CN108479697A - A kind of meso-porous carbon material and its preparation method and application of load Zero-valent Iron - Google Patents

A kind of meso-porous carbon material and its preparation method and application of load Zero-valent Iron Download PDF

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CN108479697A
CN108479697A CN201810234310.8A CN201810234310A CN108479697A CN 108479697 A CN108479697 A CN 108479697A CN 201810234310 A CN201810234310 A CN 201810234310A CN 108479697 A CN108479697 A CN 108479697A
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meso
carbon material
porous carbon
valent iron
solution
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杨志辉
易皓岚
刘维
柴立元
杨卫春
王海鹰
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Central South University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid 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 surface properties or porosity
    • B01J20/28078Pore diameter
    • B01J20/28083Pore diameter being in the range 2-50 nm, i.e. mesopores
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates

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  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of meso-porous carbon materials and its preparation method and application of load Zero-valent Iron, preparation method includes, carbonization after amidin drying containing colloidal silicon dioxide is obtained into meso-porous carbon material, then the meso-porous carbon material for loading Zero-valent Iron in meso-porous carbon material to obtain the final product through sodium borohydride reduction will be added to containing ferric solution under nonoxidizing atmosphere;It is respectively 100 400m that its specific surface area, average pore size and hole, which hold,2/ g, 5 10nm and 0.5 1.0cm3/g;To the eliminating rate of absorption of hexavalent chromium in water body up to 99% or more.The method of the present invention can realize the controlledly synthesis of the meso-porous carbon material of the load Zero-valent Iron to different size by adjusting technological parameter;Its resultant metal iron load factor is high, and stability is strong, and adsorption efficiency is high, and adsorption capacity is big;Preparation condition is mild, simple for process controllable, efficient, is suitble to large-scale production, is widely used.

Description

A kind of meso-porous carbon material and its preparation method and application of load Zero-valent Iron
Technical field
The present invention relates to the sorbing material technical fields handled for heavy metal, and in particular to a kind of Jie of load Zero-valent Iron Hole carbon material and its preparation method and application.
Background technology
In recent years, with increasing, the heavy metal pollution of the exploitation of heavy metal, smelting, processing and business manufacturing activities It is quite serious at present, to the very harmful of environment and biology, meanwhile, heavy metal cannot be biodegradable, and easily pass through food Chain and be enriched with, endanger human health.Therefore, seek suitable method processing heavy metal water body pollution and cause extensive pass Note.Currently, commonly the method for removal Heavy Metals in Waters include chemical precipitation method, ion-exchange, oxidation-reduction method, at film Logos, bioanalysis, absorption method etc., wherein absorption method are that wide method is applied in water process, have adsorbent source it is wide, can Plasticity is strong and simple operation and other advantages.
Meso-porous carbon material is a kind of novel sorbing material, stores height since it is stored with large specific surface area, hole, surface is coagulated The features such as contracting characteristic good, adsorption capacity are strong, thermal stability and chemical stability are strong has in adsorbing separation field and widely answers Use foreground;However, single meso-porous carbon material can not fully meet its particular/special requirement in adsorbing domain sometimes, therefore often need Meso-porous carbon material is modified, better adsorption effect is made it have.Zero-valent Iron has reproducibility, can be extremely strong by toxicity Hexavalent chrome reduction is the weaker trivalent chromic ion of toxicity, but Zero-valent Iron is easily reunited, and is supported in mesoporous carbon, and it is steady that it can be improved It is qualitative.However, up to the present, there is not been reported for the preparation method of the meso-porous carbon material in relation to load Zero-valent Iron.
In conclusion the meso-porous carbon material of load Zero-valent Iron how to be prepared by simple method, and applied It is the current key technical problem for being badly in need of solving in the Adsorption of hexavalent chromium in water body.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of meso-porous carbon materials and preparation method thereof of load Zero-valent Iron And application.
A kind of preparation method of the meso-porous carbon material of load Zero-valent Iron, including following step are provided according to an aspect of the present invention Suddenly:
S1, colloidal silicon dioxide is added in amidin, is dried after stirring evenly, high temperature cabonization, and use successively NaOH solution and deionized water stirring, after cleaning to neutrality, drying meso-porous carbon material;
S2, under nonoxidizing atmosphere, meso-porous carbon material obtained in dispersant PEG-4000 and step S1 is added to and is contained It in ferric solution, stirs evenly, sodium borohydride solution is then added, filtered after being stirred to react, up to negative after washing and drying The meso-porous carbon material of Zero-valent iron-carrying.
In the above-mentioned technical solutions, in step S1, the temperature and time of the high temperature cabonization is respectively 400-600 DEG C and 2- 4h。
Preferably, in the above-mentioned technical solutions, in step S2, described containing ferric solution is Iron(III) chloride hexahydrate Ethanol solution, and the mass ratio of the Iron(III) chloride hexahydrate, mesoporous carbon and PEG-4000 is (6-8):1:(1-3).
In the above-mentioned technical solutions, in step S1, the content of silica is 45- in the colloidal silicon dioxide 55wt%, the feed postition of the colloidal silicon dioxide are to be added dropwise, it is preferable that the rate of addition of the colloidal silicon dioxide For 0.1ml/s.
In the above-mentioned technical solutions, further include the heating hydrotropy solution and NaOH after colloidal silicon dioxide is added in step S1 Heating after solution is added helps cleaning, it is preferable that the heating hydrotropy solution is included at 70-80 DEG C and exists again after stirring 15-30min 15-25min is stirred at 110-125 DEG C, the heating helps cleaning to be stirred at 60-80 DEG C with the NaOH solution of 25-35wt% 15-30min。
In the above-mentioned technical solutions, in step S2, the feed postition of the sodium borohydride solution is to be added dropwise, preferably Ground, the concentration and rate of addition of the sodium borohydride solution are respectively 0.005-0.1g/ml and 0.1ml/s;The sodium borohydride The time that is stirred to react after solution is added is 30-60min.
The meso-porous carbon material for the load Zero-valent Iron that above-mentioned preparation method obtains is provided according to a further aspect of the invention;It is described The specific surface area for loading the meso-porous carbon material of Zero-valent Iron is 100-400m2/ g, average pore size 5-10nm, Kong Rongwei 0.5- 1.0cm3/g。
Answering for the meso-porous carbon material of above-mentioned preparation method or above-mentioned load Zero-valent Iron is provided according to another aspect of the invention With the specifically application in adsorbed water body in hexavalent chromium.
Preferably, the meso-porous carbon material for 25-35mg being loaded to Zero-valent Iron is added to 30ml a concentration of 15- containing hexavalent chromium In the water body of 22mg/L, control water pH value is 2-5, after stirring and adsorbing 5-8h, the eliminating rate of absorption of Cr VI is 99.2 ± 0.4%.
Advantages of the present invention:
(1) present invention only obtains meso-porous carbon material by will be carbonized after the amidin drying for containing colloidal silicon dioxide, It will contain ferric solution under nonoxidizing atmosphere again and be added in meso-porous carbon material and load zeroth order to obtain the final product through sodium borohydride reduction The meso-porous carbon material of iron, and the addition parameter by adjusting colloidal silicon dioxide, high temperature cabonization parameter and contain ferric solution Addition parameter etc., can obtain that different specific surface areas, different pore size, different holes hold and the mesoporous carbon of different Zero-valent Iron load capacity Material, to realize the controlledly synthesis for the meso-porous carbon material for loading Zero-valent Iron;
(2) the metallic iron load factor of the meso-porous carbon material of the load Zero-valent Iron prepared by the present invention is high, and stability is strong, compares table Area is big, and average pore size is small, and hole, which holds, is up to 0.5-1.0cm3/ g, adsorption efficiency is high, and adsorption capacity is big, to a concentration of 15-22mg/ The eliminating rate of absorption of hexavalent chromium in the water body of L is up to 99% or more, can reach national drinking water standard;
(3) the method mild condition of the meso-porous carbon material for the preparation load Zero-valent Iron that the present invention develops, it is simple for process controllable, Product chemistry structure and performance are stablized, and used raw material is easy to get and cheap, and equipment is simple, and production efficiency is high, is suitble to rule Modelling industrial production, and product absorption property is excellent, has a extensive future, theoretical and practical significance is great.
Description of the drawings
A kind of technique stream of the preparation method of the meso-porous carbon material for load Zero-valent Iron that Fig. 1 is provided by the embodiment of the present invention Cheng Tu;
Fig. 2 is the scanning electron microscope (SEM) photograph of the meso-porous carbon material of load Zero-valent Iron prepared in the embodiment of the present invention 1;
Fig. 3 is the energy spectrum diagram of the meso-porous carbon material of load Zero-valent Iron prepared in the embodiment of the present invention 1;
Fig. 4 is the transmission electron microscope picture of the meso-porous carbon material of load Zero-valent Iron prepared in the embodiment of the present invention 1;
Fig. 5 is nitrogen adsorption-desorption isothermal of the meso-porous carbon material of load Zero-valent Iron prepared in the embodiment of the present invention 1 Line chart.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below Example is not limited to protection scope of the present invention for illustrating the present invention, and protection scope of the present invention is with claims It is accurate.
In the examples below, stereoscan photograph and energy spectrum diagram use the JSM-IT300LA scanning electrons with energy disperse spectroscopy Microscope obtains;Nitrogen adsorption-desorption isotherm is obtained using U.S. Mike ASAP 2020, the Adsorption of hexavalent chromium Performance test is measured with diphenyl carbazide spectrophotometry.
Unless otherwise specified, experiment reagent used in the embodiment of the present invention and material etc. are commercially available, if not having Body indicates, the conventional means that technological means used in the embodiment of the present invention is well known to the skilled person.
Embodiment 1
An embodiment of the present invention provides a kind of preparation methods of the meso-porous carbon material of load Zero-valent Iron, as shown in Figure 1, specifically Steps are as follows:
S1,15g starch dissolutions are weighed in 50mL deionized waters, ultrasonic 30min, then by amidin in 80 DEG C of water Heating stirring 20min in bath, then the colloidal silicon dioxide of 20g 50wt% containing silica is added with the speed of 0.1mL/s, with The heating stirring 20min in 120 DEG C of oil baths afterwards is dried after standing cooling, and be carbonized 3h at 500 DEG C, and 100mL is used after natural cooling The NaOH solution of a concentration of 30wt% is cleaned under 70 DEG C of water-baths, is then cleaned again with deionized water until pH value is 7, due to second Alcohol is volatile, more conducively rapid draing, therefore drying for 24 hours, obtains meso-porous carbon material at 60 DEG C after finally cleaning 3 times with ethyl alcohol;
S2, it 0.6g Iron(III) chloride hexahydrates is weighed is dissolved in 120mL volume ratios VEthyl alcohol:VWaterIt is 1:In 5 ethanol water, Mesoporous carbon obtained in 0.3gPEG-4000 and 0.1g steps S1 is added to above-mentioned Iron(III) chloride hexahydrate in a nitrogen atmosphere Ethanol water in, after stirring 60min, then with the speed of 0.1mL/s the solution of 50mL sodium borohydrides containing 0.3362g is added And 60min is stirred, and it then filters, is then cleaned 3 times with ethyl alcohol, it is finally dry for 24 hours to get load zero under 60 DEG C of vacuum conditions The meso-porous carbon material of valence iron.
Sweeping for the meso-porous carbon material of load Zero-valent Iron prepared in the embodiment of the present invention 1 as shown in Figure 2, Figure 3, Figure 4 Electron microscope, energy spectrum diagram and transmission electron microscope picture are retouched, it can be seen from the figure that Zero-valent Iron has successfully loaded in mesoporous carbon;Such as Fig. 5 show the nitrogen adsorption desorption figure of the meso-porous carbon material of load Zero-valent Iron prepared in the embodiment of the present invention 1, can from figure To find out, the nitrogen adsorption desorption curve of the material is IV type curves, illustrates that the meso-porous carbon material of prepared load Zero-valent Iron is Typical mesoporous material.
Embodiment 2
An embodiment of the present invention provides a kind of preparation methods of the meso-porous carbon material of load Zero-valent Iron, are as follows:
S1,15g starch dissolutions are weighed in 50mL deionized waters, ultrasonic 30min, then by amidin in 80 DEG C of water Heating stirring 20min in bath, then the colloidal silicon dioxide of 20g 50wt% containing silica is added with the speed of 0.1mL/s, with The heating stirring 20min in 120 DEG C of oil baths afterwards is dried after standing cooling, and is carbonized at 300 DEG C, 500 DEG C and 700 DEG C respectively 3h is cleaned with the NaOH solution of a concentration of 30wt% of 100mL under 70 DEG C of water-baths after natural cooling, then clear with deionized water again Wash until pH value be 7, since ethyl alcohol is volatile, more conducively rapid draing, therefore after finally clean 3 times with ethyl alcohol at 60 DEG C dry For 24 hours, meso-porous carbon material is obtained;
S2, it 0.6g Iron(III) chloride hexahydrates is weighed is dissolved in 120mL volume ratios VEthyl alcohol:VWaterIt is 1:In 5 ethanol water, Mesoporous carbon obtained in 0.3gPEG-4000 and 0.1g steps S1 is added to above-mentioned Iron(III) chloride hexahydrate in a nitrogen atmosphere Ethanol water in, after stirring 60min, then with the speed of 0.1mL/s the solution of 50mL sodium borohydrides containing 0.3362g is added And 60min is stirred, and it then filters, is then cleaned 3 times with ethyl alcohol, it is finally dry for 24 hours to get load zero under 60 DEG C of vacuum conditions The meso-porous carbon material of valence iron.
It is the result of preparation-obtained meso-porous carbon material BET characterizations under different carburizing temperatures as shown in table 1 below.
The BET characterization result tables of comparisons of the mesoporous carbon obtained under the different carburizing temperatures of table 1
From table 1 it follows that when carburizing temperature is 500 DEG C, the prepared mesoporous carbon large specific surface area arrived, and be situated between Hole number is more.
Embodiment 3
An embodiment of the present invention provides a kind of preparation methods of the meso-porous carbon material of load Zero-valent Iron, are as follows:
S1,15g starch dissolutions are weighed in 50mL deionized waters, ultrasonic 30min, then by amidin in 80 DEG C of water Heating stirring 20min in bath, then the colloidal silicon dioxide of 20g 50wt% containing silica is added with the speed of 0.1mL/s, with The heating stirring 20min in 120 DEG C of oil baths afterwards is dried after standing cooling, and respectively at 300 DEG C, 400 DEG C, 500 DEG C and 600 DEG C Lower carbonization 3h is cleaned with the NaOH solution of a concentration of 30wt% of 100mL under 70 DEG C of water-baths after natural cooling, then spend again from Sub- water cleaning is 7 up to pH value, since ethyl alcohol is volatile, more conducively rapid draing, therefore at 60 DEG C after finally cleaning 3 times with ethyl alcohol Lower drying for 24 hours, obtains meso-porous carbon material;
S2, by mesoporous carbon obtained in step S1 and ferric trichloride mass ratio it is respectively in a nitrogen atmosphere 1:2、1:4、1: 6、1:8 and mesoporous carbon and PEG-4000 mass ratioes be respectively 1:1、1:3、1:5、1:7 carry out orthogonal test, according to embodiment 1 Method, prepare load Zero-valent Iron meso-porous carbon material.
It is 50mg/L, pH value to 30mL initial concentrations using the meso-porous carbon material of the above-mentioned load Zero-valent Iron being prepared Adsorption reaction is carried out containing hexavalent chromium solution for 4, diphenyl carbazide spectrophotometry is used to measure the reaction time as 24 hours The concentration of Cr VI, Orthogonal experiment results are as shown in table 2 below afterwards.
The material obtained under the different preparation conditions of table 2 removes the removal rate of Cr VI
It can be seen from the results in table 2 when carburizing temperature is 500 DEG C, mesoporous carbon is 1 with ferric trichloride mass ratio:(6- 8), the mass ratio of mesoporous carbon and dispersant PEG-4000 are 1:The load Zero-valent Iron obtained under the preparation condition of (1-3) it is mesoporous Carbon material is preferable except Cr VI effect.
Experimental example 1
At ambient temperature, the meso-porous carbon material for weighing the load Zero-valent Iron being prepared in 30mg embodiments 1, to 30mL The hexavalent chromium solution that contains that initial concentration is 20mg/L, pH value is 4 carries out Adsorption reaction, and light is divided using diphenylcarbazide Degree method measure the reaction time be respectively 5min, 15min, 20min, 30min, 40min, 60min, 120min, 180,240min, The concentration of Cr VI when 300min and 360min, as a result as shown in table 3 below.
The 3 differential responses time of table is to the absorption result table of comparisons containing hexavalent chromium solution that initial concentration is 20mg/L
From table 3 it is observed that adsorption time, in 60min, the rate of adsorption of Cr VI is fast, and when reacting 60min, sexavalence Chromium concn falls below 8.18mg/L from 20.00mg/L, and eliminating rate of absorption reaches 61.76%;After adsorbing 60min, the rate of adsorption subtracts Slowly, balance is reached after 6h, its a concentration of 0.17mg/L, removal rate reach 99% at this time.
Experimental example 2
At ambient temperature, the meso-porous carbon material for weighing the load Zero-valent Iron being prepared in 30mg embodiments 1, to 30mL The hexavalent chromium solution that contains that initial concentration is 20mg/L, pH value is respectively 2,3,4,5,6,7,8 and 9 carries out Adsorption reaction, adopts The concentration that the reaction time is rear Cr VI for 24 hours is measured with diphenyl carbazide spectrophotometry, as a result as shown in table 4 below.
The different initial pH values of table 4 are to the absorption result table of comparisons containing hexavalent chromium solution that initial concentration is 20mg/L
Cr VI initial concentration is can be seen that under low consistency conditions from the result in table 4, loads the mesoporous carbon of Zero-valent Iron The absorption property of material removal rate under acid or alkaline environment reaches 96% or more, and the pH value of hexavalent chromium solution is to loading zeroth order The influence of the meso-porous carbon material adsorption effect of iron is little.
Experimental example 3
At ambient temperature, the meso-porous carbon material for weighing the load Zero-valent Iron being prepared in 30mg embodiments 1, to 30mL PH value be 4 and initial concentration be respectively 21.39mg/L, 39.95mg/L, 77.57mg/L, 103.83mg/L, 149.19mg/L, 205.17mg/L's and 290.89mg/L carries out Adsorption reaction containing hexavalent chromium solution, using diphenylcarbazide spectrophotometric Method measures the concentration that the reaction time is rear Cr VI for 24 hours, as a result as shown in table 5 below.
The absorption result table of comparisons containing hexavalent chromium solution of the different initial concentrations of table 5
As can be seen from Table 5, the meso-porous carbon material for loading Zero-valent Iron is high to the hexavalent chromium solution adsorption rate of low concentration, inhales Attached effect is good, and when hexavalent chromium solution initial concentration is 21.39mg/L, material adsorption rate reaches 100%, from adsorpting data result Analysis show that the maximal absorptive capacity of the meso-porous carbon material of load Zero-valent Iron can reach 140mg/g.
Experimental example 4
At ambient temperature, weigh respectively the load Zero-valent Iron being prepared in 30mg embodiments 1 meso-porous carbon material, The commercially available Zero-valent Iron of meso-porous carbon material and 30mg that step S1 is prepared in 30mg embodiments 1, it is 4 to 30mL pH value and initial Concentration is respectively 20mg/L, 40mg/L, 80mg/L, 100mg/L, 150mg/L, 200mg/L and 300mg/L containing hexavalent chromium solution Adsorption reaction is carried out, uses the diphenyl carbazide spectrophotometry measurement reaction time for the concentration of rear Cr VI for 24 hours, Adsorption result is as shown in table 6 below.
The absorption result table of comparisons containing hexavalent chromium solution of the different sorbing materials of table 6 to different initial concentrations
As can be seen from Table 6, mesoporous carbon is prepared compared with the meso-porous carbon material of Zero-valent Iron and load Zero-valent Iron Effect when composite material is better than exclusive use mesoporous carbon to the Cr VI absorption property of solution, Zero-valent Iron is adsorbed, bears The meso-porous carbon material of Zero-valent iron-carrying adsorption rate when hexavalent chromium solution initial concentration is 21.39mg/L can reach 99.99%.
Finally, the preferred embodiment that these are only the present invention, is not intended to limit the scope of the present invention.It is all this Within the spirit and principle of invention, any modification, equivalent replacement, improvement and so on should be included in the protection model of the present invention Within enclosing.

Claims (10)

1. a kind of preparation method of the meso-porous carbon material of load Zero-valent Iron, which is characterized in that include the following steps:
S1, colloidal silicon dioxide is added in amidin, is dried after stirring evenly, high temperature cabonization, and use NaOH successively Solution and deionized water stirring, after cleaning to neutrality, drying meso-porous carbon material;
S2, under nonoxidizing atmosphere, dispersant PEG-4000 and the meso-porous carbon material are added to containing in ferric solution, It stirs evenly, sodium borohydride solution is then added, filtered after being stirred to react, up to the mesoporous carbon of load Zero-valent Iron after washing and drying Material.
2. preparation method according to claim 1, which is characterized in that in step S1, the temperature of the high temperature cabonization and when Between be respectively 400-600 DEG C and 2-4h.
3. preparation method according to claim 1 or 2, which is characterized in that described to be containing ferric solution in step S2 The ethanol solution of Iron(III) chloride hexahydrate, and the mass ratio of the Iron(III) chloride hexahydrate, mesoporous carbon and PEG-4000 is (6- 8):1:(1-3).
4. according to claim 1-3 any one of them preparation methods, which is characterized in that in step S1, the colloidal silica The content of silica is 45-55wt% in silicon, and the feed postition of the colloidal silicon dioxide is to be added dropwise, it is preferable that institute The rate of addition for stating colloidal silicon dioxide is 0.1ml/s.
5. according to claim 1-3 any one of them preparation methods, which is characterized in that further include colloidal state dioxy in step S1 SiClx be added after heating hydrotropy solution and the heating after NaOH solution addition help cleaning, it is preferable that the heating hydrotropy solution includes 15-25min is stirred at 110-125 DEG C again after stirring 15-30min at 70-80 DEG C, the heating helps cleaning to use 25- The NaOH solution of 35wt% stirs 15-30min at 60-80 DEG C.
6. according to claim 1-3 any one of them preparation methods, which is characterized in that in step S2, the sodium borohydride is molten The feed postition of liquid is to be added dropwise, it is preferable that the concentration and rate of addition of the sodium borohydride solution are respectively 0.005- 0.01g/ml and 0.1ml/s;The time that is stirred to react after the sodium borohydride solution is added is 30-60min.
7. according to the meso-porous carbon material for the load Zero-valent Iron that claim 1-6 any one of them preparation methods obtain.
8. the meso-porous carbon material of load Zero-valent Iron according to claim 7, which is characterized in that Jie of the load Zero-valent Iron The specific surface area of hole carbon material is 100-400m2/ g, average pore size 5-10nm, Kong Rongwei 0.5-1.0cm3/g。
9. loading Zero-valent Iron according to claim 1-6 any one of them preparation method or claim 7-8 any one of them Application of the meso-porous carbon material in adsorbed water body in hexavalent chromium.
10. application according to claim 9, which is characterized in that the meso-porous carbon material of Zero-valent Iron will be loaded described in 25-35mg It is added in the water body of 30mL a concentration of 15-22mg/L containing hexavalent chromium, control water pH value is 2-5, stirring and adsorbing 5-8h.
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Cited By (2)

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CN112705160A (en) * 2020-11-17 2021-04-27 扬州大学 Ordered mesoporous carbon loaded zero-valent iron composite material and preparation method and application thereof
CN113134340A (en) * 2021-04-26 2021-07-20 江苏东方维德环保科技有限公司 Chromium ion adsorbent, preparation method, application method and regeneration method thereof, and treatment method of chromium in leather tail water

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