CN101474551A - S-loaded activated carbon for mercury removal from flue gas and preparation method thereof - Google Patents
S-loaded activated carbon for mercury removal from flue gas and preparation method thereof Download PDFInfo
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- CN101474551A CN101474551A CNA2008102371903A CN200810237190A CN101474551A CN 101474551 A CN101474551 A CN 101474551A CN A2008102371903 A CNA2008102371903 A CN A2008102371903A CN 200810237190 A CN200810237190 A CN 200810237190A CN 101474551 A CN101474551 A CN 101474551A
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- active carbon
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- sulphur
- flue gas
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Abstract
The invention provides a sulfur-carrying active carbon for smoke gas demercuration and a preparation method thereof. The mass percentage content of sulfur of the sulfur-carrying active carbon is 18-30%, and the sulfur is evenly distributed on the surface of the active carbon and chemically combined with the active carbon; the granularity of the sulfur-carrying active carbon is 20-40 meshes.The preparation method comprises material preparation, thermo-precipitation preparation and cooling. In the invention, cheap sulfur is used as an additive agent of the active carbon, the content of the sulfur in the active carbon can reach 18-30% through the method of thermo-precipitation, and mercury in the smoke gas can be desorbed effectively. After the technique of thermo-precipitation, the active carbon has the advantages that the content of the sulfur is high and the sulfur is evenly distributed on the surface of the active carbon. In addition, the specific surface area, pore volume and pore diameter property and the like of the active carbon remain the same; the invention also is characterized in that the technique and the method are simple, the operation is easy and the cost is low, the method can be widely applied to the demercuration of smoke gas of coal-fired power factory and the like.
Description
Technical field
The invention belongs to the technology of preparing of modified activated carbon, be specifically related to a kind of sulfur loading active carbon that is used for flue gas demercuration, and prepare this process of active carbon.
Background technology
The discharging of coal-burning power plant's mercury is generally believed it is maximum mercury pollution source.For a long time, in order to have reduced the flue gas demercuration processing cost, reduced environmental pollution, one of ordinary skill in the art have carried out unremitting effort to the emission control of coal-fired flue-gas mercury.CN1559668 disclosed " the electrochemical regeneration method of flue gas demercuration sorbing material " for example, it is that the sorbing material that adopts activated carbon etc. to have bigger serface is a matrix, and at stromal surface infiltration sulphur, iodine, chlorine etc. are element modified, to improve absorption specificity and the adsorption capacity of material to mercury, sorbing material after the demercuration is handled through reductant-oxidant and complexing agent again, make the mercury in the sorbing material form complex ion, then under the effect of electric field force, mercury complex ion anode or negative electrode are moved, the mercury of oxidation is element mercury in cathodic reduction, and sorbing material can use as matrix once more.CN101121515 disclosed " a kind of manufacture method of special-purpose active carbon for removing mercury " for another example, it adopts the MgO of anthracite 70～80%, bituminous coal 15～25% and 2%～5% and/or 3%～10% MgSO
4, mix powder process, then, with the mixed powder that makes, by weight percentage, with powder 60～65%, pitch 5～10%, coal tar 25～30% is even with water 3～5% fully mixed alunites, is pressed into strip through press again, then after airing, charing, activation, fragmentation/screening, get sieve and go up finished product, soaked 8～10 hours with the 90% above concentrated sulfuric acid again, after sulfuric acid scrubbing is reclaimed, regulate pH to 4～8 with alkali, oven dry back screening at last.But similar these technology have affected complexity, the shortcoming that cost is higher.
At present, active carbon being carried out main methods of modification comprises: HNO
3Or H
2SO
4Oxidizing process, solution impregnation method etc., these methods mainly are to active carbon being added other element, thereby change the performance of active carbon.Such as: CN1129913 discloses a kind of method of producing modified activated carbon, and this method is to handle absorbent charcoal material in halogen atmosphere, with nucleopilic reagent the halogenation products therefrom is handled under the rising temperature then; The active carbon that this method is produced has functional group by the surface, thereby strengthens its ability in adsorption process.CN1296859 discloses a kind of active carbon coating one layer of polymeric in graininess or moulding, eliminates or reduces the product loss that is caused by dust, and do not reduce the adsorption rate of active carbon and the method for adsorption capacity.
Existing prior art is by modified activated carbon functional group, and reaching increases the charcoal absorption performance, but does not also have special at the active carbon that removes flue gas mercury.Therefore, be badly in need of on the market wanting to remove flue gas mercury, and lower-cost activated carbon.
Summary of the invention
At the prior art above shortcomings, it is low to the purpose of this invention is to provide a kind of cost, can effectively remove the sulfur loading active carbon that is used for flue gas demercuration of mercury element in the flue gas.
Another object of the present invention provides the method that a kind of preparation technology simply is used for the sulfur loading active carbon of flue gas demercuration.
The object of the present invention is achieved like this: be used for the sulfur loading active carbon of flue gas demercuration, it is characterized in that, the quality percentage composition of sulphur is 18～30% in the described sulfur loading active carbon, and sulphur is evenly distributed on activated carbon surface, and with the active carbon chemical bond; The granularity of sulfur loading active carbon is 20～40 orders.
Further, prepare the described method that is used for the sulfur loading active carbon of flue gas demercuration, may further comprise the steps:
1) get the raw materials ready: after granularity 20～40 purpose active carbon waters are rinsed well, under 105～110 ℃ of conditions, dry, standby; Select simple substance sulphur for use;
2) thermoprecipitation preparation: get fill above-mentioned simple substance sulphur heatproof container in thermoprecipitation stove bottom, more above-mentioned active carbon is inserted on second container at thermoprecipitation stove middle part; Then, sealing thermoprecipitation stove feeds high-purity N with 1～2L/min speed
230～40 minutes, discharge the air in the thermoprecipitation stove; Adjust N then
2Flow velocity is 0.5L/min, is warming up to 400～600 ℃, and stops heating after being incubated 50～90 minutes; Wherein, the weight ratio of active carbon and simple substance sulphur is 1:0.5～2.
3) adjust N
2Flow velocity be 1～2L/min, with the furnace temperature of heat of cooling precipitation stove, resulting active carbon is high-sulphur sulfur loading active carbon.
Further, the quality percentage composition of described simple substance sulphur is more than 99.9%.
Described second container is stainless (steel) wire or crucible, and the through hole of stainless (steel) wire is 200 orders.
Compared to existing technology, the present invention has following advantage:
1, the present invention adopts sulphur with low cost additive as active carbon, makes by the thermoprecipitation method that sulfur content reaches 18～30% in the active carbon, can be used in the mercury that effectively removes in the flue gas.
2, the active carbon of process heat post precipitation of the present invention not only has sulfur content height, sulphur in characteristics such as activated carbon surface are evenly distributed, and the specific area of this active carbon, pore volume and aperture character etc. still have the advantage of active carbon.
3, simple, the operation easily of process of the present invention, with low cost, the demercuration that can be widely used in coal-fired plant flue gas is used.
Description of drawings
Fig. 1 is the device schematic diagram that the present invention is used for the sulfur loading active carbon preparation method of flue gas demercuration.
Wherein: the 1-N2 bottle; 2-high temperature precipitation stove; 3-stainless steel pipe box; 4-contains second container of active carbon; 5-contains the heatproof container of sulphur; The 6-temperature regulating device.
The specific embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
The present invention relates to be used for the sulfur loading active carbon of flue gas demercuration, the quality percentage composition of sulphur is 18～30% in the sulfur loading active carbon, and sulphur is evenly distributed on activated carbon surface, and with the active carbon chemical bond; The granularity of sulfur loading active carbon is 20～40 orders.
Referring to Fig. 1, the present invention also provides a kind of preparation method who is used for the sulfur loading active carbon of flue gas demercuration, and step is as follows:
1) gets the raw materials ready.After granularity 20～40 purpose active carbon waters are rinsed well, put into drying box, 110 ℃ of bakings 1～2 hour, standby; Select simple substance sulphur for use, the quality percentage composition of the elemental sulfur in the simple substance sulphur is more than 99.9%;
2) thermoprecipitation preparation.Get fill above-mentioned simple substance sulphur heatproof container (crucible) in the thermoprecipitation furnace bottom, more described active carbon is inserted on the stainless (steel) wire at thermoprecipitation stove middle part, the stainless (steel) wire through hole is 200 orders; Then, sealing thermoprecipitation stove feeds high-purity N with 2L/min speed
230～40 minutes, discharge the air in the thermoprecipitation stove; Adjust N then
2Flow velocity is 0.5L/min, is warming up to 400-600 ℃, and stops heating after being incubated 50～90 minutes; Wherein, active carbon is 1:0.5～2 with the ratio of simple substance sulphur;
3) feeding N
2Condition under, adjust N
2Flow velocity be 1～2L/min, reduce the furnace temperature of (cooling) thermoprecipitation stove, resulting active carbon is the high sulfur loading active carbon of sulfur content.
Embodiment 1: take by weighing each 10 gram of dried active carbon and simple substance sulphur and put into two crucibles respectively, put into the thermoprecipitation stove again, placement be in proper order the active carbon crucible last, the sulphur crucible is descending; Feed N with 2L/min speed
230 minutes, to discharge the air in the stove; Adjust N
2Flow velocity is 0.5L/min, is heated to 550 ℃, and constant temperature stopped heating after 60 minutes; Feeding protection gas to furnace temperature cools off.The quality percentage composition that records sulphur in the active carbon is 21.34%.
Embodiment 2: take by weighing dry back active carbon 10 grams, each 5 gram of simple substance sulphur are put into two crucibles respectively, put into the thermoprecipitation stove again, placement be in proper order the active carbon crucible last, the sulphur crucible is following; Feed N with 2L/min speed
240 minutes, to discharge the air in the stove; Adjust N
2Flow velocity is 0.5L/min, is heated to 600 ℃, and constant temperature stopped heating after 80 minutes; Feeding protection gas to furnace temperature cools off.The quality percentage composition that records sulphur in the active carbon is 19.65%.
Embodiment 3: take by weighing each 10 gram of dry back active carbon and simple substance sulphur and put into two crucibles respectively, put into the thermoprecipitation stove again, placement be in proper order the active carbon crucible last, the sulphur crucible is following; Feed N with 2L/min speed
240 minutes, to discharge the air in the stove; Adjust N
2Flow velocity is 0.5L/min, is heated to 600 ℃, and constant temperature stopped heating after 90 minutes; Feeding protection gas to furnace temperature cools off.The quality percentage composition that records sulphur in the active carbon is 26.35%.
Embodiment 4: take by weighing dried active carbon 10 grams, each 5 gram of simple substance sulphur are put into respectively on the stainless (steel) wire and crucible of thermoprecipitation stove, placement in proper order for the stainless (steel) wire that fills active carbon last, the sulphur crucible is down; Feed N with 2L/min speed
230 minutes, to discharge the air in the stove; Adjust N
2Flow velocity is 0.5L/min, is heated to 500 ℃, and constant temperature stopped heating after 90 minutes; Feeding protection gas to furnace temperature cools off.The quality percentage composition that records sulphur in the active carbon is 24.36%.
Embodiment 5: take by weighing dried active carbon 10 grams, each 5 gram of simple substance sulphur are put into two crucibles respectively, put into the thermoprecipitation stove again, placement be in proper order the active carbon crucible last, the sulphur crucible is descending; Feed N with 2L/min speed
230 minutes, to discharge the air in the stove; Adjust N
2Flow velocity is 0.5L/min, is heated to 450 ℃, and constant temperature stopped heating after 90 minutes; Feeding protection gas to furnace temperature cools off.The quality percentage composition that records sulphur in the active carbon is 18.11%.
Because active carbon has very strong absorption property, has adsorbed airborne moisture in put procedure, therefore to dry processing before the experiment; Sulphur require to adopt is analyzed pure,, influenced the form of sulphur in the active carbon because chemical reaction can take place being introduced in the pyroprocess of other impurity elements in the sulphur.
Thermal precipitator method is handled active carbon the activated carbon surface sulfur content is significantly increased, and heating-up temperature is being controlled between 450-600 ℃.When temperature was lower than 450 ℃, the sulphur majority that exists with gaseous state existed with big molecular conformation, can cause active carbon hole plug, specific area reduction etc. in the precipitation of activated carbon surface, influenced its absorption property.Temperature surpasses 600 ℃ of skeleton structures that change active carbon, makes the active carbon distortion.When temperature is controlled between 450-600 ℃, the sulfur molecule majority exists with little molecule, can infiltrate in the active carbon space, helps the combination between the sulphur carbon on the one hand, make sulphur more even on the other hand, help improving the absorption property of active carbon in the distribution of activated carbon surface.
In heating process, walk too much sulfur vapor for fear of feeding the protection band of gas, cause the waste of resource, therefore in heating process, N
2Flow velocity is reduced to 0.5L/min from 2L/min.
Active carbon after handling is analyzed, the result shows that the binding ability between active carbon and the sulphur strengthens along with the rising of temperature, can infer that in separating thermal process chemical bond has taken place for the elemental sulfur and the active carbon that are deposited in activated carbon surface, rather than physical deposition.
The present invention is improved the activated carbon surface sulfur content by the method for thermal precipitation.Its major advantage is with low cost, and process is simple, can be applicable to remove the mercury in the flue gas, when sulfur loading active carbon of the present invention is used for demercuration, and sulphur in the active carbon and mercury generation chemical reaction, thus reach the purpose that removes mercury in the flue gas.
Gained modified activated carbon of the present invention, can pack into fixed adsorption bed or fluidisation adsorbent bed are used to handle the demercuration of mercury fume and other gases, and effect is obvious, and service time is long.Has good application prospects for the mercury that removes in the flue gas.
Claims (4)
1, be used for the sulfur loading active carbon of flue gas demercuration, it is characterized in that, the quality percentage composition of sulphur is 18～30% in the described sulfur loading active carbon, and sulphur is evenly distributed on activated carbon surface, and with the active carbon chemical bond; The granularity of sulfur loading active carbon is 20～40 orders.
2, a kind of described method that is used for the sulfur loading active carbon of flue gas demercuration of claim 1 for preparing may further comprise the steps:
1) get the raw materials ready: after granularity 20～40 purpose active carbon waters are rinsed well, under 105～110 ℃ of conditions, dry, standby; Select simple substance sulphur for use;
2) thermoprecipitation preparation: get fill above-mentioned simple substance sulphur heatproof container in thermoprecipitation stove bottom, more above-mentioned active carbon is inserted on second container at thermoprecipitation stove middle part; Then, sealing thermoprecipitation stove feeds high-purity N with 1～2L/min speed
230～40 minutes, discharge the air in the thermoprecipitation stove; Adjust N then
2Flow velocity is 0.5L/min, is warming up to 400～600 ℃, and stops heating after being incubated 50～90 minutes; Wherein, the weight ratio of active carbon and simple substance sulphur is 1:0.5～2;
3) adjust N
2Flow velocity be 1～2L/min, with the furnace temperature of heat of cooling precipitation stove, resulting active carbon is high-sulphur sulfur loading active carbon.
According to the described preparation method who is used for the sulfur loading active carbon of flue gas demercuration of claim 2, it is characterized in that 3, the quality percentage composition of described simple substance sulphur is more than 99.9%.
According to the described preparation method who is used for the sulfur loading active carbon of flue gas demercuration of claim 2, it is characterized in that 4, described second container is stainless (steel) wire or crucible, the stainless (steel) wire through hole is 200 orders.
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| CN101497029B (en) * | 2009-01-08 | 2011-06-29 | 重庆大学 | Sorbent for removing mercury from flue gas and preparation method thereof |
| CN102247823A (en) * | 2011-04-29 | 2011-11-23 | 叶向荣 | Preparation method of sulfurizing porous nanometer material for high-efficiency hydrargyrum removal |
| CN105858650A (en) * | 2016-03-22 | 2016-08-17 | 黎城蓝天燃气开发有限公司 | Method for manufacturing desulfurization denitration activated carbon by using waste activated carbon |
| CN106047387A (en) * | 2016-06-02 | 2016-10-26 | 潘成锋 | Efficient and environment-friendly coal and preparation method thereof |
| CN106237985A (en) * | 2016-08-16 | 2016-12-21 | 四川师范大学 | A kind of straw base selectivity removal of mercury material and its preparation method and application |
| CN106914215A (en) * | 2015-12-28 | 2017-07-04 | 沈阳中科环境工程科技开发有限公司 | Modified dipping sulfur molecule sieve mercury removal agent of one kind and preparation method thereof and special purpose device |
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| CN109621899A (en) * | 2019-01-17 | 2019-04-16 | 山东大学 | A kind of preparation system and method for demercuration sulfur loading active carbon/coke |
| CN112642413A (en) * | 2020-12-10 | 2021-04-13 | 北京清新环境技术股份有限公司 | Preparation method and product of mercury removal adsorbent based on active coke |
| CN115178274A (en) * | 2021-04-02 | 2022-10-14 | 中冶长天国际工程有限责任公司 | Preparation method and application of sulfur-carrying activated carbon |
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| CN115318248A (en) * | 2022-08-19 | 2022-11-11 | 宁夏华辉环保科技股份有限公司 | Accurate temperature-control sulfur-carrying activated carbon and preparation method thereof |
| CN115739018A (en) * | 2022-11-15 | 2023-03-07 | 中盐金坛盐化有限责任公司 | Preparation method and application of molten salt method sulfur modified porous material |
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- 2008-12-22 CN CN2008102371903A patent/CN101474551B/en not_active Expired - Fee Related
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| CN101497029B (en) * | 2009-01-08 | 2011-06-29 | 重庆大学 | Sorbent for removing mercury from flue gas and preparation method thereof |
| CN102247823A (en) * | 2011-04-29 | 2011-11-23 | 叶向荣 | Preparation method of sulfurizing porous nanometer material for high-efficiency hydrargyrum removal |
| CN102247823B (en) * | 2011-04-29 | 2012-12-19 | 叶向荣 | Preparation method of sulfurizing porous nanometer material for high-efficiency hydrargyrum removal |
| CN106914215A (en) * | 2015-12-28 | 2017-07-04 | 沈阳中科环境工程科技开发有限公司 | Modified dipping sulfur molecule sieve mercury removal agent of one kind and preparation method thereof and special purpose device |
| CN105858650A (en) * | 2016-03-22 | 2016-08-17 | 黎城蓝天燃气开发有限公司 | Method for manufacturing desulfurization denitration activated carbon by using waste activated carbon |
| CN105858650B (en) * | 2016-03-22 | 2018-03-20 | 黎城蓝天燃气开发有限公司 | Utilize the method for waste and old activated carbon manufacture desulphurization denitration activated carbon |
| CN106047387A (en) * | 2016-06-02 | 2016-10-26 | 潘成锋 | Efficient and environment-friendly coal and preparation method thereof |
| CN106237985A (en) * | 2016-08-16 | 2016-12-21 | 四川师范大学 | A kind of straw base selectivity removal of mercury material and its preparation method and application |
| CN106237985B (en) * | 2016-08-16 | 2018-08-31 | 四川师范大学 | A kind of stalk based selective removal of mercury material and its preparation method and application |
| CN106996884A (en) * | 2017-02-27 | 2017-08-01 | 深圳中物安防科技有限公司 | A kind of explosive gas phase detecting devices verification product and preparation method thereof |
| CN107262041A (en) * | 2017-06-16 | 2017-10-20 | 大唐环境产业集团股份有限公司 | A kind of sulfhydryl modified biomass char demercuration adsorbent and preparation method thereof |
| CN107812509A (en) * | 2017-09-14 | 2018-03-20 | 浙江工业大学 | A kind of filter membrane material and its preparation method and application |
| CN107812509B (en) * | 2017-09-14 | 2020-03-17 | 浙江工业大学 | Filtering membrane material and preparation method and application thereof |
| CN109621899A (en) * | 2019-01-17 | 2019-04-16 | 山东大学 | A kind of preparation system and method for demercuration sulfur loading active carbon/coke |
| CN109621899B (en) * | 2019-01-17 | 2020-04-28 | 山东大学 | Preparation system and method of demercuration sulfur-carrying activated carbon/coke |
| CN112642413A (en) * | 2020-12-10 | 2021-04-13 | 北京清新环境技术股份有限公司 | Preparation method and product of mercury removal adsorbent based on active coke |
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| CN115180752A (en) * | 2021-04-02 | 2022-10-14 | 中冶长天国际工程有限责任公司 | Desalination method for SRG washing wastewater by catalyzing with sulfur-containing activated carbon |
| CN115178274B (en) * | 2021-04-02 | 2023-12-29 | 中冶长天国际工程有限责任公司 | Preparation method and application of sulfur-carrying activated carbon |
| CN115180753B (en) * | 2021-04-02 | 2023-12-29 | 中冶长天国际工程有限责任公司 | Method for catalyzing and desalting SRG washing wastewater and system for catalyzing and desalting SRG washing wastewater |
| CN115180752B (en) * | 2021-04-02 | 2023-12-29 | 中冶长天国际工程有限责任公司 | Desalination method for SRG washing wastewater by catalyzing sulfur-containing activated carbon |
| CN115312716A (en) * | 2022-04-28 | 2022-11-08 | 湘潭大学 | Method for preparing sulfur-carbon composite material for all-solid-state lithium-sulfur battery by injecting sulfur through high-pressure gas phase method |
| CN115318248A (en) * | 2022-08-19 | 2022-11-11 | 宁夏华辉环保科技股份有限公司 | Accurate temperature-control sulfur-carrying activated carbon and preparation method thereof |
| CN115739018A (en) * | 2022-11-15 | 2023-03-07 | 中盐金坛盐化有限责任公司 | Preparation method and application of molten salt method sulfur modified porous material |
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