CN108940206A - A kind of carbon-based adsorbent material and preparation method thereof - Google Patents
A kind of carbon-based adsorbent material and preparation method thereof Download PDFInfo
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- 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
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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
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
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Abstract
The present invention relates to a kind of preparation methods of carbon-based adsorbent material, belong to technical field of water treatment, are specifically related to a kind of method that anodizing prepares carbon-based adsorbent material.Adsorbent material provided by the invention passes through electrochemical method oxidation and removing by fine graphite plate in deionized water, forms stable oxidation nanometer carbon liquid, then be made through dry and grinding.Testing result shows that adsorbent material made from this method has good absorption property to heavy metal ion, better than common adsorbent material active carbon.Electrochemical preparation method of the present invention is low in cost, and environmentally protective, and raw material are only graphite plate and deionized water, and intermediate product and product are nontoxic and pollution-free.
Description
Technical field
The present invention relates to a kind of adsorbent materials and preparation method thereof, belong to water treatment field, are specifically related to a kind of carbon-based
Adsorbent material and preparation method thereof.
Background technique
Sewage treatment at present is broadly divided into physics, biology and chemical method, and wherein absorption method is a kind of widely applied dirt
Method for treating water.In field of industrial waste water treatment, absorption method can be used for before biochemical method workshop section, remove some toxic organic
Object, heavy metal element, can also with advanced treating workshop section.
The commonly active charcoal of water process adsorbent material, activated alumina, silica gel, synthesis organic adsorption resin, zeolite etc.,
Container is generallyd use fix adsorbent material, sewage by wherein by method adsorb pollutant.These adsorbent materials exist
Preparation process can generate pollution, and adsorption process is easy the problem of blocking needs frequent progress to backwash and replace.These disadvantages are led
The use scope of absorption method has been caused to be limited in the lower advanced treating workshop section of pollutant concentration.
Summary of the invention
Present invention is primarily intended to solve, preparation method present in the prior art will cause pollution, use process is easy hair
The problem of raw blocking, provides a kind of carbon-based adsorbent material and preparation method thereof.The material includes the nano carbon material of various structures
Material, the surface of carbon material is partially oxidized, has good dispersibility, can direct plunge into water and use, absorption heavy metal from
After the pollutants such as son, since surface Zeta potential changes, can reunite sedimentation, can be used as sludge and exhaust.The sewage treatment material
The application method of material efficiently solves the common blockage problem of adsorption filtration method, can be used for the pretreatment and two of Industrial Waste Water Treatments
Grade processing, expands the scope of application of adsorbent material.Preparation method provided by the invention is environmentally protective, and main raw material(s) is graphite
Plate and deionized water, raw material and product are without noxious material, and no gas is useless, liquid is useless, solid waste, without carrying out blowdown.
Above-mentioned technical problem of the invention is mainly to be addressed by following technical proposals:
A kind of carbon-based adsorbent material, including single-layer graphene, multi-layer graphene, the graphite shell structurre being rolled up, stone
Black particle, unsetting carbon, at 10nm-10 μm, the surface of each material is partially oxidized scale.
A kind of preparation method of carbon-based adsorbent material, comprising the following steps:
Carbon liquid preparation step is that positive electrolysis electrode is electrolysed in deionized water to obtain oxidation nanometer carbon with graphite plate
Liquid；Wherein, in electrolytic process, the deionized water is to circulate and driven and vibrated by ultrasonic wave；
Oxidation nanometer carbon liquid is put into vacuum oven by drying steps, and setting temperature is 50-95 degrees Celsius, dry 4-
It is taken out after 12 hours.
The drying carbon material of taking-up is pulverized, is stored for future use by grinding steps.
In at least one embodiment of the present invention, in the carbon liquid preparation step, the graphite plate carbon content is greater than
99%, and graphite particle granularity is less than 100 microns.
In at least one embodiment of the present invention, the distance between positive and negative electrolysis electrode is 1-300mm, and electrolyte
Electrode is selected from austenite stainless steel plate, aluminium sheet, copper sheet, nickel plate, titanium plate or graphite plate.
In at least one embodiment of the present invention, current density is 1-500mA/cm between positive and negative electrolysis electrode2。
Therefore, the present invention has the advantage that provided carbon-based adsorbent material preparation method, at other common water
The preparation method of adsorbent material is managed, raw material only include graphite plate and deionized water, and are given up in process of production without gas, liquid
Useless, solid waste generates, environmentally protective, is suitble to industrialized production.Provided carbon-based adsorbent material, can the more typical water of application range
It handles adsorbent material to expand, is not limited only to advanced treating, is similarly applied to pre-treatment and two stage treatment workshop section.
Detailed description of the invention
Fig. 1 is that the TEM of the oxidation nanometer carbon liquid schemes, and enlargement ratio is 100,000 times.
Fig. 2 is the SEM figure of black solid described in embodiment 1, and enlargement ratio is 5000 times.
Fig. 3 is the Raman spectrum of carbon-based adsorbent material described in embodiment 2.
Fig. 4 is the grain size analysis number of ultrasonic vibrating plate group and the lower prepared carbon-based adsorbent material of single ultrasonic vibrating plate effect
According to.
Specific embodiment
Below with reference to the embodiments and with reference to the accompanying drawing the technical solutions of the present invention will be further described.
Embodiment:
The preparation method of the carbon-based adsorbent material of the present embodiment specifically includes the following steps:
Carbon liquid preparation step, using graphite plate as anode, graphite plate or metal plate are cathode, and electrode is dipped in deionized water
In, it circulates in water and is powered under the environment of ultrasound, anode graphite plate surface is inserted into graphite layers by electronics and ion, occurs
Deformation, while under the action of ultrasound, partial exfoliation, in this process, due to electrochemical reaction, graphite surface is by part oxygen
Change, forms the oxidation nanometer carbon material that can be stably dispersed in deionized water, be dispersed under the action of blender
In water, oxidation nanometer carbon liquid is made.
Oxidation nanometer carbon liquid is put into vacuum oven by drying steps, and setting temperature is 50-95 degrees Celsius, dry 4-
It is taken out after 12 hours.
The drying carbon material of taking-up is pulverized, is stored for future use by grinding steps.
Wherein, the graphite plate of the present embodiment is high purity graphite plate, and carbon content is greater than 99%, and graphite particle granularity is less than
100 microns.This is because, containing metal, acid, alkali, salt impurity, these impurity can change when graphite plate lower using purity
The Zeta potential for becoming obtained oxidation nanometer carbon liquid, causes reunion, deposited phenomenon.Graphite plate graphite particle granularity and electrochemistry are anti-
Answer stripped down oxidation nanometer carbon material size directly related, when graphite particle granularity increases, the oxidation removed is received
Rice carbon material size average will also increase, and biggish oxidation nanometer carbon material will be there is a phenomenon where reuniting, precipitating, macroscopic view ginseng
On number, the oxidation nanometer carbon liquid solid content rate of climb is slack-off, and the solid content of final oxidation nanometer carbon liquid finished product is lower；The gold
Belong to plate, be pure metal plate or alloy sheets, have certain acid resistance, preferentially select austenite stainless steel plate, aluminium sheet, copper sheet,
Nickel plate, titanium plate or graphite plate；Positive and negative anodes distance between plates is 1-300mm.
The distance between positive/negative plate need to be selected according to DC power supply maximum voltage and function, apart from excessive first in preparation
Phase due in deionized water charged particle it is few so that initial reaction is difficult, apart from carbon that is too small, falling off from graphite plate
Grain cannot be dispersed in water in time.The spacing of the present embodiment selection 5mm to 10mm.
In the present embodiment, it is electrolysed required each component, including positive and negative electrode, ultrasonic vibrating plate, blender etc., is placed in same
In container, which preferably selects to have certain acidproof and temperature capacity material, such as glass, austenitic stainless steel, organic
High molecular material.
In the present embodiment, the water in electrolytic process circulates environment and is provided by blender or water circle device, blender
Material should have certain acid-fast ability, and agitating paddle preferably selects Teflon stir paddle；Water circle device can be by additional pipeline
It is formed with water circulating pump, pipeline and water pump material preferably select acid resisting material, such as glass, austenitic stainless steel, organic polymer material
Material.
In the present embodiment, the ultrasound environments in electrolytic process are provided by ultrasonic vibrating plate, preferably select one or several ultrasound vibrations
Board group is shown at ultrasonic vibrating plate group, frequency 1-300KHz, measurement data, is prepared under a variety of ultrasonic wave collective effects carbon-based
The granularity that adsorbent material is prepared under acting on than a kind of ultrasonic wave is more evenly.As shown in figure 4, super for 20KHz, 40KHz, 80KHz
The partial size correlation data of sound and vibration board group and the lower obtained carbon-based adsorbent material of the single ultrasonic vibrating plate effect of 60Khz, uses survey
Amount equipment is laser particle analyzer.
In the present embodiment, energization in electrolytic process, should control current density between pole plate is 1-500mA/cm2.With electricity
Current density reduces, and electrochemical reaction speed reduces, and production efficiency is lower；As current density increases, obtained oxidation nanometer carbon
The average-size of material will increase, cause oxidation nanometer carbon liquid occur reunite, sedimentation, and finally oxidation nanometer carbon liquid at
The solid content of product is lower.To take into account production efficiency and controlling the size of oxidation nanometer carbon material, it is suitable that current density should be arranged in
Numerical value, should not be too large or too small.Control process can realize by process control DC power supply, can according to the current density of setting
The current maxima of DC power supply is set, and in an initial condition, charged particle is less in deionized water, and supply voltage will be set
To maximum value, with the progress of electrochemical reaction, electric current close to zero by being gradually increased, until the electric current for reaching setting is maximum
Value, voltage starts to gradually decrease, to maintain current density value constant.
In the present embodiment, electrochemical reaction should keep liquid temperature at 0-80 degrees Celsius, and the reaction time is 1-30 days；When reaction
Between determined by the solid content in nanometer carbon liquid, when solid content do not continue to rise when, electrochemical reaction should be stopped.
Oxidation nanometer carbon material in the present embodiment mainly includes single-layer graphene, multi-layer graphene, the stone being rolled up
Black shell structurre, graphite particle, unsetting carbon, scale is at 10nm-10 μm, and the surface of these materials is partially oxidized, containing rich
Rich surface functional group, thus it is not easy to reunite, it is not easily settled, it can steadily be dispersed in water, the stable oxidation of forming properties
Nanometer carbon liquid.
Oxidation nanometer carbon liquid in the present embodiment electrolytic process, with the progress of electrochemical reaction, oxidation-reduction potential by
The high, conductivity that edges up gradually increases, and pH value gradually decreases, and solid content gradually increases, final product oxidation nanometer carbon liquid, and ORP is
250-400mV, conductivity 1-5ms/cm, pH value 1.5-3.5, solid content 0.1%-0.6%.
In the present embodiment, vacuum oven in drying steps, temperature should be 30-100 degrees Celsius.
The present embodiment beneficial effect is provided carbon-based adsorbent material first, is inhaled compared with water process common in the market
Enclosure material can application range expand, be not limited only to advanced treating, be similarly applied to pre-treatment and two stage treatment workshop section.Secondly
Be that the preparation method of the carbon-based adsorbent material only includes graphite plate and deionized water, and in process of production it is useless without gas, liquid is useless,
Solid waste generates, environmentally protective, is suitble to industrialized production.
The present embodiment is described in detail below by two specific embodiments.
Embodiment 1
The step of preparing carbon-based adsorbent material is as follows:
It A. is graphite anode plate of the 1 μm of purity greater than 99% and 316 stainless steel positive plates with the interval 10mm by one group of granularity
It is placed in glass flume, sink is equipped with the water circulation system that external circulation line and circulating pump form, and is equipped with a ultrasound in sink
Vibration plate group, ultrasonic vibrating plate group include tri- ultrasonic vibrating plates of 20KHz, 40KHz, 80KHz, pour into deionized water until flooding electrode
Plate.
B. DC power supply is controlled to pole plate joining procedure, control condition is that current density is no more than 10mA/cm2, liquid temperature is not
More than 60 degrees Celsius.DC power supply and circulating pump continuous service, ultrasonic vibrating plate group are run with intermittent duty, are worked 5 minutes,
It shuts down 5 minutes, nanometer carbon liquid ORP to be oxidized, conductivity, solid content no longer significantly rise, and pH value stops after being no longer remarkably decreased
Operation.
Power supply maximum voltage is 100V, maximum current 10A.It is provided that initial setting up limits according to control condition power supply
Maximum current mode processed, according to anode plate and cathode plate size, a length of 25cm, width 20cm, setting maximum current are 5A.
Under original state, supply voltage 100V, electric current is close to 0A, and with the progress of electrochemical reaction, electric current gradually increases
Greatly, it is remained unchanged after reaching 5A, voltage is gradually decreased by 100V.At the same time, graphite plate surface constantly has misty graphite micro-
The color of abscission, water is gradually deepened.Every electrochemistry index of liquid changes simultaneously, ORP, conductivity, on solid content
It rising, pH value decline, final each index rests on ORP as 250-400mV, conductivity 1-5ms/cm, pH value 1.5-3.5, Gu
Content is 0.1%-0.6%, and no longer generation significant change, at this time oxidation nanometer carbon liquid preparation is completed.
C. the oxidation nanometer carbon liquid prepared in step B is placed in baking oven, temperature is set as 80 degrees Celsius, and drying 12 is small
When, obtain black solid.
D. black solid prepared in step C is pulverized, as carbon-based adsorbent material.
Embodiment 2
The step of preparing carbon-based adsorbent material is as follows:
It A. is graphite anode plate of 5 μm of purity greater than 99% and titanium positive plate with graphite plate, titanium plate, graphite by two pieces of granularities
The sequence of plate, the interval 5mm are placed in 316 steel water tanks, and blender and a ultrasonic vibrating plate group, ultrasonic vibrating plate group packet are equipped in sink
Two ultrasonic vibrating plates of 20KHz, 60KHz are included, pour into deionized water until flooding electrode plate.
B. DC power supply is controlled to pole plate joining procedure, control condition is that current density is no more than 20mA/cm2, liquid temperature is not
More than 70 degrees Celsius.DC power supply, blender and ultrasonic vibrating plate group continuous service, it is nanometer carbon liquid ORP to be oxidized, conductivity, solid
Content no longer significantly rises, and pH value is rear out of service after being no longer remarkably decreased.
Power supply maximum voltage is 200V, maximum current 50A.It is provided that initial setting up limits according to control condition power supply
Maximum current mode processed, according to anode plate and cathode plate size, a length of 30cm, width 30cm, setting maximum current are 36A.
Under original state, supply voltage 200V, electric current is close to 0A, and with the progress of electrochemical reaction, electric current gradually increases
Greatly, it is remained unchanged after reaching 36A, voltage is gradually decreased by 200V.At the same time, graphite plate surface constantly has misty graphite micro-
The color of abscission, water is gradually deepened.Every electrochemistry index of liquid changes simultaneously, ORP, conductivity, on solid content
It rising, pH value decline, final each index rests on ORP as 250-400mV, conductivity 1-5ms/cm, pH value 1.5-3.5, Gu
Content is 0.1%-0.6%, and no longer generation significant change, at this time oxidation nanometer carbon liquid preparation is completed.
C. the oxidation nanometer carbon liquid prepared in step B is placed in baking oven, temperature is set as 80 degrees Celsius, and drying 12 is small
When, obtain black solid.
D. black solid prepared in step C is pulverized, as carbon-based adsorbent material.
The absorption property comparative test of carbon-based adsorbent material and active carbon:
A. carbon-based adsorbent material and active carbon are mixed with 0.4% mass ratio with water respectively, and are ultrasonically treated, obtain carbon
The turbid of water mixing.
B. by the turbid of carbon-based adsorbent material and active carbon in step A respectively with Fe3+Ion concentration is 100ppm's
FeCl3Solution is mixed with the volume ratio of 1:1.
C. it by the mixed liquor ultrasound and stir process in step B, carries out to Fe3+The adsorption reaction of ion, reaction time is
0.5 hour.
D. above-mentioned mixed liquor is filtered after reacting, carbon-based adsorbent material and active carbon is filtered out, obtains more limpid
Filtrate.
E. the filtrate of carbon-based adsorbent material and active carbon in step D is taken, its supernatant is taken after static 4 hours, dilutes respectively
After ten times, with atomic absorption light spectrometry wherein Fe3+The content of ion.It is computed and measures, under the experiment condition, carbon-based adsorption material
Material and active carbon are to Fe3+The removal rate of ion is respectively 85.2% and 67.4%.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (9)
1. a kind of carbon-based adsorbent material, which is characterized in that including single-layer graphene, multi-layer graphene, the graphite shell being rolled up
Layer structure, graphite particle, unsetting carbon, at 10nm-10 μm, the surface of each material is partially oxidized scale.
2. a kind of preparation method of carbon-based adsorbent material, which comprises the following steps:
Carbon liquid preparation step makes the anolyte electrode of graphite material aoxidize the nano-sized carbon of formation in electrolytic process by vibration
Material is dissolved in liquid to prepare oxidation nanometer carbon liquid；
Drying and grinding step, the dry oxidation nanometer carbon liquid simultaneously pulverize the carbon material after drying.
3. a kind of preparation method of carbon-based adsorbent material according to claim 2, which is characterized in that the anolyte electricity
Extremely graphite plate, carbon content is greater than 99%, and graphite particle granularity is less than 100 microns.
4. a kind of preparation method of carbon-based adsorbent material according to claim 2, which is characterized in that the choosing of electrolyte electrode
From one of austenite stainless steel plate, aluminium sheet, copper sheet, nickel plate, titanium plate or graphite plate or a variety of.
5. a kind of preparation method of carbon-based adsorbent material according to claim 2, which is characterized in that positive and negative electrolysis electrode it
Between distance be 1-300mm.
6. a kind of preparation method of carbon-based adsorbent material according to claim 2, which is characterized in that be arranged in electrolytic vessel
Ultrasonic vibrating plate and agitating device.
7. a kind of preparation method of carbon-based adsorbent material according to claim 2, which is characterized in that the ultrasonic vibrating plate is
It is multiple, and it is divided into several groups, vibration frequency is different between each group.
8. a kind of preparation method of carbon-based adsorbent material according to claim 2, which is characterized in that between positive and negative electrolysis electrode
Current density is 1-500mA/cm2。
9. a kind of preparation method of carbon-based adsorbent material according to claim 2, which is characterized in that the carbon liquid preparation step
The oxidation nanometer carbon liquid parameter prepared in rapid are as follows: ORP 250-400mV, conductivity 1-5ms/cm, pH value 1.5-3.5, Gu
Content is 0.1%-0.6%.
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| KR100444358B1 (en) * | 2002-04-09 | 2004-08-16 | 한국과학기술연구원 | Surface Modification of Activated Carbon for Treatment of Wastewater |
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Application publication date: 20181207 |