CN108187623A - A kind of preparation method for effectively removing the green composite Nano magnetic material of heavy metal in environment - Google Patents
A kind of preparation method for effectively removing the green composite Nano magnetic material of heavy metal in environment Download PDFInfo
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- CN108187623A CN108187623A CN201810170801.0A CN201810170801A CN108187623A CN 108187623 A CN108187623 A CN 108187623A CN 201810170801 A CN201810170801 A CN 201810170801A CN 108187623 A CN108187623 A CN 108187623A
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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
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Abstract
A kind of preparation method for effectively removing the green composite Nano magnetic material of heavy metal in environment.The present invention relates to environmental functional Material Field, more particularly to a kind of preparation method of composite Nano magnetic material.Material after composite process is cumbersome after being modified the present invention is to solve current charcoal, expensive starting materials are modified or modify simultaneously still has the technical problems such as risk of certain secondary environmental pollution.Method：1st, biomass castoff pre-processes；2nd, thermal transition of the biomass to charcoal；3rd, charcoal and ferric iron are mixed in the liquid phase；4th, suspension is subjected to reduction reaction using liquid phase deposition, obtains the carbon material of load nano zero valence iron, rinsed, filtered, drying obtains green composite Nano magnetic material.The present invention is used to remove heavy metal in environment.In a short time, there is preferable removal ability to 6 heavy metal species common in environment, removal efficiency has higher magnetism up to more than 95%, conducive to recycling.
Description
Technical field
The present invention relates to environmental functional Material Field, more particularly to a kind of preparation side of composite Nano magnetic material
Method.
Background technology
In recent years, it due to a large amount of discharges of trade effluent, wherein a large amount of heavy metal contaminants enter in environment, is such as not added with
With processing, permanent toxic effect can be caused to organism.Currently used chemical method cost is higher, and the biological prosthetic period
It is longer to be unfavorable for the short time discharge of heavy metal is controlled.On a large scale should in terms of water process due to artificial swamp in the recent period
With and sponge city propulsion, a large amount of plant waste removes division ring as green bio matter raw material to prepare low-cost sorbent
Heavy metal in border becomes recent science hot spot, has the characteristics that at low cost, secondary environmental pollution risk is low.By biomass
The technology that pyrolysis prepares charcoal can realize the removal of heavy metal effectively under the conditions of low cost, but its there are the problem of mainly wrap
It includes：First, specific surface area is smaller, and saturated extent of adsorption is relatively low；2nd, charcoal relies primarily on physical absorption and removes removing heavy metals, causes
Removal rates are relatively low, can not quickly collect the heavy metal in environment.And modification or modification side currently for cheap biological carbon materials
Material after the big multi-method of method is cumbersome, expensive starting materials are modified or modify simultaneously still has the risk of certain secondary environmental pollution.
The problem present on limits the application of cheap green bio Carbon Materials.
Invention content
Composite process is cumbersome after being modified the present invention is to solve current charcoal, expensive starting materials are modified simultaneously or modify
The still technical problems such as risk with certain secondary environmental pollution of material afterwards, and one kind is provided and effectively removes a huge sum of money in environment
The preparation method of the green composite Nano magnetic material of category.
The present invention it is a kind of effectively remove the green composite Nano magnetic material of heavy metal in environment preparation method be specifically
It carries out according to the following steps：
First, biomass castoff is crushed into processing, and ultrapure water is used 2~3 times after crossing 30~50 mesh sieve,
Temperature is dried under conditions of being 30~50 DEG C, obtains biomass castoff powder；
2nd, biomass castoff powder is placed on quartz boat, the quartz boat for being loaded with biomass castoff powder is shifted
It is pyrolyzed into tubular type pyrolysis oven, pyrolysis temperature is risen to 550~650 from room temperature with the heating rate of 10~20 DEG C/min
DEG C, in temperature to stop 60~120min under conditions of 550~650 DEG C, nitrogen is continually fed into tubular type pyrolysis oven in pyrolytic process
Gas takes out quartz boat after the completion of pyrolysis from tubular type pyrolysis oven, obtains biological carbon feedstock；
3rd, by biological carbon feedstock using being put into FeCl after ultrapure water 2~3 times3After being mixed in solution, in room temperature condition
2.5~3.5h of lower stirring, obtains suspension；The FeCl3In solution the volume ratio of iron ion and biological carbon feedstock for (5~
45):27；
4th, the pH of suspension is adjusted to 2~7, then thereto with 20 under conditions of magnetic agitation and nitrogen protection
The speed of~60 drops/min instills NaBH4Solution, carries out separation of solid and liquid by filtering technology after reaction, and obtained solid exists
Drying and processing under nitrogen environment is then ground to obtain charcoal composite Nano magnetic material；Iron ion in the suspension
With NaBH4The molar ratio of solution is 1:(1.5~2).
Beneficial effects of the present invention：
The method of the present invention is simple, and raw material sources are extensive, at low cost, and energy consumption is few.Green composite Nano magnetic material is in environment
In terms of heavy metals removal there is vast application prospect, 60~99% are reached for 6 heavy metal species removal rates of 50mg/L concentration.
The risk of secondary pollution will not be caused to environment, and without complicated special instrument and equipment.
Description of the drawings
Fig. 1 is the low power scanning electron microscope (SEM) photograph of charcoal composite Nano magnetic material that embodiment two obtains；
Fig. 2 is the high power scanning electron microscope (SEM) photograph of charcoal composite Nano magnetic material that embodiment two obtains；
Fig. 3 is that the magnetic hysteresis for the charcoal composite Nano magnetic material that embodiment one, embodiment two and embodiment three obtain is bent
Line；Wherein 1 is embodiment one, and 2 be embodiment two, and 3 be embodiment three；
Fig. 4 is that the charcoal composite Nano magnetic material obtained using embodiment two is adsorbed front and rear liquid-phase collection photograph
Piece；Before wherein heavy metal ion is adsorbed in left side for adsorbent, after heavy metal ion is adsorbed in right side completely for adsorbent；
Fig. 5 is the obtained charcoal composite Nano magnetic material of embodiment two for 6 heavy metal species common in environment
Removal efficiency；Wherein A is single metallic solution, and B is mixed metal solution.
Specific embodiment
Specific embodiment one：Biomass castoff is crushed processing by present embodiment one, and crosses 30~50 mesh sieve
Ultrapure water is used afterwards 2~3 times, dried under conditions of being 30~50 DEG C in temperature, obtain biomass castoff powder；
2nd, biomass castoff powder is placed on quartz boat, the quartz boat for being loaded with biomass castoff powder is shifted
It is pyrolyzed into tubular type pyrolysis oven, pyrolysis temperature is risen to 550~650 from room temperature with the heating rate of 10~20 DEG C/min
DEG C, in temperature to stop 60~120min under conditions of 550~650 DEG C, nitrogen is continually fed into tubular type pyrolysis oven in pyrolytic process
Gas takes out quartz boat after the completion of pyrolysis from tubular type pyrolysis oven, obtains biological carbon feedstock；
3rd, by biological carbon feedstock using being put into FeCl after ultrapure water 2~3 times3After being mixed in solution, in room temperature condition
2.5~3.5h of lower stirring, obtains suspension；The FeCl3In solution the volume ratio of iron ion and biological carbon feedstock for (5~
45):27；
4th, the pH of suspension is adjusted to 2~7, then thereto with 20 under conditions of magnetic agitation and nitrogen protection
The speed of~60 drops/min instills NaBH4Solution, carries out separation of solid and liquid by filtering technology after reaction, and obtained solid exists
Drying and processing under nitrogen environment is then ground to obtain charcoal composite Nano magnetic material；Iron ion in the suspension
With NaBH4The molar ratio of solution is 1:(1.5~2).
The purpose of processing of pulverizing and sieving in present embodiment step 1 is to speed up the pyrolytic process of biomass, improves charcoal
Specific surface area, dispersibility and thermal conduction rate, while improve the uniformity of composite material in step 4.
It is for abundant carbonated material to be heated up in present embodiment step 2 with 15 DEG C/min heating rates；In pyrolytic process
Nitrogen is passed through, biomass is on the one hand made fully to be cracked under oxygen-free environment, so as to utmostly utilize carbon therein.
Biological carbon feedstock is put into FeCl by present embodiment step 33Mixed in solution, it is therefore an objective to make biological carbon surface with
Fe3+It comes into full contact with, and is evenly distributed on its surface, the nano-particle that raising is subsequently prepared is in the dispersibility of biological carbon surface.
Present embodiment step 4 makes nanometer nulvalent iron particle slowly be given birth in biological carbon surface by liquid-phase reduction sedimentation
It is long, with the Organic functional groups on its surface to be chemically bound together.
Green composite Nano magnetic material prepared by present embodiment the method for the present invention is used to remove weight common in environment
Metal pollutant, this method first pre-processes biomass castoff (reed stalk), and is carried out pyrolysis processing, passes through
FeCl3Solution is mixed with charcoal, makes biological carbon surface and Fe3+It comes into full contact with, and is evenly distributed on its surface, improve
The nano-particle subsequently prepared is in the dispersibility of biological carbon surface；Make nanometer nulvalent iron particle finally by liquid-phase reduction sedimentation
It is slowly grown in biological carbon surface, the Organic functional groups with its surface not only make charcoal table to be chemically bound together
One layer of nano zero valence iron of face uniform load, while the degree of scatter of nano-particle is improved using the porosity of charcoal, from
And improve its reactivity；Green composite Nano magnetic material has 6 kinds of environment common heavy metals higher removal energy
Power, while there is higher magnetism, conducive to recycling.
The FeCl3Solution allocation method is as follows：Under the conditions of pH is 4~5, iron chloride is dissolved in ultra-pure water, is configured
Into ferric chloride solution.
Specific embodiment two：The present embodiment is different from the first embodiment in that：Biomass described in step 1
Waste is reed rod.It is other same as the specific embodiment one.
Specific embodiment three：The present embodiment is different from the first and the second embodiment in that：40 mesh are crossed in step 1
Ultrapure water is used after sieve 2~3 times.It is other the same as one or two specific embodiments.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：In step 1
Temperature is dried under conditions of being 40 DEG C.It is other identical with one of specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：In step 2 with
Pyrolysis temperature is risen to 600 DEG C by the heating rate of 15 DEG C/min from room temperature.It is other identical with one of specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：In step 2
Temperature stops 90min under conditions of being 600 DEG C.It is other identical with one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Nitrogen in step 2
Gas is passed through rate as 200mL/min.It is other identical with one of specific embodiment one to six.
Present embodiment is passed through nitrogen with the rate of 200mL/min can more efficiently utilize inert gas.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Institute in step 3
State FeCl3The volume ratio of iron ion and biological carbon feedstock is (10~40) in solution:27.Other and specific embodiment one to seven
One of it is identical.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：It will in step 4
The pH of suspension is adjusted to 3~6.It is other identical with one of specific embodiment one to eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：In step 4
NaBH is instilled with the speed of 30~50 drops/min thereto under conditions of magnetic agitation and nitrogen protection4Solution；The suspension
Middle iron ion and NaBH4The molar ratio of solution is 1:1.6.It is other identical with one of specific embodiment one to nine.
Beneficial effects of the present invention are verified by following embodiment：
Embodiment one：A kind of preparation method for effectively removing the green composite Nano magnetic material of heavy metal in environment is specific
It is to carry out according to the following steps：
First, biomass castoff is crushed into processing, and ultrapure water is used 2~3 times after crossing 40 mesh sieve, in temperature
It is dried under conditions of being 40 DEG C, obtains biomass castoff powder；
2nd, biomass castoff powder is placed on quartz boat, the quartz boat for being loaded with biomass castoff powder is shifted
It is pyrolyzed into tubular type pyrolysis oven, pyrolysis temperature is risen to 600 DEG C from room temperature with the heating rate of 15 DEG C/min, is in temperature
It stops 90min under conditions of 600 DEG C, nitrogen is continually fed into tubular type pyrolysis oven in pyrolytic process, from tubular type heat after the completion of pyrolysis
Quartz boat is taken out in solution stove, obtains biological carbon feedstock；Nitrogen is passed through rate as 200mL/min；
3rd, by 0.5g biologies carbon feedstock using being put into FeCl after ultrapure water 2~3 times3After being mixed in solution, in room temperature
Under the conditions of stir 3h, obtain suspension；The FeCl3The volume ratio of iron ion and biological carbon feedstock is 10 in solution:27；
4th, the pH of suspension is adjusted to 5, then under conditions of magnetic agitation and nitrogen protection thereto with 40 drops/
The speed of min instills NaBH4Solution carries out separation of solid and liquid by filtering technology after reaction, and obtained solid is in nitrogen ring
Drying and processing under border is then ground to obtain charcoal composite Nano magnetic material；Iron ion and NaBH in the suspension4
The molar ratio of solution is 1:1.6.Embodiment two：The present embodiment and embodiment one the difference lies in：Described in step 3
FeCl3The volume ratio of iron ion and biological carbon feedstock is 20 in solution:27.Other are identical with embodiment one.
Embodiment three：The present embodiment and embodiment one the difference lies in：FeCl described in step 33In solution iron from
The volume ratio of son and biological carbon feedstock is 40:27.Other are identical with embodiment one.
Fig. 1 is the low power scanning electron microscope (SEM) photograph of charcoal composite Nano magnetic material that embodiment two obtains；Fig. 2 is embodiment
The two obtained high power scanning electron microscope (SEM) photographs of charcoal composite Nano magnetic material；Fig. 3 is embodiment one, embodiment two and embodiment
The three obtained B-H loops of charcoal composite Nano magnetic material；Wherein 1 is embodiment one, and 2 be embodiment two, and 3 is implement
Example three；Fig. 4 is that the charcoal composite Nano magnetic material obtained using embodiment two is adsorbed front and rear liquid-phase collection photo；Its
Before heavy metal ion is adsorbed in middle left side for adsorbent, after heavy metal ion is adsorbed in right side completely for adsorbent；It can from Fig. 1 and Fig. 2
To find out, biological carbon materials area load one layer of nanometer nulvalent iron particle, size pass through chemistry between 100~200nm
Key is closely linked, and is evenly distributed in around surface and gap.By Fig. 3 and Fig. 4 it is found that present embodiment obtained
Material has higher magnetism (30~50emu/g), and is easily recycled from liquid phase.Fig. 5 is what embodiment two obtained
Charcoal composite Nano magnetic material is for the removal efficiency of 6 heavy metal species common in environment；The initial concentration of heavy metal is
50mg/L；Wherein A is single metallic solution, and B is mixed metal solution, and the single metallic solution is Pb2+、Cd2+、Cr6+、Cu2 +、Ni2+Or Zn2+Single solution；The mixed metal solution is Pb2+、Cd2+、Cr6+、Cu2+、Ni2+And Zn2+Mixed solution；
The green composite Nano magnetic material that present embodiment obtains has good removal energy for 6 common heavy metal species of environment
Power.Concrete operations for the removal of heavy metal in environment are that 0.05g biological carbon materials are added to a concentration of 50mg/L of 25mL
Heavy metal solution in, and vibrated 24 hours at 30 DEG C.After reaction, the charcoal in solid slurry is removed with magnet,
And then 10mL samples are determined the sample of filtering by analyzing ICP-AES residual by one 0.22 micron of filter
Remaining heavy metal concentration.Heavy metal solution is single metallic solution or mixed metal solution.
Claims (10)
1. a kind of preparation method for effectively removing the green composite Nano magnetic material of heavy metal in environment, it is characterised in that effectively
The preparation method of the green composite Nano magnetic material of heavy metal specifically carries out according to the following steps in removal environment：
First, biomass castoff is crushed into processing, and ultrapure water is used 2~3 times after crossing 30~50 mesh sieve, in temperature
It is dried under conditions of being 30~50 DEG C, obtains biomass castoff powder；
2nd, biomass castoff powder is placed on quartz boat, the quartz boat for being loaded with biomass castoff powder is transferred to pipe
It is pyrolyzed in formula pyrolysis oven, pyrolysis temperature is risen to 550~650 DEG C from room temperature with the heating rate of 10~20 DEG C/min,
Temperature stops 60~120min under conditions of being 550~650 DEG C, is continually fed into nitrogen in tubular type pyrolysis oven in pyrolytic process, heat
Quartz boat is taken out from tubular type pyrolysis oven after the completion of solution, obtains biological carbon feedstock；
3rd, by biological carbon feedstock using being put into FeCl after ultrapure water 2~3 times3After being mixed in solution, stir at ambient temperature
2.5~3.5h is mixed, obtains suspension；The FeCl3The volume ratio of iron ion and biological carbon feedstock is (5~45) in solution:27；
4th, the pH of suspension is adjusted to 2~7, then thereto with 20~60 under conditions of magnetic agitation and nitrogen protection
The speed of drop/min instills NaBH4Solution carries out separation of solid and liquid by filtering technology after reaction, and obtained solid is in nitrogen
Drying and processing under environment is then ground to obtain charcoal composite Nano magnetic material；In the suspension iron ion with
NaBH4The molar ratio of solution is 1:(1.5~2).
2. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that biomass castoff described in step 1 is reed rod.
3. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that use ultrapure water 2~3 times after 40 mesh sieve is crossed in step 1.
4. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that dried under conditions of being 40 DEG C in temperature in step 1.
5. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that pyrolysis temperature is risen to 600 DEG C from room temperature with the heating rate of 15 DEG C/min in step 2.
6. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that stop 90min under conditions of being 600 DEG C in temperature in step 2.
7. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that nitrogen is passed through rate as 200mL/min in step 2.
8. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that FeCl described in step 33The volume ratio of iron ion and biological carbon feedstock is (10~40) in solution:
27。
9. a kind of preparation for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Method, it is characterised in that adjust the pH of suspension to 3~6 in step 4.
10. a kind of system for effectively removing the green composite Nano magnetic material of heavy metal in environment according to claim 1
Preparation Method, it is characterised in that thereto with the speed of 30~50 drops/min under conditions of magnetic agitation and nitrogen protection in step 4
Degree instills NaBH4Solution；Iron ion and NaBH in the suspension4The molar ratio of solution is 1:1.6.
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| CN109908862A (en) * | 2019-03-18 | 2019-06-21 | 湖南农业大学 | A kind of cadmium pollution renovation agent |
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| CN113185983A (en) * | 2021-05-12 | 2021-07-30 | 湖南省农业环境生态研究所 | Soil conditioner and preparation method and application thereof |
| CN113477214A (en) * | 2021-07-10 | 2021-10-08 | 浙江科技学院 | Preparation method and application of green nano iron-based biomass charcoal adsorption material |
| CN114917869A (en) * | 2022-05-11 | 2022-08-19 | 浙江科技学院 | Preparation method of waste green tea charcoal for preferential adsorption of heavy metals |
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| CN114917869A (en) * | 2022-05-11 | 2022-08-19 | 浙江科技学院 | Preparation method of waste green tea charcoal for preferential adsorption of heavy metals |
| CN114917869B (en) * | 2022-05-11 | 2024-02-13 | 浙江科技学院 | Preparation method of waste green tea biochar for preferential adsorption of heavy metals |
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Application publication date: 20180622 |