CN101597056B - Activated carbon surface passivation method - Google Patents
Activated carbon surface passivation method Download PDFInfo
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- CN101597056B CN101597056B CN2009100748558A CN200910074855A CN101597056B CN 101597056 B CN101597056 B CN 101597056B CN 2009100748558 A CN2009100748558 A CN 2009100748558A CN 200910074855 A CN200910074855 A CN 200910074855A CN 101597056 B CN101597056 B CN 101597056B
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Abstract
An activated carbon surface passivation method includes that: an activated carbon is placed into a reactor, 2-10L inert gas per gram activated carbon is led into the reactor in one hour, and the temperature is heated up from room temperature to 400-500 DEG C at a speed of 1-10 DEG C per minute and remains for 0.5-2h; the reactor is cooled to room temperature in inert gas, the activated carbon is taken out, the activated carbon, hydrazine hydrate and diethylene are prepared into mixed solution by the ratio of 1kg activated carbon, 1-3L 70-85% of hydrazine hydrate, 1-3kg NaOH and 3-5L diethylene glycol, the temperature is heated up from room temperature to 150-180 DEG C and remains for 2-3h, excessive hydrazine and water are steamed out, the temperature is further heated up to 190-220 DEG Cand remains for 3-5h and then is reduced to room temperature, and filtering, washing and drying are carried out, thus obtaining the activated carbon with passivated surface. The invention has the advantages of no change of specific area of the activated carbon during surface passivation and low comprehensive cost.
Description
Technical field
The present invention provides a kind of method of activated carbon surface passivation, is the method that the activated carbon surface oxygen-containing functional group is removed specifically.
Background technology
Because gac at high temperature reacts acquisition by containing charcoal precursor and some oxygen containing activators such as water vapour, CO2 or KOH, so some oxygen-containing functional groups are contained on the surface of gac inevitably.These surfaces have the gac of oxygen-containing functional group when the absorption that is used for petroleum substance, owing to interacting, the low-level hydro carbons of oxygen-containing functional group and some produces relatively large heat, the danger that causes petroleum products to catch fire strengthens, therefore must the oxygen-containing functional group of activated carbon surface be removed, made its surface passivation.
At present, the most general method of eliminate activity carbon surface oxygen-containing functional group is in thermal treatment or heat-treat in reducing atmosphere such as H2 in inert atmosphere such as N2 or Ar gas under the high temperature more than 800 ℃, to take off the oxygen-containing functional group of activated carbon surface more than 90%, but after so high Temperature Treatment, the specific surface area of gac will present decline by a relatively large margin, considerable change also will take place in pore structure, finally cause the deterioration of charcoal absorption performance.
Summary of the invention
The purpose of this invention is to provide the unconverted surface passivation method of a kind of gac specific surface area in the surface passivation process.
Principle of the present invention is such: (generally below 500 ℃) thermal treatment gac in N2 or Ar gas at first at low temperatures, to remove the carboxyl functional group of activated carbon surface, use the solution of hydrazine hydrate, NaOH and glycol ether to be reduced then 150-220 ℃ of carbonyl functional group with activated carbon surface, can remove the functional group of activated carbon surface like this, thereby make the surface of gac that passivation take place.
Concrete implementation process is as follows:
Gac is put into reactor, in 1 hour, feed the rare gas element that 2-10 rises,, be raised to 400-500 ℃, stop 0.5-2h from room temperature with the heat-up rate of 1-10 ℃/min with 1 gram gac; In rare gas element, be as cold as room temperature afterwards, take out gac, rise the hydrazine hydrate of 70-85wt% in 1Kg gac: 1-3: 1-3KgNaOH: 3-5 rises the ratio of glycol ether, and gac, hydrazine hydrate, NaOH and glycol ether are mixed with mixing solutions, and after being heated to 150-180 ℃ from room temperature, stop 2-3h and steam excessive hydrazine and water, further be warmed up to 190-220 ℃ again, stop 3-5h, cool to room temperature afterwards, filter, washing, drying obtains the gac of surface passivation.
Aforesaid gac comprises spheric active carbon, Powdered Activated Carbon, granulated active carbon and activated carbon fiber;
Aforesaid rare gas element comprises N
2Or Ar gas.
Advantage of the present invention just is:
(1) temperature that is adopted is lower than 500 ℃, can guarantee that the absorption property of gac is unaffected;
(2) carbonyl that adopts the method for hydrazine hydrate reduction can guarantee that activated carbon surface is difficult to desorption is reduced;
(3) because all reactions are all carried out under lower temperature, comprehensive cost is lower.
Embodiment
Embodiment 1
The 1Kg spheric active carbon is put into reactor, feed the N2 of 2000L/h., be raised to 400 ℃ with the heat-up rate of 1 ℃/min, stop 0.5h from room temperature; In inert atmosphere, be as cold as room temperature afterwards, take out gac, in 1KgAC: the hydrazine hydrate of 3 liters of 70wt% (unit): 1KgNaOH: the ratio of 3 liters of glycol ethers is mixed with mixture, and after being heated to 150 ℃ from room temperature, stopping 2h and steam excessive hydrazine and water, further be warmed up to 190 ℃ again, stop 3h, cool to room temperature afterwards, filter, washing, drying obtains the gac of surface passivation.The surface oxygen functional group of gac is 2mg/mol before the passivation, and specific surface area is 848m2/g, and passivation rear surface oxygen-containing functional group and specific surface area are respectively 0.12mg/mol and 842m2/g.
Embodiment 2
The 1Kg granulated active carbon is put into reactor, feed the N2 of 5000L/h., be raised to 450 ℃ with the heat-up rate of 3 ℃/min, stop 1h from room temperature; In inert atmosphere, be as cold as room temperature afterwards, take out gac, in 1KgAC: the hydrazine hydrate of 2 liters of 75wt%: 3KgNaOH: the ratio of 5 liters of glycol ethers is mixed with mixture, and after being heated to 150 ℃ from room temperature, stopping 3h and steam excessive hydrazine and water, further be warmed up to 190 ℃ again, stop 4h, cool to room temperature afterwards, filter, washing, drying obtains the gac of surface passivation.The surface oxygen functional group of gac is 2.3mg/mol before the passivation, and specific surface area is 1032m2/g, and passivation rear surface oxygen-containing functional group and specific surface area are respectively 0.22mg/mol and 1034m2/g.
Embodiment 3
1Kg200 purpose Powdered Activated Carbon is put into reactor, feed the Ar of 8000L/h., be raised to 500 ℃ with the heat-up rate of 5 ℃/min, stop 2h from room temperature; In inert atmosphere, be as cold as room temperature afterwards, take out gac, in 1KgAC: the hydrazine hydrate of 2 liters of 80wt%: 2KgNaOH: the ratio of 4 liters of glycol ethers is mixed with mixture, from and after room temperature is heated to 150 ℃, stop 3h and steam excessive hydrazine and water, further be warmed up to 190 ℃ again, stop 5h, cool to room temperature afterwards, filter, washing, drying obtains the gac of surface passivation.The surface oxygen functional group of gac is 1.9mg/mol before the passivation, and specific surface area is 2052m2/g, and passivation rear surface oxygen-containing functional group and specific surface area are respectively 0.13mg/mol and 2060m2/g.
Embodiment 4
1Kg asphalt based active carbon fiber is put into reactor, feed the Ar of 10000L/h., be raised to 500 ℃ with the heat-up rate of 10 ℃/min, stop 1.5h from room temperature; In inert atmosphere, be as cold as room temperature afterwards, take out gac, in 1KgAC: the hydrazine hydrate of 1 liter of 85wt%: 3KgNaOH: the ratio of 3 liters of glycol ethers is mixed with mixture, and after being heated to 150 ℃ from room temperature, stopping 2h and steam excessive hydrazine and water, further be warmed up to 190 ℃ again, stop 4h, cool to room temperature afterwards, filter, washing, drying obtains the gac of surface passivation.The surface oxygen functional group of activated carbon fiber is 1.8mg/mol before the passivation, and specific surface area is 1144m2/g, and passivation rear surface oxygen-containing functional group and specific surface area are respectively 0.11mg/mol and 1141m2/g.
Claims (3)
1. the passivating method of an activated carbon surface is characterized in that comprising the steps:
Gac is put into reactor, in 1 hour, feed the rare gas element that 2-10 rises,, be raised to 400-500 ℃, stop 0.5-2h from room temperature with the heat-up rate of 1-10 ℃/min with 1 gram gac; In rare gas element, be as cold as room temperature afterwards, take out gac, rise the hydrazine hydrate of 70-85wt% in 1Kg gac: 1-3: 1-3KgNaOH:3-5 rises the ratio of glycol ether, and gac, hydrazine hydrate, NaOH and glycol ether are mixed with mixing solutions, and after being heated to 150-180 ℃ from room temperature, stop 2-3h and steam excessive hydrazine and water, further be warmed up to 190-220 ℃ again, stop 3-5h, cool to room temperature afterwards, filter, washing, drying obtains the gac of surface passivation.
2. the passivating method of a kind of activated carbon surface as claimed in claim 1 is characterized in that described gac is spheric active carbon, Powdered Activated Carbon, granulated active carbon or activated carbon fiber.
3. the passivating method of a kind of activated carbon surface as claimed in claim 1 is characterized in that described rare gas element comprises N
2Or Ar gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100748558A CN101597056B (en) | 2009-07-07 | 2009-07-07 | Activated carbon surface passivation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100748558A CN101597056B (en) | 2009-07-07 | 2009-07-07 | Activated carbon surface passivation method |
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| CN101597056A CN101597056A (en) | 2009-12-09 |
| CN101597056B true CN101597056B (en) | 2011-04-06 |
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| CN2009100748558A Expired - Fee Related CN101597056B (en) | 2009-07-07 | 2009-07-07 | Activated carbon surface passivation method |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8652995B2 (en) * | 2011-07-19 | 2014-02-18 | Corning Incorporated | Steam activated non-lignocellulosic based carbons for ultracapacitors |
| CN104835651B (en) * | 2015-03-13 | 2018-07-27 | 宁波中车新能源科技有限公司 | A kind of high durable activated carbon and the preparation method using its ultracapacitor |
| CN105369242B (en) * | 2015-11-02 | 2017-11-28 | 常熟风范电力设备股份有限公司 | A kind of adjusting method of steel construction passivation temperature |
| CN105321733A (en) * | 2015-11-24 | 2016-02-10 | 中国林业科学研究院林产化学工业研究所 | Method for efficiently removing chemical groups from surface of supercapacitor carbon and supercapacitor carbon |
| CN106115686B (en) * | 2016-06-20 | 2017-12-15 | 浙江旺林生物科技有限公司 | A kind of passivation technology of nano material |
| CN105948035A (en) * | 2016-07-13 | 2016-09-21 | 南京林大活性炭有限公司 | Active carbon capable of eliminating surface chemical groups as well as preparation method and application thereof |
| KR102506938B1 (en) * | 2018-02-02 | 2023-03-07 | 현대자동차 주식회사 | Method for manufacturing activated carbon |
| CN112174135A (en) * | 2020-10-12 | 2021-01-05 | 江苏浦士达环保科技股份有限公司 | Method for refining water vapor activated super capacitor carbon |
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