorbance increase, until absorption reaches flat
Weighing apparatus.We can also be seen that adsorbent is 155.8 mg/g to the maximum saturation adsorbance of nickel ion from figure, illustrate the present invention
Adsorbent be that a kind of this adsorption capacity is big, efficient adsorbent for heavy metal.
Claims (6)
1. a kind of method of efficient removal heavy metal in waste water nickel ion, includes the following steps:
(1)Graphene oxide is dissolved in the water, with ultrasonic atomizer by solution atomization, then by tube furnace, is used in combination poly- four
Vinyl fluoride filter membrane is collected, dry to get graphene microsphere adsorbing agent;
(2)By a certain amount of step(1)The graphene microballoon of middle preparation is added in certain density nickel-containing waste water, in room temperature and
Under conditions of certain pH value, certain time is reacted, is then centrifuged for, the concentration of the front and back nickel ion of test absorption calculates adsorbance.
2. a kind of method of efficient removal heavy metal in waste water nickel ion according to claim 1, which is characterized in that described
Step(1)Described in graphene oxide solution mass concentration be 7-10 wt.%.
3. a kind of method of efficient removal heavy metal in waste water nickel ion according to claim 1, which is characterized in that described
Step(2)The quality of middle graphene microballoon is 5-15 mg.
4. a kind of method of efficient removal heavy metal in waste water nickel ion according to claim 1, which is characterized in that described
Step(2)Middle nickel ion solution concentration is 10 ~ 1000 mg/L.
5. a kind of method of efficient removal heavy metal in waste water nickel ion according to claim 1, which is characterized in that described
Step(2)The pH value of middle solution is 2 ~ 10, and the reaction time is 0 ~ 300 min.
6. a kind of method of efficient removal heavy metal in waste water nickel ion according to claim 1, which is characterized in that described
Step(2)Middle centrifugal rotational speed is 8000 ~ 12000 rpm, and centrifugation time is 3 ~ 10 min.
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Citations (6)
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---|---|---|---|---|
US20120168383A1 (en) * | 2010-12-29 | 2012-07-05 | Korea Institute Of Science And Technology | Graphene-iron oxide complex and fabrication method thereof |
CN103663601A (en) * | 2013-08-05 | 2014-03-26 | 南昌大学 | Method for absorptively separating low-concentration heavy-metal ions by utilizing graphene oxide colloid |
CN105884100A (en) * | 2016-06-08 | 2016-08-24 | 浙江奇彩环境科技股份有限公司 | Heavy metal wastewater treatment method |
WO2016172755A1 (en) * | 2015-04-28 | 2016-11-03 | Monash University | Non-covalent magnetic graphene oxide composite material and method of production thereof |
CN106268644A (en) * | 2016-09-12 | 2017-01-04 | 方亚鹏 | A kind of High-efficient Water scavenging material and preparation method and application |
CN107200375A (en) * | 2017-08-09 | 2017-09-26 | 苏州佰锐生物科技有限公司 | A kind of efficient method for removing metal copper ion in waste water |
-
2018
- 2018-07-03 CN CN201810710866.XA patent/CN108793308A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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US20120168383A1 (en) * | 2010-12-29 | 2012-07-05 | Korea Institute Of Science And Technology | Graphene-iron oxide complex and fabrication method thereof |
CN103663601A (en) * | 2013-08-05 | 2014-03-26 | 南昌大学 | Method for absorptively separating low-concentration heavy-metal ions by utilizing graphene oxide colloid |
WO2016172755A1 (en) * | 2015-04-28 | 2016-11-03 | Monash University | Non-covalent magnetic graphene oxide composite material and method of production thereof |
CN105884100A (en) * | 2016-06-08 | 2016-08-24 | 浙江奇彩环境科技股份有限公司 | Heavy metal wastewater treatment method |
CN106268644A (en) * | 2016-09-12 | 2017-01-04 | 方亚鹏 | A kind of High-efficient Water scavenging material and preparation method and application |
CN107200375A (en) * | 2017-08-09 | 2017-09-26 | 苏州佰锐生物科技有限公司 | A kind of efficient method for removing metal copper ion in waste water |
Non-Patent Citations (1)
Title |
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