CN113120904B - Activated carbon treatment method - Google Patents
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- CN113120904B CN113120904B CN201911418294.9A CN201911418294A CN113120904B CN 113120904 B CN113120904 B CN 113120904B CN 201911418294 A CN201911418294 A CN 201911418294A CN 113120904 B CN113120904 B CN 113120904B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 191
- 238000000034 method Methods 0.000 title claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000007790 solid phase Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 19
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical group OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 26
- 229910052799 carbon Inorganic materials 0.000 abstract description 19
- 239000011148 porous material Substances 0.000 abstract description 9
- 229930195733 hydrocarbon Natural products 0.000 abstract description 2
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 2
- 239000004215 Carbon black (E152) Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 239000000203 mixture Substances 0.000 description 20
- 238000001914 filtration Methods 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 9
- 230000007935 neutral effect Effects 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 7
- 239000002131 composite material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000009489 vacuum treatment Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- MQKXWEJVDDRQKK-UHFFFAOYSA-N bis(6-methylheptyl) butanedioate Chemical compound CC(C)CCCCCOC(=O)CCC(=O)OCCCCCC(C)C MQKXWEJVDDRQKK-UHFFFAOYSA-N 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 1
- 235000019797 dipotassium phosphate Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- -1 nitrogen-containing compound Chemical class 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000002025 wood fiber Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
-
- 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
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3071—Washing or leaching
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/378—Purification
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses an activated carbon treatment method, which comprises the steps of uniformly mixing activated carbon and an alcohol solvent, carrying out solid-liquid separation, drying a separated solid-phase material, uniformly mixing the dried solid-phase material with an additive and water, carrying out solid-liquid separation again, drying the separated solid-phase material, and further carrying out high-temperature heat treatment under a vacuum condition. The method can remove hydrocarbon and inorganic impurities in the active carbon pore canal to obtain high-quality active carbon.
Description
Technical Field
The invention belongs to the field of preparation of porous materials, and particularly relates to an activated carbon treatment method.
Background
The activated carbon is prepared by pyrolyzing and activating carbon-containing raw materials such as wood, coal, petroleum coke and the like, and is a carbon material with a developed pore structure, a larger specific surface area, abundant surface chemical groups and stronger specific adsorption capacity. The activated carbon material is widely applied to the fields of chemical catalysis, chemical separation and purification, environmental protection and the like.
CN109835897A discloses a metal/heteroatom modified distiller's grain-based activated carbon and a preparation method thereof. Crushing dried spirit vinasse, adding a nitrogen-containing compound and a transition metal compound, carbonizing the spirit vinasse at 600-900 ℃ for 1-3 hours in a nitrogen atmosphere, soaking carbonized active carbon in acid for 5-15 hours, filtering, washing and drying; and finally, activating the carbonized activated carbon at the high temperature of 700-900 ℃ for 2-5 h in the atmosphere of activated gas to obtain the metal/heteroatom modified white spirit vinasse-based activated carbon.
CN109876772A discloses a nano carbon fiber and active carbon composite material and a preparation method thereof, the invention comprises the steps of firstly respectively preparing a polyvinyl alcohol solution and a nickel nitrate hexahydrate solution: then dropwise adding dilute hydrochloric acid into the polyvinyl alcohol solution, adding the nickel nitrate hexahydrate into the polyvinyl alcohol solution, and uniformly stirring; then, dripping ethylene glycol and triethanolamine into the mixed solution and uniformly stirring to prepare transparent sol liquid; then adding activated carbon, carrying out ultrasonic treatment, and standing to obtain precursor sol; then drying the precursor sol into a precursor xerogel; then the precursor xerogel is put into a vertical roasting furnace of the reactor for treatment; and then soaking the composite material containing nickel in dilute hydrochloric acid or dilute nitric acid to remove surface metal oxides, washing with deionized water, and drying to obtain the composite material of the carbon nanofibers and the activated carbon.
CN109735966A discloses a method for preparing an activated carbon fiber with a hollow structure from wood fibers, comprising the steps of putting paper into a tube furnace, heating to 200-300 ℃ under the protection of nitrogen, heating to 400-600 ℃, and keeping the temperature for a period of time to obtain the carbon fiber. And then, taking phosphoric acid, zinc chloride, ammonium chloride, potassium hydroxide, sodium hydroxide and dipotassium phosphate as activating agents, and carrying out activation reaction at 600-800 ℃ to obtain the activated carbon fiber with the hollow structure.
CN109701492A discloses a functional graphene composite activated carbon and a preparation method thereof, wherein different raw materials are weighed in proportion; preparing a modified graphene dispersion aqueous solution; adding granular activated carbon into the prepared graphene solution; and adding the additive into the solution, stirring, heating again after the reaction is finished, and drying to obtain the functional graphene composite activated carbon.
The activated carbon has various types and different preparation methods, and the preparation process routes are different due to different raw material sources, but the activated carbon products obtained by the existing method contain trace impurities. Especially, for the high surface area activated carbon material, because the surface area is too high and the pore is tiny, in some special high-standard application scenes, the activated carbon material containing trace impurities cannot meet the application requirements, and therefore, the development of a purification treatment method for the activated carbon material is urgently needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an activated carbon treatment method, which can remove hydrocarbons and inorganic impurities in activated carbon pore canals to obtain high-quality activated carbon. The method solves the technical problem that impurities exist in active carbon channels obtained by the existing active carbon preparation method or active carbon channels subjected to or not subjected to regeneration treatment after use to block the active carbon channels, so that physicochemical properties such as surface area and service performance of the active carbon channels are influenced, and the active carbon materials cannot be used in an application scene with extremely severe cleanliness.
The invention provides an activated carbon treatment method, which comprises the following steps:
(1) Uniformly mixing activated carbon and an alcohol solvent, then carrying out solid-liquid separation, and drying the separated solid-phase material;
(2) Uniformly mixing the dried material obtained in the step (1), an additive and water, and then carrying out solid-liquid separation;
(3) And (3) drying the solid-phase material obtained by separation in the step (2), and further performing high-temperature heat treatment under a vacuum condition.
In the above activated carbon treatment method, the activated carbon in step (1) may be a commercially available activated carbon, may be an activated carbon obtained according to a conventional preparation method, or may be an activated carbon which has been used or has not been subjected to regeneration treatment.
In the activated carbon treatment method, the alcohol solvent in the step (1) is one or more of methanol, ethanol, propanol and butanol, preferably ethanol.
In the above activated carbon treatment method, the mixing operation in the step (1) and the step (2) may be performed by stirring, preferably, by stirring under ultrasonic conditions. The ultrasonic frequency is 15 KHz-10 MHz, and the power is 20-100W/L according to the volume of the solution. The ultrasonic time is 0.5 to 10 hours, preferably 1 to 8 hours.
In the activated carbon treatment method, the mass ratio of the activated carbon to the alcohol solvent in the step (1) is 8-35: 100, preferably 10 to 30:100.
in the above activated carbon treatment method, the solid-liquid separation in the step (1) and the step (2) may be performed by filtration, and the filtration is washed with deionized water until the filtrate is neutral.
In the activated carbon treatment method, the drying in the step (1) and the step (3) is carried out for 5 to 15 hours at the temperature of between 100 and 140 ℃.
In the above activated carbon treatment method, the additive in step (2) is one or more of sodium dodecyl sulfate, diisooctyl succinate sodium sulfonate, and cetyltrimethylammonium bromide, preferably sodium dodecyl sulfate or cetyltrimethylammonium bromide.
In the activated carbon treatment method, the mass ratio of the solid-phase material obtained after the treatment in the step (1) in the step (2) to the additive to the water is 1-20: 0.1 to 0.2:100, preferably 2 to 18:0.2 to 1.8:100.
in the above activated carbon treatment method, the high-temperature heat treatment in the step (3) is carried out at 400 to 800 ℃ for 2 to 7 hours, preferably at 450 to 750 ℃ for 3 to 6 hours; the degree of vacuum is 4 to 22Pa, preferably 5 to 20Pa.
Compared with the prior art, the purification treatment method of the active carbon has the following advantages:
the existing activated carbon purification treatment method is to treat activated carbon at high temperature usually, most impurities in the activated carbon are decomposed at high temperature and discharged, and finally, a purified activated carbon product is obtained. The active carbon obtained after the treatment by the existing high-temperature treatment method can meet the use requirements of general industry. However, the activated carbon has a very rich micropore system and a narrow pore size, and particularly, part of active centers with strong activity in micropore channels have very strong adsorption force on part of impurity substances adsorbed in the pore channels, so that the impurities are very difficult to remove. Even if the impurities are removed, if the impurities cannot be timely and quickly removed from the treatment system, the impurities can be re-adsorbed by the activated carbon, and because the activated carbon mainly comprises microporous channels which are extremely narrow, as long as a trace amount of impurities block orifices in a certain channel or other positions of other channels, the microporous channels can lose effects, namely the surface area of the channel is lost. A trace amount of impurities has a large influence on the surface area of the material. A trace amount of impurities has a large influence on the surface area of the material. This may affect the use of the carbon material in high-demand fields such as batteries. The active carbon treatment method comprises the steps of firstly mixing the active carbon with the alcohol solvent, then further treating the mixture with the additive solution, and finally combining the high-temperature heat treatment under the vacuum condition, so that the pollutants with weak adhesion in the microporous pore passages can be removed to the maximum extent, the impurities are quickly discharged out of a treatment system, the separation of the impurities which are difficult to remove is enhanced, and the impurity substances are prevented from being adsorbed again. Solves the problems that the prior microporous material has extremely strong adsorption force due to the electric field effect, has extremely narrow pore passage and is extremely difficult to completely recover the surface area.
Detailed Description
The following detailed description of the embodiments of the present invention is provided, but it should be noted that the scope of the present invention is not limited by the embodiments.
The surface area of the sample related to the invention adopts N 2 And (4) performing adsorption-desorption test, and calculating the surface area according to a BET formula.
The method of the invention embodies the treatment effect of the method through the change of the surface area before and after the treatment of the activated carbon.
Example 1
Mixing 15g of activated carbon A and 115g of ethanol, stirring for 2 hours under the ultrasonic condition, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then mixing with 1.8g of sodium dodecyl sulfate and 120g of deionized water, stirring for 2 hours in an ultrasonic environment, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering until the filtrate is neutral, and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then placing the mixture into a high-temperature furnace, setting the vacuum degree to be 15Pa, heating to 510 ℃ and carrying out constant-temperature treatment for 5h to obtain pure active carbon. The surface area of the original activated carbon was 1522 m 2 Per g, surface area after treatment 1637 m 2 (iv) g. Indicating that the impurities in the original sample were removed.
Example 2
Taking 10g of activated carbon B and 100g of activated carbon BMixing alcohol, stirring for 1h under ultrasonic condition, wherein the frequency of ultrasonic wave is 15KHz, and the power is 100W/L according to the volume of the solution; then filtering and drying the obtained solid-phase material for 7 hours at 108 ℃; then mixing with 0.2g of hexadecyl trimethyl ammonium bromide and 100g of deionized water, stirring for 1h under an ultrasonic environment, wherein the frequency of ultrasonic waves is 15KHz, and the power is 100W/L according to the volume of the solution; then filtering until the filtrate is neutral, and drying the obtained solid-phase material for 7 hours at 108 ℃; then placing the mixture into a high-temperature furnace, setting the vacuum degree to be 5Pa, heating to 750 ℃ and carrying out constant-temperature treatment for 3h to obtain pure active carbon. The surface area of the original activated carbon was 1936 m 2 (iv)/g, surface area after treatment 2152 m 2 (ii) in terms of/g. Indicating that the impurities in the original sample were completely removed.
Example 3
Mixing 30g of activated carbon C with 100g of ethanol, stirring for 8 hours under the ultrasonic condition, wherein the frequency of ultrasonic waves is 10MHz, and the power is 20W/L according to the volume of the solution; then filtering and drying the obtained solid-phase material for 12 hours at the temperature of 110 ℃; then 18g of activated carbon is taken to be mixed with 1.8g of hexadecyl trimethyl ammonium bromide and 100g of deionized water, and the mixture is stirred for 8 hours under the ultrasonic environment, wherein the frequency of ultrasonic waves is 10MHz, and the power is 20W/L according to the volume of the solution; then filtering until the filtrate is neutral, and drying the obtained solid-phase material for 12 hours at the temperature of 110 ℃; then placing the mixture into a high-temperature furnace, setting the vacuum degree to be 20Pa, heating to 450 ℃ and carrying out constant-temperature treatment for 6h to obtain pure active carbon. The surface area of the original activated carbon was 1850 m 2 (g) a surface area after treatment of 1908 m 2 (ii) in terms of/g. Indicating that the impurities in the original sample were completely removed.
Example 4
Mixing 16g of activated carbon D with 120g of ethanol, stirring for 4 hours under the ultrasonic condition, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then drying for 4.5h at 110 ℃; then filtering and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then 10g of active carbon is taken to be mixed with 1.28g of sodium dodecyl sulfate and 110g of deionized water, and the mixture is stirred for 4 hours under the ultrasonic environment, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering until the filtrate is neutral, and adding the obtained solid-phase material at 1Drying at 10 deg.C for 10h; then the mixture is put into a high temperature furnace, the vacuum degree is set to be 8Pa, and the mixture is heated to 680 ℃ for constant temperature treatment for 3.5h, thus obtaining pure active carbon. The surface area of the original activated carbon was 1763 m 2 (g) surface area after treatment 1817m 2 (iv) g. Indicating that the impurities in the original sample were completely removed.
Example 5
Mixing activated carbon E17 g and 105g of ethanol, stirring for 6 hours under the ultrasonic condition, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering and drying the obtained solid-phase material for 11 hours at the temperature of 102 ℃; then, 11 g of activated carbon is mixed with 1.01g of hexadecyl trimethyl ammonium bromide and 90g of deionized water, and the mixture is stirred for 6 hours in an ultrasonic environment, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering until the filtrate is neutral, and drying the obtained solid-phase material for 11 hours at the temperature of 102 ℃; then placing the mixture into a high-temperature furnace, setting the vacuum degree to be 11Pa, heating to 495 ℃ and carrying out constant-temperature treatment for 4h to obtain pure original activated carbon with the surface area of 1590 m 2 Per g, surface area after treatment 1628 m 2 (ii) in terms of/g. Indicating that the impurities in the original sample were completely removed.
Comparative example 1
Mixing 15g of activated carbon A and 115g of ethanol, stirring for 2 hours under the ultrasonic condition, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then placing the mixture into a high-temperature furnace, setting the vacuum degree to be 15Pa, heating the mixture to 510 ℃ and carrying out constant-temperature treatment for 5 hours, wherein the surface area of the obtained sample is 1616 m 2 (iv) g. Then placing the mixture into a high-temperature furnace, setting the vacuum degree to be 15Pa, heating to 510 ℃ and carrying out constant-temperature treatment for 10h, wherein the surface area of the obtained sample is 1631 m 2 (original activated carbon surface area 1522 m) 2 In terms of/g). It is shown that the elimination of the additive increases the difficulty of removing impurities and the vacuum treatment time must be increased to achieve better effect
In the above activated carbon treatment method, the high-temperature heat treatment in the step (3) is carried out at 400 to 800 ℃ for 2 to 7 hours, preferably at 450 to 750 ℃ for 3 to 6 hours; the degree of vacuum is 4 to 22Pa, preferably 5 to 20Pa.
Is 1637 m 2 /g
Comparative example 2
Mixing 15g of activated carbon A, 1.8g of sodium dodecyl sulfate and 120g of deionized water, and stirring for 2 hours in an ultrasonic environment, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering until the filtrate is neutral, and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then the mixture is put into a high-temperature furnace, the vacuum degree is set to be 15Pa, the mixture is heated to 510 ℃ and treated for 5 hours at constant temperature, and the surface area of the obtained sample is 1601 m 2 (iv) g. Then placing the mixture into a high-temperature furnace, setting the vacuum degree to be 15Pa, heating the mixture to 510 ℃ and carrying out constant-temperature treatment for 10 hours to obtain a sample with the surface area of 1635 m 2 Perg (original activated carbon surface area 1522 m) 2 In terms of/g). The reason is that the elimination of the alcohol solvent increases the difficulty of impurity removal, and more vacuum treatment time is needed to achieve better effect
Comparative example 3
Mixing 15g of activated carbon A and 115g of ethanol, stirring for 2 hours under the ultrasonic condition, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then mixing with 1.8g of sodium dodecyl sulfate and 120g of deionized water, stirring for 2 hours in an ultrasonic environment, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering until the filtrate is neutral, and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then the mixture is put into a common high-temperature furnace, and the temperature is raised to 510 ℃ for constant-temperature treatment for 5 hours. The surface area of the original activated carbon is 1522 m 2 Per g, surface area after treatment 1529 m 2 (iv) g. Compared with example 1, it is demonstrated that the conventional high temperature treatment method is hardly effective for the residual hard-to-remove impurities in the sample.
Comparative example 4
Mixing 15g of activated carbon A and 115g of ethanol, stirring for 2 hours under the ultrasonic condition, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then filtering and drying the obtained solid-phase material for 10 hours at the temperature of 110 ℃; then mixing with 1.8g of sodium dodecyl sulfate and 120g of deionized water, stirring for 2 hours in an ultrasonic environment, wherein the frequency of ultrasonic waves is 1MHz, and the power is 50W/L according to the volume of the solution; then theFiltering until the filtrate is neutral, and drying the obtained solid-phase material at 110 ℃ for 10 hours; then the mixture is put into a high temperature furnace, the vacuum degree is set to be 100Pa, and the mixture is heated to 510 ℃ for constant temperature treatment for 5h. The surface area of the original activated carbon is 1522 m 2 Per gram, surface area after treatment 1588 m 2 (ii) in terms of/g. It is demonstrated that impurities in the sample are difficult to completely remove by processing the sample at a vacuum degree lower than the required vacuum degree of the present invention.
Claims (12)
1. An activated carbon treatment process, comprising the steps of:
(1) Uniformly mixing activated carbon and an alcohol solvent, then carrying out solid-liquid separation, and drying the separated solid-phase material; the alcohol solvent is one or more of methanol, ethanol, propanol and butanol;
(2) Uniformly mixing the dried material obtained in the step (1), an additive and water, and then carrying out solid-liquid separation, wherein the additive is lauryl sodium sulfate or hexadecyl trimethyl ammonium bromide;
(3) And (3) drying the solid-phase material obtained by separation in the step (2), and further performing high-temperature heat treatment under a vacuum condition, wherein the high-temperature heat treatment is performed at 400-800 ℃ for 2-7 h, and the vacuum degree is required to be 4-22 Pa.
2. The activated carbon treatment method according to claim 1, wherein the alcohol solvent in the step (1) is ethanol.
3. The activated carbon treatment method according to claim 1, wherein the mixing in the step (1) and the step (2) is performed by stirring.
4. The activated carbon treatment method according to claim 3, wherein the mixing in the step (1) and the step (2) is stirred under ultrasonic conditions.
5. The activated carbon treatment method according to claim 4, wherein the ultrasonic frequency is 15KHz to 10MHz, and the power is 20 to 100W/L in terms of the volume of the solution; the ultrasonic time is 0.5-10 h.
6. The activated carbon treatment method according to claim 4, wherein the ultrasonic frequency is 15KHz to 10MHz, and the power is 20 to 100W/L in terms of the volume of the solution; the ultrasonic time is 1-8 h.
7. The activated carbon treatment method according to claim 1, wherein the mass ratio of the activated carbon to the alcohol solvent in the step (1) is from 8 to 35:100.
8. the activated carbon treatment method according to claim 1 or 7, wherein the mass ratio of the activated carbon to the alcohol solvent in the step (1) is 10 to 30:100.
9. the activated carbon treatment method according to claim 1, wherein the drying in the steps (1) and (3) is carried out at 100 to 140 ℃ for 5 to 15 hours.
10. The activated carbon treatment method according to claim 1, wherein the mass ratio of the solid phase material obtained after the treatment in the step (1) in the step (2), the additive and the water is 1-20: 0.1 to 0.2:100.
11. the activated carbon treatment method according to claim 1 or 10, wherein the mass ratio of the solid phase material obtained after the treatment in the step (1) in the step (2), the additive and the water is 2-18: 0.2 to 1.8:100.
12. the activated carbon treatment method according to claim 1, wherein the high-temperature heat treatment in the step (3) is a treatment at 450 to 750 ℃ for 3 to 6 hours; the vacuum degree is required to be 5-20 Pa.
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