CN105013442B - Preparation method for ordered modified mesoporous carbon material - Google Patents
Preparation method for ordered modified mesoporous carbon material Download PDFInfo
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- CN105013442B CN105013442B CN201510398778.7A CN201510398778A CN105013442B CN 105013442 B CN105013442 B CN 105013442B CN 201510398778 A CN201510398778 A CN 201510398778A CN 105013442 B CN105013442 B CN 105013442B
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 66
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004094 surface-active agent Substances 0.000 claims abstract description 28
- -1 potassium ferricyanide Chemical compound 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 12
- 239000010865 sewage Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 238000004040 coloring Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 abstract 1
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 235000013736 caramel Nutrition 0.000 abstract 1
- 239000008098 formaldehyde solution Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011799 hole material Substances 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 238000009284 supercritical water oxidation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- CUHVTYCUTYWQOR-UHFFFAOYSA-N formaldehyde Chemical compound O=C.O=C CUHVTYCUTYWQOR-UHFFFAOYSA-N 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 231100000025 genetic toxicology Toxicity 0.000 description 1
- 230000001738 genotoxic effect Effects 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical group [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000003908 liver function Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Abstract
The invention relates to a preparation method for an ordered modified mesoporous carbon material, belonging to the technical field of preparation of mesoporous carbon materials. The method comprises the following steps: preparing a surfactant ethanol solution, adding resorcinol and potassium ferricyanide into the surfactant ethanol solution under a nitrogen atmosphere, carrying out stirring, and allowing the resorcinol to be completely dissolved; adding hydrochloric acid, adjusting the obtained solution to be acidic, carrying out stirring, and allowing potassium ferricyanide to be completely dissolved; adding a formaldehyde solution, carrying out stirring, and allowing the obtained system to gradually become caramel colour; pouring a clear liquid, and subjecting a solid to ageing; after aging is completed, carrying out vacuum heat polymerization; subjecting the obtained solid to calcination under the nitrogen atmosphere, and after calcination is completed, carrying out cooling to room temperature; and subjecting the obtained solid to calcination again in a muffle furnace, and carrying out cooling and grinding. According to the invention, a whole reaction system is under the nitrogen atmosphere, so iron ions are completely used for modification; reaction time is short, and heat polymerization temperature is low, so reaction conditions are easy to control; polar organic pollutants are easy to adsorb, and a mesoporous carbon material has magnetic property and is easy to separate.
Description
Technical field
The invention belongs to meso-porous carbon material preparing technical field, specifically, it is related to one kind and uses the potassium ferricyanide as changing
Property agent, the preparation method of the in order modified meso-porous carbon material for being prepared using soft template method in acid condition.
Background technology
Mesoporous material not only aperture it is moderate, with larger specific surface area and wall thickness, and with higher heat endurance and
Hydrothermal stability.With going deep into for research, the superiority of meso-porous carbon material is progressively highlighted.It is mesoporous compared with mesoporous silica-base material
Material with carbon element is except with addition to bigger specific surface area and pore volume, it may have higher chemical stability, mechanical stability and its
Good electric conductivity, is with a wide range of applications in fields such as absorption, separation, catalysis, hydrogen storage, battery, ultracapacitors.
DMF is widely used in petrochemical field as industrial chemicals and fine solvent.Produce in chemical products production process
Contain substantial amounts of DMF in raw waste water, being often only the waste water containing DMF of leather industry discharge just there are as many as 100,000,000 tons.DMF is because causing
Liver function exception, genotoxicity, increase the harm such as cancered danger and concerned.Process containing DMF waste water
The active sludge of main method, absorption method, extraction, membrane technology, supercritical water oxidation method, chemical method etc..But above each side
Method has problems, and activated sludge process has process time length and halfway problem of degrading；Supercritical water oxidation method is due to bar
Part is harsh, it is difficult to large-scale application；Chemical method power consumption is big, high cost；The finite capacity of adsorbent in absorption method, receives after absorption
Collection, regeneration power consumption are big.For absorption method, the property of adsorbent greatly limit the practical application of the method.Therefore, open
Send out adsorption capacity a kind of greatly, the adsorbent for being easy to collect after polarity organic pollution, absorption can be adsorbed very necessary.
Chinese patent 201310232070.5 disclose the meso-porous carbon material of a kind of carried metal or metal oxide and its
Preparation method, comprises the following steps：It is 40-64 by mass ratio:18-40:60-120:3:The surfactant of 2000-3000,
Phenol, formaldehyde, NaOH, water mixing, reaction 16-24h is obtained carbon matrix precursor solution；By loading metal-salt according to phenol
Feed intake mass ratio 0.02-2:20 are added in carbon matrix precursor solution, react 20-30h；Loading metal-salt is selected from gold chloride, nitric acid
One kind in silver, chloroplatinic acid, cadmium nitrate, iron chloride, nickel chloride, cobalt acetate；Loading metal-salt is added in carbon matrix precursor solution,
The water of 2-4 times of carbon matrix precursor liquor capacity is additionally added simultaneously；Reaction gained solid is cleaned, is dried, under non-oxidizing atmosphere
Roasting.Metal ion easily generates precipitation with hydroxyl reaction, affects the pore-size distribution of mesoporous carbon, affects the distribution of carried metal equal
Even property, while weaker to Adsorption of Organic power.
The content of the invention
It is an object of the invention to the shortcoming for overcoming prior art to exist, seeks design one kind in acid condition, with soft
Prepared by template, with large specific surface area, high hydrothermal stability, to polar organic matter high adsorption capacity in petrifaction sewage, together
When there is magnetic to be easily recycled, the preparation method of the in order modified meso-porous carbon material of the industrial wastewaters such as DMF absorption can be applied to.
To achieve these goals, the technical solution used in the present invention is：A kind of preparation of meso-porous carbon material modified in order
Method, comprises the following steps：
Step 1：It is surface-active in 60%～70% ethanol solution that surfactant is dissolved in into volume fraction in container
Agent is surfactant with the mass ratio of ethanol solution：Ethanol solution=2.5～3:16；
Step 2：In nitrogen atmosphere, add resorcinol and the potassium ferricyanide into container, resorcinol, the potassium ferricyanide and
The mass ratio of surfactant is resorcinol：The potassium ferricyanide：Surfactant=2.5～3:0.1～0.35:2.5～3, stir
Mix, be completely dissolved resorcinol；
Step 3：Hydrochloric acid is added in the solution of step 2, solution is adjusted to into acidity, stirred, make the potassium ferricyanide completely molten
Solution；
Step 4：Formalin is added in the solution of step 3, formaldehyde is with the mass ratio of resorcinol in formalin
Formaldehyde:Resorcinol=0.21～0.8：2.5～3, stirring, system gradually becomes burnt sugar coloring；
Step 5：Supernatant is toppled over, solid is aged；Vacuum hot polymerization after the completion of ageing；
Step 6：Solid roasting under the conditions of nitrogen atmosphere that step 5 vacuum hot polymerization is obtained, is down to room temperature after roasting；
Step 7：The solid that step 6 is obtained roasting again in Muffle furnace, grinds after cooling, is modified in order mesoporous
Material with carbon element.
Preferably, the surfactant is F127；
Preferably, it is 0.5～1 that the step 3 adds the Ph values of solution after hydrochloric acid；
Preferably, the mass fraction of formalin is 37%；
Preferably, the vacuum hot polymerization is 100 DEG C of vacuum 20～24h of hot polymerization in vacuum drying chamber；
Preferably, what the step 5 was aged concretely comprises the following steps：16～20h is aged at 30 DEG C；
Preferably, step 6 roasting is concretely comprised the following steps：Under the conditions of nitrogen atmosphere, in tubular heater, with 2
DEG C/heating rate of min is warming up to 180 DEG C, in this temperature calcination 5h, then is continuously heating to 400 with the heating rate of 2 DEG C/min
DEG C, then 850 DEG C are warming up to the heating rate of 5 DEG C/min, roasting 2h；
Preferably, step 7 roasting is concretely comprised the following steps：Heated up with the programming rate of 8 DEG C/min in Muffle furnace
To 450 DEG C, roasting 2h at this temperature；
The meso-porous carbon material modified in order is used to adsorb polarity organic pollution in petrifaction sewage；Jie modified in order
The DMF that hole material with carbon element is used in absorption effluent, in order modified meso-porous carbon material and the mass ratio of DMF are the mesoporous carbon materials that are modified in order
Material：DMF=0.8～1.2:5, be preferably modified in order meso-porous carbon material：DMF=1:5；The meso-porous carbon material modified in order is used
When DMF in absorption effluent, stir speed (S.S.) is 600-1800r/min, and preferably its stir speed (S.S.) is 1000r/min；It is described to have
During the DMF that the modified meso-porous carbon material of sequence is used in absorption effluent, the sewage containing DMF is alkalescence, and preferably its pH value is 9.
Beneficial effects of the present invention are：1) whole reaction system is sour environment, it is to avoid the iron ion in the potassium ferricyanide exists
Producing modifying function previous existence is modified into precipitating, be entirely used for；2) phenolic resin is prepared using resorcinol, the reaction time is short, heat
Poly- temperature is low, easy control of reaction conditions, realizes reaction speed very fast and controllable；3) in meso-porous carbon material surface introducing-CN
Base, makes meso-porous carbon material be easy to adsorb polarity organic pollution, and Fe is generated during roasting2O3, it is dispersed in Jie
On the material with carbon element of hole, make meso-porous carbon material that there is magnetic to be easily isolated；4) by the modified rate of adsorption for making meso-porous carbon material significantly
Improve, and adsorption saturation time is longer, while adsorbance substantially increases.
Description of the drawings
Fig. 1 is modified meso-porous carbon material in order and meso-porous carbon material infrared ray diffraction comparison diagram；
Fig. 2 is modified meso-porous carbon material N in order2Adsorption desorption curve map；
Fig. 3 is modified meso-porous carbon material DMF adsorption isotherm line charts in order；
Fig. 4 is modified meso-porous carbon material DMF adsorption dynamics adsorption kinetics figures in order；
As shown in Figure 1 curve 1 is mesoporous carbon infrared ray diffraction collection of illustrative plates, and curve 2 is modified meso-porous carbon material infrared ray diffraction in order
Collection of illustrative plates；As shown in Figure 2 curve 1 is N2Adsorption curve, curve 2 is N2Desorption curve.
Specific embodiment
Below by specific embodiment, the invention will be further described：
Embodiment 1
The preparation method of the meso-porous carbon material modified in order of the present embodiment, comprises the following steps：
Step 1：Surfactant is dissolved in the ethanol solution that volume fraction is 65% in container, surfactant is
F127 is surfactant with the mass ratio of ethanol solution：Ethanol solution=2.5:16；
Step 2：In nitrogen atmosphere, add resorcinol and the potassium ferricyanide into container, resorcinol, the potassium ferricyanide and
The mass ratio of surfactant is resorcinol：The potassium ferricyanide：Surfactant=2.5:0.1:2.5, stirring makes resorcinol
It is completely dissolved；
Step 3：Hydrochloric acid is added in the solution of step 2, solution is adjusted to into acidity, the Ph values for entering solution after hydrochloric acid are
0.5, stirring is completely dissolved the potassium ferricyanide；
Step 4：The quality that mass fraction is 37% formalin, formaldehyde and resorcinol is added in the solution of step 3
Than for formaldehyde:Resorcinol=0.21:2.5, stirring, system gradually becomes burnt sugar coloring；
Step 5：Supernatant is toppled over, solid is aged into 16h at 30 DEG C；After the completion of ageing 100 in vacuum drying chamber
DEG C vacuum hot polymerization 24h；
Step 6：The solid that step 5 vacuum hot polymerization is obtained under the conditions of nitrogen atmosphere, in tubular heater, with 2 DEG C/
The heating rate of min is warming up to 180 DEG C, in this temperature calcination 5h, then is continuously heating to 400 DEG C with the heating rate of 2 DEG C/min,
Then 850 DEG C are warming up to the heating rate of 5 DEG C/min, room temperature is down in roasting under the conditions of roasting 2h nitrogen atmospheres after roasting；
Step 7：The solid that step 6 is obtained is warming up to 450 DEG C in Muffle furnace with the programming rate of 8 DEG C/min, here
Roasting temperature 2h roastings again, grind after cooling, and be modified in order meso-porous carbon material.
The DMF that in order modified meso-porous carbon material is used in absorption effluent, be modified in order meso-porous carbon material and the mass ratio of DMF
For orderly modified meso-porous carbon material：DMF=1.2:5；During the DMF that in order modified meso-porous carbon material is used in absorption effluent, stirring
Speed is 600r/min；During the DMF that in order modified meso-porous carbon material is used in absorption effluent, the sewage containing DMF is alkalescence, its
PH value is 10.
Embodiment 2
The preparation method of the meso-porous carbon material modified in order of the present embodiment, comprises the following steps：
Step 1：Surfactant is dissolved in the ethanol solution that volume fraction is 60% in container, surfactant is
F127 is surfactant with the mass ratio of ethanol solution：Ethanol solution=3:16；
Step 2：In nitrogen atmosphere, add resorcinol and the potassium ferricyanide into container, resorcinol, the potassium ferricyanide and
The mass ratio of surfactant is resorcinol：The potassium ferricyanide：Surfactant=3:0.35:3, stirring makes resorcinol complete
CL；
Step 3：Hydrochloric acid is added in the solution of step 2, solution is adjusted to into acidity, the Ph values for adding solution after hydrochloric acid are
1, stirring is completely dissolved the potassium ferricyanide；
Step 4：The quality that mass fraction is 37% formalin, formaldehyde and resorcinol is added in the solution of step 3
Than for formaldehyde:Resorcinol=0.8：3, stirring, system gradually becomes burnt sugar coloring；
Step 5：Supernatant is toppled over, solid is aged into 20h at 30 DEG C；After the completion of ageing 100 in vacuum drying chamber
DEG C vacuum hot polymerization 20h；
Step 6：The solid that step 5 vacuum hot polymerization is obtained under the conditions of nitrogen atmosphere, in tubular heater, with 2 DEG C/
The heating rate of min is warming up to 180 DEG C, in this temperature calcination 5h, then is continuously heating to 400 DEG C with the heating rate of 2 DEG C/min,
Then 850 DEG C are warming up to the heating rate of 5 DEG C/min, room temperature is down in roasting under the conditions of roasting 2h nitrogen atmospheres after roasting；
Step 7：The solid that step 6 is obtained is warming up to 450 DEG C in Muffle furnace with the programming rate of 8 DEG C/min, here
Roasting temperature 2h roastings again, grind after cooling, and be modified in order meso-porous carbon material.
The DMF that in order modified meso-porous carbon material is used in absorption effluent, be modified in order meso-porous carbon material and the mass ratio of DMF
For orderly modified meso-porous carbon material：DMF=0.8:5；During the DMF that in order modified meso-porous carbon material is used in absorption effluent, stirring
Speed is 1800r/min；During the DMF that in order modified meso-porous carbon material is used in absorption effluent, the sewage containing DMF is alkalescence,
Its pH value is 8.
Embodiment 3
The preparation method of the meso-porous carbon material modified in order of the present embodiment, comprises the following steps：
Step 1：Surfactant is dissolved in the ethanol solution that volume fraction is 70% in container, surfactant is
F127 is surfactant with the mass ratio of ethanol solution：Ethanol solution=3:16；
Step 2：In nitrogen atmosphere, add resorcinol and the potassium ferricyanide into container, resorcinol, the potassium ferricyanide and
The mass ratio of surfactant is resorcinol：The potassium ferricyanide：Surfactant=3:0.2:3, stirring makes resorcinol complete
Dissolving；
Step 3：The hydrochloric acid that mass fraction is 37% is added in the solution of step 2, solution is adjusted to into acidity, add salt
The Ph values of solution are 0.8 after acid, and stirring is completely dissolved the potassium ferricyanide；
Step 4：The quality that mass fraction is 37% formalin, formaldehyde and resorcinol is added in the solution of step 3
Than for formaldehyde:Resorcinol=0.5：3, stirring, system gradually becomes burnt sugar coloring；
Step 5：Supernatant is toppled over, solid is aged into 20h at 30 DEG C；After the completion of ageing 100 in vacuum drying chamber
DEG C vacuum hot polymerization 20h；
Step 6：The solid that step 5 vacuum hot polymerization is obtained under the conditions of nitrogen atmosphere, in tubular heater, with 2 DEG C/
The heating rate of min is warming up to 180 DEG C, in this temperature calcination 5h, then is continuously heating to 400 DEG C with the heating rate of 2 DEG C/min,
Then 850 DEG C are warming up to the heating rate of 5 DEG C/min, room temperature is down in roasting under the conditions of roasting 2h nitrogen atmospheres after roasting；
Step 7：The solid that step 6 is obtained is warming up to 450 DEG C in Muffle furnace with the programming rate of 8 DEG C/min, here
Roasting temperature 2h roastings again, grind after cooling, and be modified in order meso-porous carbon material.
The DMF that in order modified meso-porous carbon material is used in absorption effluent, be modified in order meso-porous carbon material and the mass ratio of DMF
For orderly modified meso-porous carbon material：DMF=1:5；During the DMF that in order modified meso-porous carbon material is used in absorption effluent, stirring speed
Rate is 1000r/min；During the DMF that in order modified meso-porous carbon material is used in absorption effluent, the sewage containing DMF is alkalescence, its
PH value is 9.
Claims (9)
1. a kind of preparation method of in order modified meso-porous carbon material, it is characterised in that comprise the following steps：
Step 1：Surfactant is dissolved in into volume fraction in 60%-70% ethanol solutions in container, surfactant with
The mass ratio of ethanol solution is surfactant：Ethanol solution=2.5～3:16；
Step 2：In nitrogen atmosphere, resorcinol and the potassium ferricyanide, resorcinol, the potassium ferricyanide and surface are added into container
The mass ratio of activating agent is resorcinol：The potassium ferricyanide：Surfactant=2.5～3:0.1～0.35:2.5～3, stirring makes
Resorcinol is completely dissolved；
Step 3：Hydrochloric acid is added in the solution of step 2, it is 0.5-1 that solution is adjusted into pH, and stirring makes the potassium ferricyanide completely molten
Solution；
Step 4：Formalin is added in the solution of step 3, formaldehyde is formaldehyde with the mass ratio of resorcinol:Resorcinol=
0.21～0.8:2.5～3, stirring, system gradually becomes burnt sugar coloring；
Step 5：Supernatant is toppled over, solid is aged；Vacuum hot polymerization after the completion of ageing；
Step 6：Solid roasting under the conditions of nitrogen atmosphere that step 5 vacuum hot polymerization is obtained, is down to room temperature after roasting；
Step 7：The solid that step 6 is obtained roasting again in Muffle furnace, grinds after cooling, and be modified in order mesoporous carbon materials
Material.
2. the preparation method of in order modified meso-porous carbon material according to claim 1, it is characterised in that：The surface-active
Agent is F127.
3. the preparation method of in order modified meso-porous carbon material according to claim 1, it is characterised in that：The matter of formalin
Amount fraction is 37%.
4. the preparation method of the in order modified meso-porous carbon material according to any one of claim 1-3, it is characterised in that：It is described
Step 5 vacuum hot polymerization is concretely comprised the following steps：100 DEG C of vacuum 20～24h of hot polymerization in vacuum drying chamber.
5. the preparation method of the in order modified meso-porous carbon material according to any one of claim 1-3, it is characterised in that：It is described
What step 5 was aged concretely comprises the following steps：16～20h is aged at 30 DEG C.
6. the preparation method of the in order modified meso-porous carbon material according to any one of claim 1-3 1, it is characterised in that：Institute
State concretely comprising the following steps for step 6 roasting：Under the conditions of nitrogen atmosphere, in tubular heater, heated up with the heating rate of 2 DEG C/min
To 180 DEG C, in this temperature calcination 5h, then 400 DEG C are continuously heating to the heating rate of 2 DEG C/min, then with the liter of 5 DEG C/min
Warm ramp to 850 DEG C, roasting 2h.
7. the preparation method of the in order modified meso-porous carbon material according to any one of claim 1-3, it is characterised in that：It is described
Step 7 roasting is concretely comprised the following steps：450 DEG C are warming up to the programming rate of 8 DEG C/min in Muffle furnace, at this temperature roasting
2h。
8. the preparation method of in order modified meso-porous carbon material according to claim 1, it is characterised in that：It is described modified in order
Meso-porous carbon material is used to adsorb polarity organic pollution in petrifaction sewage.
9. the preparation method of in order modified meso-porous carbon material according to claim 1, it is characterised in that：It is described modified in order
The DMF that meso-porous carbon material is used in absorption effluent, in order modified meso-porous carbon material and the mass ratio of DMF are modified mesoporous carbon in order
Material：DMF=0.8～1.2:5；During the DMF that the meso-porous carbon material modified in order is used in absorption effluent, stir speed (S.S.) is
600-1800r/min；During the DMF that the meso-porous carbon material modified in order is used in absorption effluent, the sewage containing DMF is alkali
Property.
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| CN109046246B (en) * | 2018-09-06 | 2021-03-16 | 青岛科技大学 | Resource utilization method of m-phenylenediamine hydrolysis waste residue |
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