CN101613102B - Method for preparing photocatalytic active carbon - Google Patents
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- CN101613102B CN101613102B CN2008101155235A CN200810115523A CN101613102B CN 101613102 B CN101613102 B CN 101613102B CN 2008101155235 A CN2008101155235 A CN 2008101155235A CN 200810115523 A CN200810115523 A CN 200810115523A CN 101613102 B CN101613102 B CN 101613102B
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Abstract
The invention relates to a method for preparing photocatalytic active carbon. The method comprises the following steps that: high-sulfur petroleum coke and/or high-sulfur coal is used as a raw material, and the granularity of the raw material is between 10 and 250 meshes; a mixture containing the raw material and a zinc chloride activator of which the mass ratio is between 0.1:1 and 2:1 undergoes heat insulation reaction at a temperature of between 500 and 1,000 DEG C for 0.5 to 4 hours; and a reactant is washed and dried. In the photocatalytic active carbon prepared by the method, a photocatalyst and active carbon have strong bonding force and are difficult to lose, provide photocatalysis and can also ensure long service life of the photocatalytic active carbon. The invention also provides the photocatalytic active carbon prepared by the method, which has dual functions of adsorption and photocatalysis, can remarkably prolong the service life of the active carbon, and reduce the needed regeneration frequency; meanwhile, the method uses the high-sulfur petroleum coke, the high-sulfur coal and the like as the raw materials to solve the problem of air pollution brought when the high-sulfur petroleum coke and the high-sulfur coal are used as fuel.
Description
Technical field
The present invention relates to the process of active carbon that a kind of preparation has photo-catalysis capability, relate in particular to a kind of by the synthetic method that obtains the photocatalyst activity charcoal of original position.The present invention also relates to a kind of photocatalytic active carbon product that obtains by aforesaid method simultaneously.
Background technology
Gac has very big specific surface area, therefore has very strong adsorptive power, is mainly used to adsorb the poisonous and harmful impurity of removing in water or the atmosphere, perhaps with the color that removes liquid.For example, a very useful approach is with the organic impurity that removes in the micro polluted source, thereby obtains to drink other water of level.
Gac in use for some time, it is saturated that adsorptive capacity will be tending towards, adsorptive power decreases or disappears.At this moment, the gac that must more renew perhaps makes old regeneration of activated carbon.Regeneration means commonly used comprise heating, pickling, alkali cleaning and solvent cleaning etc.Yet the gac that more renews also abandons old gac, will cause unnecessary waste.And select the method regenerated carbon of heating will expend a large amount of fuel, and emit poisonous gas; Method regenerated carbon with cleaning will produce new contaminated liquid, needs additionally further to handle.Therefore, aforesaid method all is not the optimum handling method of economic environmental protection.
A kind of method of new regeneration of activated carbon is arranged at present, in gac, add photocatalyst, for example titanium dioxide exactly.Photocatalyst the ultraviolet ray or contain under the irradiation of ultraviolet light source (for example sunlight), to produce transition of electron, high-octane electronics can with the material generation oxidation or the reduction reaction of catalyst surface, thereby the hazardous and noxious substances of macromolecule is decomposed into low-molecular-weight innoxious substance.Therefore, photocatalyst can be used for regenerated carbon, and the hazardous and noxious substances of adsorbing in the gac is decomposed, and can make gac keep adsorptive power and not produce extra pollution in long time, does not also need to consume a lot of energy.
Based on such thinking, some have occurred and adopted photocatalyst and gac bonded patent, for example U.S. Pat P 6673738, USP 5965479, USP 5266540.The common feature of the technical scheme of these patent disclosures is: photocatalyst is to add, and that is to say, the technical scheme of above-mentioned patent disclosure is that active carbon finished products and photocatalyst finished product are mixed, and obtains to have the gac of photo-catalysis capability.It is pointed out that the preparation of photocatalyst in these patents and the preparation of gac are two complete incoherent processes, photocatalyst is just sneaked into gac passively.The shortcoming of this way is, the bonding force of photocatalyst and gac is not strong, and photocatalyst runs off easily in the use; Though use binding agent can improve the bonding force of photocatalyst and gac to a certain extent, be present in the binding agent of activated carbon surface and the adsorptive power that photocatalyst can reduce gac.In addition, the photocatalyst purity of sneaking into also has very high requirement, after the photocatalyst that purity is not high is sneaked into gac, can bring other impurity to gac, influences the absorption property of gac.
Principal element in refinery coke and the coal is a carbon, the topmost purposes of these raw materials is as fuel at present, if do not handle but do not carry out desulfurization, element sulphur in refinery coke and the coal enters in the atmosphere, can cause serious atmospheric pollution, therefore the open report that utilizes these feedstock production gacs is also arranged, for example application number is 200610017471.9,200610019321,200610046177 and 200610057999 etc. Chinese patent application discloses and used the technical scheme of refinery coke as the feedstock production gac, application number is that 200610098623 Chinese patent application also discloses the technology of high sulphur coal as the feedstock production gac that adopt.But do not consider any photochemical catalysis factor in the disclosed technical scheme, that is, it only is to have put down in writing to utilize refinery coke or high sulphur coal to prepare the technology of gac.
Therefore, the preparation of photocatalyst and the preparation of gac are combined, the method for preparation of active carbon that obtains not need to use binding agent, photocatalyst and gac to have strong bonding force is one of this area problem demanding prompt solution.Simultaneously, adopting refinery coke and coal etc. as raw material in the technology of preparation gac, solve the pollution problem that these raw materials act as a fuel and bring when using, also is a developing direction with better prospect in this area.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of method for preparing photocatalytic active carbon, be raw material with high sulfur petroleum coke or high sulphur coal, obtain photocatalytic active carbon by generated in-situ mode.
The present invention also aims to provide a kind of photocatalytic active carbon, it has the absorption and the ability of photocatalysis Decomposition organic impurity, can be widely used in the improvement of water pollution and topsoil.
For achieving the above object, the invention provides a kind of method for preparing photocatalytic active carbon, this method comprises: with high sulfur petroleum coke and/or high sulphur coal is raw material, and the granularity of raw material is the 10-250 order, make and comprise described raw material and zinc chloride activation agent, and the two mass ratio be 0.1: 1 to 2: 1 mixture at 500-1000 ℃ of insulation reaction 0.5-4 hour, and reactant washed the exsiccant process.
According to concrete technical scheme of the present invention, preferably, the temperature of insulation reaction may be controlled to 650-900 ℃.And insulation reaction both can be carried out under air atmosphere, also can carry out under torpescence atmosphere, and wherein, torpescence atmosphere comprises one or more in nitrogen, argon gas and the helium etc.
In the process of preparation photocatalytic active carbon, zinc chloride is as activator, has very crucial effect, on the one hand can the etching raw material, generate gac; On the other hand can with the element sulphur generation chemical reaction in the raw material, generate the zinc sulphide with photocatalysis in generated in-situ mode, wherein, zinc sulphide can form good binding with gac, improve its bonding force, the photocatalytic active carbon that obtained performance is stable.Can also comprise alkali metal hydroxide in the mixture that contains raw material and zinc chloride, this alkali metal hydroxide comprises KOH, NaOH or its combination etc.; And the mass ratio of raw material and alkali metal hydroxide may be controlled to 0.1: 1 to 2: 1.Alkali metal hydroxide can be used as secondary activation agent, plays the effect that improves activation effect.Above-mentioned activator and secondary activation agent all can add with the form of the aqueous solution, and the amount of the aqueous solution is as the criterion with the amount of wherein contained activator.
Method for preparation of active carbon provided by the invention is a raw material with high sulfur petroleum coke and high sulphur coal etc. mainly, by adding activator, makes it generate gac; The adding of activator can make the gac of final acquisition have higher specific surface area, helps improving the absorption property of gac.Method for preparation of active carbon provided by the invention is particularly useful for high sulfur petroleum coke and high sulphur coal as raw material; Preferably, be used as the high sulfur petroleum coke of raw material and refinery coke and the coal (raw coal) that high sulphur coal can be higher than 2% (weight percent) for sulphur content among the present invention.
The granularity of raw material used in the present invention can be about 10-250 order, can its granularity be met the demands by raw material is ground separately; For reaching mixed effect preferably, also can earlier raw material be mixed obtaining mixture with activator (also can comprise secondary activation agent), then mixture is ground.
Before carrying out insulation reaction, can be earlier the raw material that reaches granularity requirements and the mixture of activator and/or secondary activation agent be carried out pre-treatment, be about to said mixture in 200-500 ℃ of insulation pre-treatment 0.2-10 hour, and pretreatment temperature is lower than the temperature of insulation reaction.Said mixture is carried out pre-treatment, can improve the specific surface area of gac, make the photocatalytic active carbon of last acquisition have preferable absorption property and photocatalysis performance.
Carrying out pre-treatment is in order to improve the specific surface area of gac, according to concrete technical scheme of the present invention, can carry out pre-treatment earlier before insulation reaction to mixture; In the concrete operations, can in the mixture of raw material and zinc chloride activation agent, add secondary activation agent and carry out pre-treatment afterwards again; Can also add secondary activation agent earlier in raw material, the mixture to raw material and secondary activation agent carries out pre-treatment then, adds the zinc chloride activation agent again after the pre-treatment, carries out follow-up steps such as insulation reaction.
According to concrete technical scheme of the present invention, pre-treatment can be carried out under air atmosphere, also can carry out under torpescence atmosphere, and wherein, torpescence atmosphere comprises one or more in nitrogen, argon gas and the helium etc.
The present invention also provides a kind of photocatalytic active carbon, and it is to prepare through above-mentioned method, has absorption and light-catalysed dual-use function.This photocatalytic active carbon has generated in-situ zinc sulphide photocatalyst, in absorption impurity, can also utilize the photocatalysis Decomposition organic impurity, can be widely used in the improvement of water pollution and topsoil etc.
Adopt method provided by the invention to prepare photocatalytic active carbon and have following advantage:
1, the photocatalyst in Zhi Bei the photocatalytic active carbon is generated in-situ, and is strong with the bonding force of gac, in use is difficult for running off, and when photocatalysis is provided, can also guarantee that photocatalytic active carbon has long work-ing life;
2, Zhi Bei photocatalytic active carbon has absorption and light-catalysed dual-use function, can the significant prolongation gac work-ing life, significantly reduce the needed regeneration times of gac;
3, the step of preparation photocatalytic active carbon is simple, can one the step machine, avoid adopting the step complexity that the method that adds photocatalyst brings, problem with high costs; And preparation method provided by the invention adopts high sulfur petroleum coke and high sulphur coal as raw material, does not need to adopt high-purity photocatalyst, also can effectively reduce cost;
4, high sulfur petroleum coke and high sulphur coal can be prepared into the novel material of high added value, the atmospheric pollution that has brought when having avoided raw material (high sulfur petroleum coke and high sulphur coal) as fuel.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the gac of embodiment 1 preparation.
Fig. 2 is that the gac of embodiment 1 preparation decomposes the ratio of methylene blue and the relation curve between the ultraviolet irradiation time.
Fig. 3 is the X ray diffracting spectrum of the gac of embodiment 2 preparations.
Fig. 4 is that the gac of embodiment 2 preparations decomposes the ratio of methylene blue and the relation curve between the ultraviolet irradiation time.
Fig. 5 is the X ray diffracting spectrum of the gac of embodiment 3 preparations.
Fig. 6 is that the gac of embodiment 3 preparations decomposes the ratio of methylene blue and the relation curve between the ultraviolet irradiation time.
Embodiment
Below describe the present invention program's enforcement and the beneficial effect that is had in detail by specific embodiment, but but can not form any qualification to practical range of the present invention.
The method for preparing photocatalytic active carbon provided by the invention can comprise following concrete steps:
1, according to raw material: the zinc chloride activation agent=(0.1-2): the ratio of 1 (weight ratio) obtains mixture with raw material and activator mix, as required, can also be according to raw material: alkali metal hydroxide=(0.1-2): the ratio of 1 (weight ratio) is further added alkali metal hydroxide (being secondary activation agent) in mixture, comprise KOH, NaOH or its combination, activator (comprising secondary activation agent) can add with the form of the aqueous solution;
Wherein, raw material is high sulfur petroleum coke or high sulphur coal, especially sulphur content is above refinery coke or a coal of 2% weight percent, this raw material can with activator mix before grind to form and be of a size of 10-250 purpose fine powder, perhaps the mixture of raw material and activator (can comprise secondary activation agent) being ground to form grain size is 10-250 purpose powder;
2, for the specific surface area of the photocatalytic active carbon that improves last acquisition, can carry out pre-treatment to the mixture of mixture, raw material and the secondary activation agent of raw material and zinc chloride activation agent or the mixture of raw material and activator (comprising secondary activation agent), its concrete processing step and parameter are: with said mixture 200-500 ℃ of insulation pre-treatment 0.2-10 hour;
Wherein, when in carrying out pretreated mixture, not comprising the zinc chloride activation agent, after pre-treatment, should in this mixture, add the zinc chloride activation agent; When in carrying out pretreated mixture, not comprising secondary activation agent,, can after pre-treatment, add secondary activation agent for improving activation effect;
3, the mixture that above-mentioned steps is obtained was at 500-1000 ℃ of insulation reaction 0.5-4 hour;
4, washing, oven dry, the photocatalytic active carbon after obtaining handling.
Embodiment 1
Selecting high sulfur petroleum coke for use is raw material, and wherein the content of sulphur is 3.53% (weight percent); 10 gram refinery cokes and 40 gram zinc chloride are mixed, put into the planetary ball mill ball milling, obtaining granularity is 100 purpose mixtures; Mixture is put into activation furnace, feed nitrogen atmosphere, carried out pre-treatment in 10 hours 200 ℃ of insulations then, activation furnace was warming up to 500 ℃ of insulation reaction 4 hours then; After the cooling, product is washed with distilled water to pH value=7, uses oven for drying then, obtain photocatalytic active carbon.
Figure 1 shows that the X ray diffracting spectrum of this photocatalytic active carbon, can see in the gac product and contain zinc sulphide.After testing, the specific surface area of product (photocatalytic active carbon) is 200.17m
2/ g.With accurate weighing 0.5 gram of products therefrom, the absorption methylene blue is to saturated, put into beaker then, add the methylene blue solution of 70 milliliters of 100mg/L again, seal with preservative film, be placed on the constant temperature blender with magnetic force and stir and with the ultra violet lamp of wavelength 365nm, ultraviolet lamp is 15 centimetres apart from the distance of liquid level, the absorbancy of usefulness spectrophotometer measurement liquid.Figure 2 shows that measuring result, promptly gac decomposes the ratio of methylene blue and the relation curve between the ultraviolet irradiation time, can see that gac has decomposed adsorbed methylene blue at short notice.
Embodiment 2
Selecting high sulphur coal for use is raw material, and wherein the content of sulphur is 5.25% (weight percent); 10 gram high sulphur coal are put into the planetary ball mill ball milling, and obtaining granularity is 200 purpose fine powders; Fine powder is put into 30 gram water, put into 30 gram KOH then and fully mix, and flooded 2 hours; Mixture is put into activation furnace in 350 ℃ of insulation pre-treatment 1 hour, cooling subsequently; Again products obtained therefrom is put into 30 gram water, put into 30 gram zinc chloride then and fully mix, and flooded 2 hours; Mixture is put into activation furnace be warming up to 1000 ℃ of insulation reaction 0.5 hour, cooling then, washing, drying obtains photocatalytic active carbon.
Fig. 3 is the X ray diffracting spectrum of this photocatalytic active carbon, can see in the gac product and contain zinc sulphide.After testing, the specific surface area of product (photocatalytic active carbon) is 1078.25m
2/ g.With accurate weighing 0.5 gram of products therefrom, the absorption methylene blue is to saturated, put into beaker then, add the methylene blue solution of 70 milliliters of 100mg/L again, seal with preservative film, be placed on the constant temperature blender with magnetic force and stir and with the ultra violet lamp of wavelength 365nm, ultraviolet lamp is 15 centimetres apart from the distance of liquid level.Absorbancy with spectrophotometer measurement liquid.Figure 4 shows that measuring result, promptly gac decomposes the ratio of methylene blue and the relation curve between the ultraviolet irradiation time, can see that gac has decomposed adsorbed methylene blue at short notice.
Embodiment 3
Selecting high sulfur petroleum coke for use is raw material, and wherein the content of sulphur is 3.53% (weight percent); 10 gram high sulphur coal are put into the planetary ball mill ball milling, and obtaining granularity is 200 purpose fine powders; Fine powder is put into 30 gram water, put into 40 gram KOH then and fully mix, and flooded 2 hours; Mixture is put into activation furnace in 450 ℃ of insulation pre-treatment 1 hour, cooling subsequently; Again products obtained therefrom is put into 30 gram water, put into 35 gram zinc chloride then and fully mix, and flooded 2 hours; Mixture is put into activation furnace be warming up to 850 ℃ of insulation reaction 0.5 hour, cooling then, washing, drying obtains photocatalytic active carbon.
Fig. 5 is the X ray diffracting spectrum of this photocatalytic active carbon, can see in the gac product and contain zinc sulphide.After testing, the specific surface area of product (photocatalytic active carbon) is 1525.61m
2/ g.With accurate weighing 0.5 gram of products therefrom, the absorption methylene blue is to saturated, put into beaker then, add the methylene blue solution of 70 milliliters of 100mg/L again, seal with preservative film, be placed on the constant temperature blender with magnetic force and stir and with the ultra violet lamp of wavelength 365nm, ultraviolet lamp is 15 centimetres apart from the distance of liquid level.Absorbancy with spectrophotometer measurement liquid.Figure 6 shows that measuring result, promptly gac decomposes the ratio of methylene blue and the relation curve between the ultraviolet irradiation time, can see that gac has decomposed adsorbed methylene blue at short notice.
Claims (9)
1. method for preparing photocatalytic active carbon, this method comprises: with high sulfur petroleum coke and/or high sulphur coal is raw material, and the granularity of raw material is the 10-250 order, make and comprise described raw material and zinc chloride activation agent, and the two mass ratio be 0.1: 1 to 2: 1 mixture at 500-1000 ℃ of insulation reaction 0.5-4 hour, and reactant washed the exsiccant process; Wherein, described high sulfur petroleum coke and high sulphur coal are respectively refinery coke and the raw coal that sulphur content is higher than 2% weight.
2. the method for claim 1, wherein the temperature of described insulation reaction is 650-900 ℃.
3. also comprise alkali metal hydroxide in the method for claim 1, wherein described mixture.
4. method as claimed in claim 3, wherein, described alkali metal hydroxide comprises KOH, NaOH or its combination.
5. as claim 3 or 4 described methods, wherein, the mass ratio of described raw material and alkali metal hydroxide is 0.1: 1 to 2: 1.
6. as claim 1 or 3 described methods, wherein, described mixture is before insulation reaction, and prior to 200-500 ℃ of insulation pre-treatment 0.2-10 hour, and this pretreatment temperature was lower than the temperature of insulation reaction.
7. method as claimed in claim 4, wherein, described method comprises: the mixture of raw material and alkali metal hydroxide is incubated pre-treatment 0.2-10 hour prior to 200-500 ℃, and this pretreatment temperature is lower than the temperature of insulation reaction; Add the zinc chloride activation agent to this in pretreated mixture, the mass ratio of described raw material and zinc chloride activation agent is 0.1: 1 to 2: 1, and is at 500-1000 ℃ of insulation reaction 0.5-4 hour, that the reactant washing is dry.
8. as claim 1 or 7 described methods, wherein, described insulation reaction or pre-treatment are carried out under air atmosphere, perhaps carry out under torpescence atmosphere, and described torpescence atmosphere comprises one or more in nitrogen, argon gas and the helium.
9. method as claimed in claim 6, wherein, described insulation reaction or pre-treatment are carried out under air atmosphere, perhaps carry out under torpescence atmosphere, and described torpescence atmosphere comprises one or more in nitrogen, argon gas and the helium.
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| KR101840488B1 (en) * | 2010-03-31 | 2018-03-20 | 주식회사 쿠라레 | Activated carbon and uses thereof |
| CN102627279A (en) * | 2012-03-29 | 2012-08-08 | 南京正森环保科技有限公司 | Method for preparing smoke mercury-removing activated carbon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030100445A1 (en) * | 2001-11-28 | 2003-05-29 | Toshiya Ueda | Photocatalytic active carbon, colored photocatalytic active carbon, coloring active carbon, and deodorant and adsorption product using them |
| CN1884062A (en) * | 2006-07-10 | 2006-12-27 | 山西中良煤化工科技有限公司 | Process of continuous preparation of activated carbon with high specific surface area |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030100445A1 (en) * | 2001-11-28 | 2003-05-29 | Toshiya Ueda | Photocatalytic active carbon, colored photocatalytic active carbon, coloring active carbon, and deodorant and adsorption product using them |
| CN1884062A (en) * | 2006-07-10 | 2006-12-27 | 山西中良煤化工科技有限公司 | Process of continuous preparation of activated carbon with high specific surface area |
Non-Patent Citations (1)
| Title |
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| A. Ahmadpour et al..The preparation of active carbons from coal by chemical and physical activation.《Carbon》.1996,第34卷(第4期),471-479. * |
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