CN109967035A - A kind of EGTA modified magnetic carbon adsorbent and preparation method thereof and its application method - Google Patents
A kind of EGTA modified magnetic carbon adsorbent and preparation method thereof and its application method Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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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- 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 technical field of absorbent, discloses a kind of EGTA modified magnetic carbon adsorbent and preparation method thereof and its application method, method include: by Fe3O4Powder is added to the water, and is added after ultrasonic disperse into glucose solution, reacts 1-10h at a temperature of 120-200 DEG C, obtain Fe3O4@mC；By Fe3O4@mC is added to H2O2In solution, ultrasonic disperse, to Fe3O4@mC is activated；By the Fe of activation3O4@mC is dispersed in water, and EGTA solution is added, heats and stirs, and is reacted 1-8h, is obtained EGTA modified magnetic carbon adsorbent.By the modified magnetic carbon adsorbent of EGTA, adsorption capacity is big, and removal of heavy metal ions rate is high, and the stability of absorption is strong.
Description
Technical field
The present invention relates to technical field of absorbent more particularly to a kind of EGTA modified magnetic carbon adsorbent and preparation method thereof
And its application method.
Background technique
Heavy metal pollution is the environmental pollution caused by being endangered due to heavy metal and its compound, mainly water pollution,
In addition there are also solid waste and atmosphere pollution.Heavy metal accumulation is very strong, is unable to auto-degradation, when it is discharged into water,
Water body and ambient enviroment will certainly be polluted, the generations such as Measures of Algae in Water Body, fish, shellfish can also be endangered, polluted water quality,
The enrichment of metal ion is caused by biological chain concentration.
The processing method of heavy metal wastewater thereby all has some disadvantages at present or cost price is excessively high, or separation it is more difficult and
Form secondary pollution etc..There are also existing being much to adsorb using magnetic carbon adsorbent to heavy metal wastewater thereby, heavy metal is removed,
But existing magnetic carbon adsorbent, when removing heavy metal wastewater thereby, adsorption effect is unobvious, and absorption stability is poor.
Summary of the invention
In view of this, the present invention provides a kind of EGTA modified magnetic carbon adsorbent and preparation method thereof and its application sides
Method, by the modified magnetic carbon adsorbent of EGTA, adsorption capacity is big, and removal of heavy metal ions rate is high.
A kind of preparation method of EGTA modified magnetic carbon adsorbent, method include:
S1. by Fe3O4Powder is added to the water, and is added after ultrasonic disperse into glucose solution, at a temperature of 120-200 DEG C
1-10h is reacted, Fe is obtained3O4@mC；
S2. by Fe3O4@mC is added to H2O2In solution, ultrasonic disperse, to Fe3O4@mC is activated；
S3. by the Fe of activation3O4@mC is dispersed in water, and EGTA solution is added, heats and stirs, and is reacted 1-8h, is obtained
EGTA modified magnetic carbon adsorbent.
Preferably, the Fe in the step S13O4Powder preparation method are as follows:
Taking the ratio between amount of substance is the FeCl of 2:13·6H2O and FeCl2·4H2O is dissolved in the water, and stirs evenly, and obtains
Mixed solution；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 60-80 DEG C of water-bath, stirring is slowly added to ammonium hydroxide, reacts
1-2h obtains Fe3O4；
By Fe3O4It is washed with water to neutrality, is dried in vacuo 6-12h under conditions of 50-80 DEG C, obtains Fe3O4Powder.
Preferably, the EGTA solution manufacturing method in the step S3 are as follows:
In NaOH solution, EGTA powder is added, EGTA solution is made.
Preferably, after the step S1, before step S2 further include:
The Fe that will be obtained3O4@mC carries out water and dehydrated alcohol washing, dry and grinding.
Preferably, after the step S3 further include:
EGTA modified magnetic carbon adsorbent is washed, dried and ground.
Preferably, the step S1 specifically:
By Fe3O4Powder is added in pure water, ultrasonic disperse 10-20min, is added after ultrasonic disperse into glucose solution,
Fe3O4Powder and glucose quality ratio are 1:(5-30), Fe3O4With glucose solution mixing ultrasonic disperse 5-15min, in 120-
1-10h is reacted at a temperature of 200 DEG C, obtains Fe3O4@mC。
Preferably, the step S2 specifically:
By Fe3O4The H that it is 15-30% to concentration that@mC, which is added,2O2In solution, ultrasonic disperse 10-30min, to Fe3O4@mC into
Row activation.
Preferably, the step S3 specifically:
By the Fe of activation3O4@mC is scattered in pure water, EGTA solution is added, wherein Fe3O4The mass ratio of@mC and EGTA
For (2:1)-(1:10), 1-8h is reacted, obtains EGTA modified magnetic carbon adsorbent after washing is dry.
A kind of EGTA modified magnetic carbon adsorbent, the adsorbent are made according to the above method.
A kind of application method of EGTA modified magnetic carbon adsorbent, method are as follows:
By EGTA modified magnetic carbon adsorbent made from the above method and heavy metal wastewater thereby hybrid reaction, to being mixed after reaction
System applies magnetic field, and the magnetic adsorbent for being adsorbed with heavy metal is separated with aqueous solution.
The present invention provides a kind of EGTA modified magnetic carbon adsorbent and preparation method thereof and its application methods, by EGTA
Modified magnetic carbon adsorbent, adsorption capacity is big, and removal of heavy metal ions rate is high, and the stability of absorption is strong；Preparation method
Preparation condition is simple, mild, energy saving, and short preparation period is at low cost.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are some of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
It should be appreciated that ought use in this specification and in the appended claims, term " includes " and "comprising" instruction
Described feature, entirety, step, operation, the presence of element and/or component, but one or more of the other feature, whole is not precluded
Body, step, operation, the presence or addition of element, component and/or its set.
It will be further appreciated that the term "and/or" used in description of the invention and the appended claims is
Refer to any combination and all possible combinations of one or more of associated item listed, and including these combinations.
A kind of preparation method of EGTA modified magnetic carbon adsorbent, method include:
Fe3O4The preparation of powder:
Taking the ratio between amount of substance is the FeCl of 2:13·6H2O and FeCl2·4H2O is dissolved in the water, and stirs evenly, and obtains
Mixed solution；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 60-80 DEG C of water-bath, stirring is slowly added to ammonium hydroxide, reacts
1-2h obtains Fe3O4；
By Fe3O4It is washed with water to neutrality, is dried in vacuo 6-12h under conditions of 50-80 DEG C, obtains Fe3O4Powder, it is spare；
The preparation of EGTA solution:
In NaOH solution, EGTA powder is added, EGTA solution is made, it is spare；
Fe3O4The preparation of@mC: by the Fe of preparation3O4Powder is added to the water, ultrasonic disperse 10-20min, adds after ultrasonic disperse
Enter into glucose solution, Fe3O4Powder and glucose quality ratio are 1:5-30, Fe3O4With glucose solution mixing ultrasonic disperse
5-15min reacts 1-10h at a temperature of 120-200 DEG C, obtains Fe3O4@mC；It will obtain Fe3O4@mC carries out water and dehydrated alcohol
Washing, dry and grinding.
Fe3O4The activation of@mC: by Fe3O4The H that it is 15-30% to concentration that@mC, which is added,2O2In solution, every gram of Fe3O4@mC powder
15-30mL H is added in end2O2Solution, ultrasonic disperse 15-30min, to Fe3O4@mC is activated；
Fe3O4The preparation of@mC@EGTA: by the Fe of activation3O4@mC is dispersed in water, and the EGTA solution prepared is added, adds
Heat simultaneously stirs, wherein Fe3O4The mass ratio of@mC and EGTA are 2:1-1:10, react 1-8h, obtain the absorption of EGTA modified magnetic charcoal
Agent；EGTA modified magnetic carbon adsorbent is washed, dried and ground.
Wherein, water used generally uses the higher water of purity, generally uses ultrapure water；Fe3O4@mC is with magnetic four
Fe 3 O is kernel, and outside coats layer of particles carbon；Fe3O4@mC@EGTA is that magnetic ferroso-ferric oxide is most kernel, intermediate
Layer of particles carbon is coated, outermost layer clad is EGTA, since EGTA is a kind of strong complexing agent, can be formed and be tied with various heavy
The stable complex of structure, can play good removal effect in middle low concentration heavy metal water；Have to heavy metal very strong
Suction-operated, when being grafted to Fe3O4When in the particulate carbon of@mC, it is grafted on Fe3O4The EGTA counterweight on the surface@mC@EGTA
Metal ion is adsorbed, i.e., carries out chelating with heavy metal ion and adsorbed；And Fe simultaneously3O4To be magnetic, when application magnetic field
When, it can be adsorbed.And in preparation method, preparation condition is simple, reaction is mild, energy saving, preparation period is short, at low cost,
Preferable economic benefit can be obtained.
EGTA modified magnetic carbon adsorbent (the i.e. Fe of preparation3O4@mC@EGTA), property is stablized, and adsorption effect is good, absorption
Capacity is big, and removal of heavy metal ions rate is high, and the stability of absorption is strong, magnetic recovery and can repeatedly utilize.
Specific embodiment 1
A kind of preparation method of EGTA modified magnetic carbon adsorbent, method include:
Fe3O4The preparation of powder:
Take 8.115gFeCl3·6H2O and 2.984gFeCl2·4H2O is dissolved in 250mL water, and mixed solution is transferred to
In 500mL three-necked flask, stir evenly；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 70 DEG C of water-bath, stirring, 12.5mL concentration, which is added dropwise, is
25% ammonium hydroxide reacts 1h, obtains Fe3O4；
By Fe3O4It is transferred in beaker with pure water 3 times to neutrality, supernatant liquor is toppled over magnet separation, at 70 DEG C
Under the conditions of be dried in vacuo 8 hours, it is spare；
The preparation of EGTA solution:
0.1gNaOH is added in 250mL beaker and is dissolved in 120mL pure water, then weighs 0.5gEGTA powder and configuration completion is added
NaOH weak solution in, be made EGTA solution, it is spare；
Fe3O4The preparation of@mC: by the Fe of preparation3O4Powder is added in pure water, ultrasonic disperse 10min, adds after ultrasonic disperse
Enter to being introduced into 80mL glucose solution, Fe3O4Powder and glucose quality ratio are 1:15, Fe3O4It is mixed with glucose solution super
Sound disperses 5min, reacts 4h at a temperature of 180 DEG C, obtains Fe3O4@mC；It will obtain Fe3O4@mC carries out water and dehydrated alcohol is washed
It washs, dries 8h at 50 °C, grind 10min with agate mortar after drying；
Fe3O4The activation of@mC: the Fe that 0.5g preparation is completed3O4@mC is added into 250mL beaker, and 7.5mL30% is added
H2O2In solution after ultrasonic activation 30min, with pure water 5 times；
Fe3O4The preparation of@mC@EGTA: by the Fe of activation3O4@mC is scattered in 60mL pure water, in 50 DEG C of bath temperatures, is stirred
Mixing speed is that Fe is added dropwise with the speed of 5mL/min in EGTA solution under 180rpm3O4In@mC dispersion, wherein
Fe3O4The mass ratio of@mC and EGTA are 1:8, react 8h, obtain EGTA modified magnetic carbon adsorbent；EGTA modified magnetic charcoal is inhaled
Attached dose, with pure water 3 times, is placed in 50 DEG C of baking ovens dry 8h, grinds 10min with agate mortar after drying.
Specific embodiment 2
A kind of preparation method of EGTA modified magnetic carbon adsorbent, method include:
Fe3O4The preparation of powder:
Taking the ratio between amount of substance is the FeCl of 2:13·6H2O and FeCl2·4H2O is dissolved in the water, and stirs evenly, and obtains
Mixed solution；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 60 DEG C of water-bath, stirring, it is 25% that concentration, which is added dropwise,
Ammonium hydroxide reacts 2h, obtains Fe3O4；
By Fe3O4It is washed with water to neutrality, is dried in vacuo 12h under conditions of 50 DEG C, obtains Fe3O4Powder, it is spare；
The preparation of EGTA solution:
In NaOH solution, EGTA powder is added, wherein the mass ratio of NaOH and EGTA is 1:4, and EGTA solution is made, standby
With；
Fe3O4The preparation of@mC: by the Fe of preparation3O4Powder is added to the water, ultrasonic disperse 20min, is added after ultrasonic disperse
Into 0.4mol/L glucose solution, Fe3O4Powder and glucose quality ratio are 1:30, Fe3O4Ultrasound is mixed with glucose solution
Disperse 5min, reacts 6h at a temperature of 160 DEG C, obtain Fe3O4@mC；It will obtain Fe3O4@mC carries out water and dehydrated alcohol washing,
It is dry at a temperature of 70 DEG C, then grind.
Fe3O4The activation of@mC: by Fe3O4The H that it is 15% to concentration that@mC, which is added,2O2In solution, every gram of Fe3O4@mC powder adds
Enter 30mL H2O2Solution, ultrasonic disperse 15min, to Fe3O4@mC is activated；
Fe3O4The preparation of@mC@EGTA: by the Fe of activation3O4@mC is dispersed in water, in 70 DEG C of bath temperatures, mixing speed
For the EGTA solution prepared under 200rpm, is added, wherein Fe3O4The mass ratio of@mC and EGTA are 2:1, react 3h, obtain
EGTA modified magnetic carbon adsorbent；EGTA modified magnetic carbon adsorbent is washed, dried and ground.
Specific embodiment 3
A kind of preparation method of EGTA modified magnetic carbon adsorbent, method include:
Fe3O4The preparation of powder:
Taking the ratio between amount of substance is the FeCl of 2:13·6H2O and FeCl2·4H2O is dissolved in the water, and stirs evenly, and obtains
Mixed solution；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 80 DEG C of water-bath, stirring, it is 25% that concentration, which is added dropwise,
Ammonium hydroxide reacts 1h, obtains Fe3O4；
By Fe3O4It is washed with water to neutrality, is dried in vacuo 6h under conditions of 80 DEG C, obtains Fe3O4Powder, it is spare；
The preparation of EGTA solution:
In NaOH solution, EGTA powder is added, wherein the mass ratio of NaOH and EGTA is 1:3, and EGTA solution is made, standby
With；
Fe3O4The preparation of@mC: by the Fe of preparation3O4Powder is added to the water, ultrasonic disperse 10min, is added after ultrasonic disperse
Into 0.8mol/L glucose solution, Fe3O4Powder and glucose quality ratio are 1:5, Fe3O4Ultrasound is mixed with glucose solution
Disperse 15min, reacts 2h at a temperature of 200 DEG C, obtain Fe3O4@mC；It will obtain Fe3O4@mC carries out water and dehydrated alcohol washing,
It is dry at a temperature of 60 DEG C, then grind.
Fe3O4The activation of@mC: by Fe3O4The H that it is 25% to concentration that@mC, which is added,2O2In solution, every gram of Fe3O4@mC powder adds
Enter 20mL H2O2Solution, ultrasonic disperse 30min, to Fe3O4@mC is activated；
Fe3O4The preparation of@mC@EGTA: by the Fe of activation3O4@mC is dispersed in water, in 80 DEG C of bath temperatures, mixing speed
For the EGTA solution prepared under 100rpm, is added, wherein Fe3O4The mass ratio of@mC and EGTA are 1:10, react 1h, obtain
EGTA modified magnetic carbon adsorbent；EGTA modified magnetic carbon adsorbent is washed, dried and ground.
Specific embodiment 4
A kind of preparation method of EGTA modified magnetic carbon adsorbent, method include:
Fe3O4The preparation of powder:
Taking the ratio between amount of substance is the FeCl of 2:13·6H2O and FeCl2·4H2O is dissolved in the water, and stirs evenly, and obtains
Mixed solution；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 65 DEG C of water-bath, stirring, it is 25% that concentration, which is added dropwise,
Ammonium hydroxide reacts 1.5h, obtains Fe3O4；
By Fe3O4It is washed with water to neutrality, is dried in vacuo 10h under conditions of 70 DEG C, obtains Fe3O4Powder, it is spare；
The preparation of EGTA solution:
In NaOH solution, EGTA powder is added, wherein the mass ratio of NaOH and EGTA is 1:2, and EGTA solution is made, standby
With；
Fe3O4The preparation of@mC: by the Fe of preparation3O4Powder is added to the water, ultrasonic disperse 15min, is added after ultrasonic disperse
Into 0.6mol/L glucose solution, Fe3O4Powder and glucose quality ratio are 1:20, Fe3O4Ultrasound is mixed with glucose solution
Disperse 10min, reacts 10h at a temperature of 120 DEG C, obtain Fe3O4@mC；It will obtain Fe3O4@mC carries out water and dehydrated alcohol is washed
It washs, it is dry at a temperature of 55 DEG C, then grind.
Fe3O4The activation of@mC: by Fe3O4The H that it is 20% to concentration that@mC, which is added,2O2In solution, every gram of Fe3O4@mC powder adds
Enter 25mL H2O2Solution, ultrasonic disperse 20min, to Fe3O4@mC is activated；
Fe3O4The preparation of@mC@EGTA: by the Fe of activation3O4@mC is dispersed in water, in 60 DEG C of bath temperatures, mixing speed
For the EGTA solution prepared under 150rpm, is added, wherein Fe3O4The mass ratio of@mC and EGTA are 1:3, react 5h, obtain
EGTA modified magnetic carbon adsorbent；EGTA modified magnetic carbon adsorbent is washed, dried and ground.
Specific embodiment 5
A kind of preparation method of EGTA modified magnetic carbon adsorbent, method include:
Fe3O4The preparation of powder:
Taking the ratio between amount of substance is the FeCl of 2:13·6H2O and FeCl2·4H2O is dissolved in the water, and stirs evenly, and obtains
Mixed solution；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 75 DEG C of water-bath, stirring, it is 25% that concentration, which is added dropwise,
Ammonium hydroxide reacts 1.8h, obtains Fe3O4；
By Fe3O4It is washed with water to neutrality, is dried in vacuo 8h under conditions of 50-80 DEG C, obtains Fe3O4Powder, it is spare；
The preparation of EGTA solution:
In NaOH solution, EGTA powder is added, wherein the mass ratio of NaOH and EGTA is 1:1, and EGTA solution is made, standby
With；
Fe3O4The preparation of@mC: by the Fe of preparation3O4Powder is added to the water, ultrasonic disperse 14min, is added after ultrasonic disperse
Into 0.6mol/L glucose solution, Fe3O4Powder and glucose quality ratio are 1:15, Fe3O4Ultrasound is mixed with glucose solution
Disperse 8min, reacts 8h at a temperature of 140 DEG C, obtain Fe3O4@mC；It will obtain Fe3O4@mC carries out water and dehydrated alcohol washing,
It is dry at a temperature of 65 DEG C, then grind；
Fe3O4The activation of@mC: by Fe3O4The H that it is 15% to concentration that@mC, which is added,2O2In solution, every gram of Fe3O4@mC powder adds
Enter 30mL H2O2Solution, ultrasonic disperse 18min, to Fe3O4@mC is activated；
Fe3O4The preparation of@mC@EGTA: by the Fe of activation3O4@mC is dispersed in water, in 55 DEG C of bath temperatures, mixing speed
For the EGTA solution prepared under 120rpm, is added, wherein Fe3O4The mass ratio of@mC and EGTA are 1:5, react 7h, obtain
EGTA modified magnetic carbon adsorbent；EGTA modified magnetic carbon adsorbent is washed, dried and ground.
The EGTA modified magnetic carbon adsorbent of specific embodiment 1-5 preparation, i.e. Fe3O4@mC@EGTA adsorbent is applied,
And the result after application is measured.
The application method of EGTA modified magnetic carbon adsorbent, EGTA modified magnetic carbon adsorbent and heavy metal wastewater thereby obtained
Mixing after reacting 12h in 25 DEG C of gas bath shaking tables, applies magnetic field to mixed system after reaction, will be adsorbed with the magnetism of heavy metal
Adsorbent is separated with aqueous solution；Wherein, EGTA modified magnetic carbon adsorbent is reacted with heavy metal wastewater thereby and is essentially
EGTA and heavy metal ion form complex compound or chelate, achieve the purpose that purification of waste water.
Application note is specifically carried out to single heavy metal waste water with EGTA modified magnetic carbon adsorbent prepared by embodiment 1.
Using 1: the EGTA modified magnetic carbon adsorbent 20mg prepared with embodiment 1 is weighed in 250mL conical flask, to cone
The lead (II) ion waste water that 100mL20mg/L is added in shape bottle, after reacting 12h in 25 DEG C of gas bath shaking tables, Magnetic Isolation is obtained
Treated water, wherein the concentration of remaining lead (II) ion is 0.1474mg/L, removal rate 99.09%, the suction of the material
Attached capacity is 99.09mg/g.
Using 2: the EGTA modified magnetic carbon adsorbent 20mg prepared with embodiment 1 is weighed in 250mL conical flask, to cone
The lead (II) ion waste water that 100mL60mg/L is added in shape bottle, after reacting 12h in 25 DEG C of gas bath shaking tables, Magnetic Isolation is obtained
Treated water, wherein the concentration of remaining lead (II) ion is 29.3766mg/L, removal rate 52.11%, the suction of the material
Attached capacity is 156.33mg/g.
Using 3: the EGTA modified magnetic carbon adsorbent 20mg prepared with embodiment 1 is weighed in 250mL conical flask, to cone
The divalent cadmium ion waste water that 100mL10mg/L is added in shape bottle, after reacting 12h in 25 DEG C of gas bath shaking tables, Magnetic Isolation is obtained
Treated water, wherein the concentration of remaining divalent cadmium ion is that Atomic absorption can not detect, removal rate is almost 100%.
When EGTA modified magnetic carbon adsorbent prepared by embodiment 1 carries out Adsorption to single heavy metal ion, go
Except rate is very high, especially for the lower waste liquid of concentration, removal rate almost can achieve 100%, and adsorption capacity is high, absorption
Capacity can achieve 156.33mg/g.
Using 4: same application method is applied embodiment 1-5 to mixture-metal waste liquid, by the EGTA of 20mg
Modified magnetic carbon adsorbent be added to 100mL cupric, lead, zinc, iron, nickel, cadmium mixture-metal waste liquid in heavy metal ion
It is adsorbed, wherein the concentration of the every metal ion species of copper, lead, zinc, iron, nickel, cadmium is 5mg/L, to various heavy before purifying
Concentration is measured respectively, then is measured to more metal concentrations after absorption, and calculates total removal rate and comprehensive adsorption capacity,
Application the result is as follows:
As seen from the above table: when carrying out Adsorption to multi-metal system waste liquid, total removal rate can achieve 99% or more,
And its adsorption capacity, in 148mg/g or more, removal rate is high, and adsorption capacity is big, and adsorbent property is stablized, and adsorption effect is good.
And this EGTA modified magnetic carbon adsorbent had not only had the good heavy metal chelating ability of EGTA, but also had magnetic material
Segregative characteristic can be recycled for multiple times in practical application.
The steps in the embodiment of the present invention can be sequentially adjusted, merged and deleted according to actual needs.
It is described in detail herein, applies specific case and the principle of the present invention and embodiment are explained
It states, above embodiments are merely used to help understand method and its core concept of the invention；Meanwhile for the general skill of this field
Art personnel, according to the thought of the present invention, there will be changes in the specific implementation manner and application range, in conclusion this
Description should not be construed as limiting the invention.
It is apparent to those skilled in the art that for convenience and simplicity of description, the system of foregoing description
It with the specific work process of unit, can refer to corresponding processes in the foregoing method embodiment, details are not described herein.
Claims (10)
1. a kind of preparation method of EGTA modified magnetic carbon adsorbent, which is characterized in that method includes:
S1. by Fe3O4Powder is added to the water, and is added after ultrasonic disperse into glucose solution, reacts at a temperature of 120-200 DEG C
1-10h obtains Fe3O4@mC；
S2. by Fe3O4@mC is added to H2O2In solution, ultrasonic disperse, to Fe3O4@mC is activated；
S3. by the Fe of activation3O4@mC is dispersed in water, and EGTA solution is added, heats and be stirred to react 1-8h, and it is modified to obtain EGTA
Magnetic carbon adsorbent.
2. preparation method according to claim 1, which is characterized in that the Fe in the step S13O4Powder preparation method
Are as follows:
Taking the ratio between amount of substance is the FeCl of 2:13·6H2O and FeCl2·4H2O is dissolved in the water, and stirs evenly, and obtains mixing molten
Liquid；
Under nitrogen atmosphere, under conditions of mixed solution being placed in 60-80 DEG C of water-bath, stirring is slowly added to ammonium hydroxide, reacts 1-
2h obtains Fe3O4；
By Fe3O4It is washed with water to neutrality, is dried in vacuo 6-12h under conditions of 50-80 DEG C, obtains Fe3O4Powder.
3. preparation method according to claim 1, which is characterized in that the EGTA solution manufacturing method in the step S3
Are as follows:
In NaOH solution, EGTA powder is added, EGTA solution is made.
4. preparation method according to claim 1, which is characterized in that after the step S1, before step S2 further include:
The Fe that will be obtained3O4@mC carries out water and dehydrated alcohol washing, dry and grinding.
5. preparation method according to claim 1, which is characterized in that after the step S3 further include:
EGTA modified magnetic carbon adsorbent is washed, dried and ground.
6. preparation method according to claim 1, which is characterized in that the step S1 specifically:
By Fe3O4Powder is added in pure water, and the Fe into glucose solution is added after ultrasonic disperse3O4Powder and glucose quality ratio
For 1:(5-30), Fe3O4With glucose solution mixing ultrasonic disperse 5-15min, 1-10h is reacted at a temperature of 120-200 DEG C, is obtained
To Fe3O4@mC。
7. preparation method according to claim 1, which is characterized in that the step S2 specifically:
By Fe3O4The H that it is 15-30% to concentration that@mC, which is added,2O2In solution, ultrasonic disperse 10-30min, to Fe3O4@mC lives
Change.
8. preparation method according to claim 1, which is characterized in that the step S3 specifically:
By the Fe of activation3O4@mC is scattered in pure water, and EGTA solution is added, heats and stirs, wherein Fe3O4@mC's and EGTA
Mass ratio is (2:1)-(1:10), reacts 1-8h, obtains EGTA modified magnetic carbon adsorbent after washing is dry.
9. a kind of EGTA modified magnetic carbon adsorbent, which is characterized in that the adsorbent is -8 any described according to claim 1
Method is made.
10. a kind of application method of EGTA modified magnetic carbon adsorbent, which is characterized in that method are as follows:
EGTA modified magnetic carbon adsorbent made from any method of claim 1-8 is mixed instead with heavy metal wastewater thereby
It answers, magnetic field is applied to mixed system after reaction, the magnetic adsorbent for being adsorbed with heavy metal is separated with aqueous solution.
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