CN102120178A - Active semicoke adsorbing agent and preparation method thereof - Google Patents
Active semicoke adsorbing agent and preparation method thereof Download PDFInfo
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- CN102120178A CN102120178A CN 201110036170 CN201110036170A CN102120178A CN 102120178 A CN102120178 A CN 102120178A CN 201110036170 CN201110036170 CN 201110036170 CN 201110036170 A CN201110036170 A CN 201110036170A CN 102120178 A CN102120178 A CN 102120178A
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Abstract
The invention discloses a preparation method of an active semicoke adsorbing agent, which comprises the steps of: preprocessing semicoke as a raw material, i.e. crushing and screening the semicoke as the raw material; selecting particles with a certain size; washing the selected particles with deionized water for multiple times for removing fine powder therein, drying at high temperature until reaching constant weight; and carrying out HNO3 activation, KOH activation and heating water thermochemical activation on the particles sequentially, washing the activated particles with deionized water to be neutral, drying at high temperature until reaching constant weight, and finally obtaining the active semicoke adsorbing agent. The invention has the advantages of wide source of raw materials and simple preparation process; the obtained adsorbing agent can better replace active carbon; and experiments prove that the adsorbing agent has better adsorbing effect on methylbenzene, absorbing capacity of reaching 207g methylbenzene/g C, and no secondary pollution in the whole preparation process, and accords with the environment protection idea.
Description
Technical field
The present invention relates to a kind of active carbocoal preparation of adsorbent method, relate in particular to and a kind ofly can substitute the active carbocoal preparation of adsorbent method that active carbon is used for the purifying volatile industrial organic exhaust gas.
Background technology
At present, utilize active carbon to handle in the industrial organic exhaust gas for adsorbent and be most widely used, but active carbon exists following shortcoming: (1) adsorption capacity is low, in use needs frequent the replacing or regeneration, makes troubles to operational administrative; (2) cost is higher, and frequent replacing has increased operating cost greatly; (3) can not realize basic regeneration, must cause regenerating not exclusively and the handling problem of the organic exhaust gas of regeneration.
Semicoke is the flammable solid product by coal low temperature distillation gained, and its main component is carbon, ash content and volatile matter.Compare with active carbon, its volatile matter content height, porosity is big, has stronger reactivity with carbon monoxide, steam etc.Resident's gas engineering of provinces such as China Shanxi, Shaanxi adopts upright furnace gas making more, a large amount of semicokes of by-product, and pile up like a mountain for these semicokes, serious environment pollution.Therefore, utilize angle to consider, demand developing the new approaches and the new product of these semicokes urgently from environment and clean coal technology.The present invention is conceived to improve the preparation method and the system of active carbocoal, improves its adsorptivity to organic exhaust gas.
Summary of the invention
In order to solve above-mentioned defective of the prior art, the invention provides and a kind ofly improve adsorption capacity, realize regeneration, reduce cost and realize the semicoke preparation of adsorbent method that waste product utilizes again.
For achieving the above object, the present invention has adopted following technical scheme.
A kind of active carbocoal preparation of adsorbent method is characterized in that, comprising:
Wherein, the temperature of hyperthermia drying is 110 ℃.
Wherein, described a certain size particle is a 10-20 purpose particle.
Wherein, described HNO
3The step of activation is: be 45% HNO in concentration with described particle
3In the solution, under 80 ℃ temperature, soaked 4 hours.
Wherein, the step of described KOH activation is: described particle in the KOH of 0.1mol/L solution, under 80 ℃ temperature, was soaked 4 hours.
A kind of active carbocoal adsorbent is characterized in that: its specific area is 555.56m
2/ g, iodine number is 811.38mg/g, surperficial soda acid total amount is 0.8649mmol/g.
The invention has the beneficial effects as follows: raw material sources are extensive, and preparation process is simple, and cost is low, and integrated cost only is about 1/3rd of an active carbon; The adsorbent of gained can well substitute active carbon, the experiment proved that the adsorption effect of toluene fine, adsorption capacity reaches 207mg toluene/gC, and is approaching to the absorption property of toluene with active carbon, and avoided using active carbon to need the drawback of repeated regeneration and replacing; Adsorb the modified semicoke behind a large amount of organic exhaust gas, its fugitive constituent and calorific value all increase, and can mix with raw coal and mix burning, as circulating fluidized bed boiler fuel, have realized that really " complete alternation " do not have any pollution, reach " zero-emission " target; Non-secondary pollution in the preparation process, nitric acid and KOH can be by recycling and reusing, and environmental protection is significant; On the basis of semicoke, improve its absorption property to VOC by physics, chemical modification, compare before active carbocoal after the modification and the modification, its pore-size distribution is more optimized, specific area improves more than 30%, improves more than 30% to the absorption property of the pollution components such as benzene,toluene,xylene among the VOCs.
Description of drawings
Fig. 1 is a semicoke adsorbent preparation method flow chart of the present invention;
Wherein: the 1-pretreatment unit; The 2-Constant Temp. Oven; The 3-thermostat water bath; The 4-autoclave; The HNO of 5-45%
3Solution; 6-0.1mol/L KOH solution.
The specific embodiment
Below, the invention will be further described in conjunction with the accompanying drawings and embodiments.
A kind of active carbocoal preparation of adsorbent method includes following steps, and the raw material semicoke is carried out preliminary treatment; Described preliminary treatment is that the raw material semicoke is pulverized, sieved, and chooses wherein a certain size particle, is preferably 10-20 purpose particle herein; To the described particle chosen repeatedly, be generally three times and get final product, in order to remove fine powder wherein with deionized water rinsing; With the flushing after particle in Constant Temp. Oven hyperthermia drying to constant weight; Next, it is carried out HNO successively
3Activation and oven dry, KOH activation and oven dry and activation of heating hydrothermal chemistry and oven dry.
Described HNO
3The step of activation is: be 45% HNO in concentration with described particle
3In the solution, under 80 ℃ temperature, soaked 4 hours; To spend deionised water through the particle of overactivation to neutral, wash afterwards in Constant Temp. Oven hyperthermia drying to constant weight.
The step of described KOH activation is: described particle in the KOH of 0.1mol/L solution, under 80 ℃ temperature, was soaked 4 hours; To spend deionised water through the particle of overactivation to neutral, wash afterwards in Constant Temp. Oven hyperthermia drying to constant weight.
Described HNO
3Activation and KOH activation step all are to finish in thermostat water bath.
The step of described heating hydrothermal chemistry activation is: particle is mixed with 1: 3 ratio with water in autoclave, under 280 ℃ temperature, depress at 65 normal atmospheres, the admixture activation time is 2 hours; To spend deionised water through the particle of overactivation to neutral, wash afterwards in Constant Temp. Oven hyperthermia drying to constant weight.
The temperature of above-mentioned hyperthermia drying is 110 ℃.
Through just having obtained the active carbocoal adsorbent behind above-mentioned pre-treatment step and the various activation step, the specific area of this active carbocoal adsorbent is 555.56m
2/ g, iodine number is 811.38mg/g, surperficial soda acid total amount is 0.8649mmol/g.
Claims (8)
1. an active carbocoal preparation of adsorbent method is characterized in that, comprising:
Step 1, the raw material semicoke is carried out preliminary treatment; Described preliminary treatment is that the raw material semicoke is pulverized, sieved, and chooses wherein a certain size particle;
Step 2, to the described particle chosen with deionized water rinsing repeatedly in order to removing fine powder wherein, and is dried to constant weight under the high temperature;
Step 3, described particle is carried out HNO
3Activation activated particles is spent deionised water to neutral, and hyperthermia drying is to constant weight;
Step 4, described particle is carried out KOH activation, activated particles is spent deionised water to neutral, and hyperthermia drying is to constant weight;
Step 5, described particle is heated hydrothermal chemistry activation, activated particles is spent deionised water to neutral, and hyperthermia drying is to constant weight; The described active carbocoal adsorbent of final acquisition.
2. a kind of active carbocoal preparation of adsorbent method as claimed in claim 1, it is characterized in that: the temperature of hyperthermia drying is 110 ℃.
3. a kind of active carbocoal preparation of adsorbent method as claimed in claim 1 is characterized in that: described a certain size particle is a 10-20 purpose particle.
4. a kind of active carbocoal preparation of adsorbent method as claimed in claim 1 is characterized in that: described HNO
3The step of activation is: be 45% HNO in concentration with described particle
3In the solution, under 80 ℃ temperature, soaked 4 hours.
5. as claim 1 or 4 described a kind of active carbocoal preparation of adsorbent methods, it is characterized in that: the step of described KOH activation is: described particle in the KOH of 0.1mol/L solution, under 80 ℃ temperature, was soaked 4 hours.
6. a kind of active carbocoal preparation of adsorbent method as claimed in claim 1, it is characterized in that: the step of described heating hydrothermal chemistry activation is: particle is mixed with 1: 3 ratio with water in autoclave, under 280 ℃ temperature, depress at 65 normal atmospheres, the admixture activation time is 2 hours.
7. a kind of active carbocoal preparation of adsorbent method as claimed in claim 5, it is characterized in that: the step of described heating hydrothermal chemistry activation is: particle is mixed with 1: 3 ratio with water in autoclave, under 280 ℃ temperature, depress at 65 normal atmospheres, the admixture activation time is 2 hours.
8. active carbocoal adsorbent, it is characterized in that: its specific area is 555.56m
2/ g, iodine number is 811.38mg/g, surperficial soda acid total amount is 0.8649mmol/g.
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Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102600800A (en) * | 2012-04-06 | 2012-07-25 | 昆明理工大学 | Preparation method of semi-coke adsorbent |
CN103253776A (en) * | 2013-05-28 | 2013-08-21 | 武汉钢铁(集团)公司 | Semi-coke microbial carrier and preparation method thereof |
CN104525113A (en) * | 2014-12-26 | 2015-04-22 | 合肥工业大学 | Method for preparing adsorbent by using semi-coke modification |
CN105174350A (en) * | 2015-09-07 | 2015-12-23 | 延安大学 | Method of treating phenolic wastewater by adopting magnetic semicoke adsorbent |
CN106010601A (en) * | 2016-06-01 | 2016-10-12 | 湖南农业大学 | Biochar prepared from banana peel, preparation method and application thereof |
CN106622124A (en) * | 2016-11-29 | 2017-05-10 | 西安科技大学 | High-adsorbability activated semi-coke as well as preparation method and application thereof |
CN106669601A (en) * | 2016-11-29 | 2017-05-17 | 西安科技大学 | High-absorbability activated semi-coke and preparation method and application thereof |
CN108273474A (en) * | 2018-02-14 | 2018-07-13 | 福建农林大学 | A kind of preparation method of modified activated carbon of the surface rich in phenolic hydroxyl group |
CN109225129A (en) * | 2017-07-11 | 2019-01-18 | 内蒙古大学 | A kind of production method of the preceding modified microballoon functionality straw charcoal of hydro-thermal preparation |
CN109603752A (en) * | 2019-01-14 | 2019-04-12 | 中国科学院兰州化学物理研究所 | The method for preparing heavy metal-polluted soil curing materials using oil shale semi-coke |
CN110465265A (en) * | 2018-05-11 | 2019-11-19 | 萍乡市华星环保工程技术有限公司 | Organic waste-gas adsorbant and preparation method thereof |
CN111167407A (en) * | 2020-01-16 | 2020-05-19 | 陕西科技大学 | Semi-coke activated carbon adsorbent, KOH alkali fusion preparation method thereof and application of semi-coke activated carbon adsorbent in removing tetracycline in water |
CN111591986A (en) * | 2020-04-10 | 2020-08-28 | 山东大学 | Plant VOCs treatment method and system based on petrochemical enterprise byproduct petroleum coke upgrading utilization |
CN111715187A (en) * | 2020-07-14 | 2020-09-29 | 陕西煤业化工技术研究院有限责任公司 | Coal pyrolysis semicoke adsorption material and preparation method and application thereof |
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CN102600800A (en) * | 2012-04-06 | 2012-07-25 | 昆明理工大学 | Preparation method of semi-coke adsorbent |
CN103253776A (en) * | 2013-05-28 | 2013-08-21 | 武汉钢铁(集团)公司 | Semi-coke microbial carrier and preparation method thereof |
CN103253776B (en) * | 2013-05-28 | 2014-11-12 | 武汉钢铁(集团)公司 | Semi-coke microbial carrier and preparation method thereof |
CN104525113A (en) * | 2014-12-26 | 2015-04-22 | 合肥工业大学 | Method for preparing adsorbent by using semi-coke modification |
CN105174350B (en) * | 2015-09-07 | 2017-10-24 | 延安大学 | Using the method for magnetic semi-coke adsorbent Phenol-Containing Wastewater Treatment |
CN105174350A (en) * | 2015-09-07 | 2015-12-23 | 延安大学 | Method of treating phenolic wastewater by adopting magnetic semicoke adsorbent |
CN106010601A (en) * | 2016-06-01 | 2016-10-12 | 湖南农业大学 | Biochar prepared from banana peel, preparation method and application thereof |
CN106622124A (en) * | 2016-11-29 | 2017-05-10 | 西安科技大学 | High-adsorbability activated semi-coke as well as preparation method and application thereof |
CN106669601A (en) * | 2016-11-29 | 2017-05-17 | 西安科技大学 | High-absorbability activated semi-coke and preparation method and application thereof |
CN109225129A (en) * | 2017-07-11 | 2019-01-18 | 内蒙古大学 | A kind of production method of the preceding modified microballoon functionality straw charcoal of hydro-thermal preparation |
CN108273474A (en) * | 2018-02-14 | 2018-07-13 | 福建农林大学 | A kind of preparation method of modified activated carbon of the surface rich in phenolic hydroxyl group |
CN110465265A (en) * | 2018-05-11 | 2019-11-19 | 萍乡市华星环保工程技术有限公司 | Organic waste-gas adsorbant and preparation method thereof |
CN109603752A (en) * | 2019-01-14 | 2019-04-12 | 中国科学院兰州化学物理研究所 | The method for preparing heavy metal-polluted soil curing materials using oil shale semi-coke |
CN109603752B (en) * | 2019-01-14 | 2021-12-31 | 中国科学院兰州化学物理研究所 | Method for preparing soil heavy metal solidified material by using oil shale semicoke |
CN111167407A (en) * | 2020-01-16 | 2020-05-19 | 陕西科技大学 | Semi-coke activated carbon adsorbent, KOH alkali fusion preparation method thereof and application of semi-coke activated carbon adsorbent in removing tetracycline in water |
CN111591986A (en) * | 2020-04-10 | 2020-08-28 | 山东大学 | Plant VOCs treatment method and system based on petrochemical enterprise byproduct petroleum coke upgrading utilization |
CN111591986B (en) * | 2020-04-10 | 2022-03-11 | 山东大学 | Plant VOCs treatment method and system based on petrochemical enterprise byproduct petroleum coke upgrading utilization |
CN111715187A (en) * | 2020-07-14 | 2020-09-29 | 陕西煤业化工技术研究院有限责任公司 | Coal pyrolysis semicoke adsorption material and preparation method and application thereof |
CN111715187B (en) * | 2020-07-14 | 2023-09-22 | 陕西煤业化工技术研究院有限责任公司 | Coal pyrolysis semicoke adsorption material and preparation method and application thereof |
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Application publication date: 20110713 |