CN100335408C - Production of active carbon with Chinese chestnut - Google Patents

Production of active carbon with Chinese chestnut Download PDF

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Publication number
CN100335408C
CN100335408C CNB2005100191194A CN200510019119A CN100335408C CN 100335408 C CN100335408 C CN 100335408C CN B2005100191194 A CNB2005100191194 A CN B2005100191194A CN 200510019119 A CN200510019119 A CN 200510019119A CN 100335408 C CN100335408 C CN 100335408C
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temperature
chestnut shell
carbon
gac
active carbon
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CN1746107A (en
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刘理根
陈俊
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The present invention relates to a method for preparing active carbon from chestnut shells as raw materials. In the preparation method, dust and foreign matter of chestnut shells are cleaned, and the chestnut shells are dried at the temperature of 105 to 140 DEG C; the chestnut shells are ground into fine powder with the granularity of less than 0.053mm, and the fine powder is uniformly mixed with the water solution of zinc chloride with the concentration of 0.15 to 0.45 mol to be made into granules with the diameter of 4 to 5mm, or spherules with the specification; the granules or the spherules are moved in a charring furnace for carbonization under the condition of oxygen separation at the temperature of 380 to 680 DEG C for 200 to 240 minutes after the granules or the spherules are dried to eliminate water, and then are moved in a vertical activation furnace to be activated in an air stream with the temperature of 550 to 650 DEG C and the pressure of 0.08 to 0.15MPa for 30 to 45 minutes; activation products are washed for dezincification in the HCl water solution with the pH value of 2 to 2.5 and the temperature of 85 to 95 DEG C; the solid-liquid separation of the activation products is carried out, and water is added for washing into neutrality; solid materials are dried and dewatered, and are ground and graded finally; namely, the active carbon of ground granules, or the powdered activated carbon, or the spherical active carbon is obtained.

Description

The chestnut shell preparation method of active carbon
Technical field:
The present invention relates to the gac industrial process, particularly is the industrial process of feedstock production gac with the chestnut shell.
Background technology:
Gac is the black cellular solid, and unique pore texture makes it have very high specific surface area and surface functional group in the body, has good chemical stability, physical strength and performance such as acidproof, alkaline-resisting, heat-resisting.Organic or inorganic material in gas, the solution and colloidal solid all had very strong adsorptive power.Be widely used in solution decolorizing and refining, gas sweetening in the Chemical Manufacture, make catalyzer and support of the catalyst.Continuous expansion along with the gac purposes, demand increases day by day, the research of relevant gac is also deep further, around enhance product performance, increase range of application, the purpose that reduces production costs, aspects such as raw material type, preparation technology, product structure have been obtained a large amount of achievements both at home and abroad.The gac raw material is all carbon containing matters.Plant waste and agricultural shell slag all can be used for preparing gac, in industrial production, used as raw materials such as coconut husk, Pericarppium Armeniacae Amarum, nut-shell, corn cob, oil tea shell, camellia seed, oil palm shell, bagasse, tobacco rod, straw, Testa Viciae fabae, rice bar and cotton stalks, not only enrich the resource of drawing materials of gac greatly, also driven development of rural economy simultaneously.
Chestnut shell is a kind of agricultural byproducts waste material, piles up everywhere in the Chinese chestnut producing region, and except that minute quantity was used for peasant household's auxiliary fuel, main processing mode was to burn and abandon on the spot, has wasted resource at present, not only influences the also easy initiation fire of environment.Make raw material with chestnut shell, produce gac, make waste material obtain attached value utilization with absorption property, turn waste into wealth, turn bane into boon, resources advantage is changed into economic advantages, not only increased the gac raw material type but also alleviated the pressure of environmental purification, bigger economic worth and social effect had been arranged.
The chestnut shell gac is not seen the production instance report up to now.
In order to adapt to different purposes to the gac shape need, satisfy adsorption effect, at present, activated carbon variety has granular (spherical grain, rectangular grain, broken kernel), powdery and fibrous three kinds.The chestnut shell raw material is suitable for preparing spherical granulated carbon, broken granulated carbon and powdery carbon.
Summary of the invention:
The purpose of this invention is to provide a kind of is the feedstock production process of active carbon with the chestnut shell.
With the chestnut shell is that feedstock production process of active carbon step is as follows:
1st, chestnut shell is removed the dust foreign material, 105~140 ℃ of oven dry, be ground into granularity and be<0.053 fine powder, with concentration be that 0.15~0.45mol solder(ing)acid mixes, the add-on of liquor zinci chloridi is 45~75% of a chestnut shell fine powder quality, make the granular of diameter 4~5mm, perhaps directly make the peloid of specification with tablets press, drying removes moisture content;
2nd, step 1 drying removes the bulk goods behind the water, moves in the charring furnace, and charing is 200~240 minutes under 380~680 ℃ of temperature and oxygen barrier condition;
3rd, the bulk goods after step 2 charing changes activation furnace over to, 550~650 ℃ of temperature, activates 30~45 minutes in the superheated vapour air-flow of pressure 0.08~0.15MPa;
4th, with the HCl solution washing dezincify of 85~95 ℃ of pellet pH 2~2.5, temperature after step 3 activation, solid-liquid separates again, and it is clean to neutrality to add washing; the solid materials drying and dehydrating; last crushing and classification obtains broken kernel gac, powdered carbon, or the spherulitic gac.
Different varieties gac different fineness raw material, spherical granulated carbon, raw material granularity 90% is by 0.043~0.038mm; Broken granulated carbon and powdery carbon, raw material granularity 70% is by 0.053~0.043mm.
Chestnut shell be short texture, in the high carbon content material of flourishing capillary-size pore is arranged.The preparation gac, raw material need be crushed to certain fineness, and the size of granularity and charing intensity, activation effect and washing degree are the key problem in technology of chestnut shell gac.The pore texture of particle size influences finished particle inside, granulation mass density, physical strength and absorption property.Raw material granularity is thin more, and specific surface area is big more, and powder is easy to the activator dipping evenly, bonds easily between raw material powder and the activator, is easy to moulding; The particulate raw material also helps the formation of initial hole, and makes that particle surface after the moulding is more smooth, quality is finer and close, can guarantee that finished product has higher volume density and physical strength.Granularity is meticulous can to increase energy consumption, also makes troubles for production technique.The different varieties gac can be used the different fineness raw material.As spherical granulated carbon, raw material granularity requires 90% by 0.043~0.038mm; Broken granulated carbon and powdery carbon, raw material granularity 70% is by 0.053~0.043mm.
The chestnut shell carbonization temperature is low, the suitable first low temperature of carbonization process arrives the pyritous type of heating at a slow speed, Decomposition through differing temps, progressively remove water of constitution, gas and low-melting tar class volatile matter in the raw material, aliphatic side chains ruptures in succession, tar generated when the zinc chloride of interior hole path suppressed the raw material pyrolysis, thereby prevented to stop up its pyrogenous origin pore by tar, finally formed the netted solid carbon skeleton of high-specific surface area of special pore texture.
Activation is a gac perforate reaming process, is the important step that improves quality of activated carbon.The endoporus characteristics of enriching of chestnut shell, the activator zinc chloride is easy to immerse the interlayer deep along capillary channel, high temperature action during activation, the zinc chloride forced dehydration is added overfire air stream afterwards and is washed away outside the outlet orifice, promoted the perforate reaming effect of reactivation process, help improving the specific surface area and the reactive functionality feature of product, guarantee its good absorption property.
Washing process mainly reclaims zinc chloride, is the key that guarantees activated carbon product purity and reduce the zinc chloride process cost.Washing comprises salt acid treatment and two steps of washing, its objective is the removal of impurity, makes muriate contained in the gac, total iron cpd, ash content and pH value reach standard.Remove iron cpd with acid, add in the alkali and free acid, with hot water wash to there not being the chlorine root.The gac of cleaning is through dehydration, drying.
Embodiment:
Embodiment 1
The preparation of chestnut shell broken kernel gac and powdered carbon
Production process is as follows: chestnut shell is removed foreign material such as dust, 105~140 ℃ of oven dry, being ground into 70% granularity is the following fine powder of 0.053mm, mix with powerful mixer with the solder(ing)acid of concentration 0.15mol, the add-on of liquor zinci chloridi is 45% of a chestnut shell fine powder quality, make the granular of diameter 4~5mm, drying removes moisture content, move in the charring furnace, charing is 240 minutes under 380~680 ℃ of temperature and oxygen barrier condition, earlier be warmed up to 680 ℃ from 380 ℃, 680 ℃ of insulations 150 minutes with 200 ℃ speed per hour.Pellet after the charing changes vertical activation furnace over to; 550~650 ℃ of temperature; activation is 30 minutes in the overfire air stream of pressure 0.08~0.15MPa; then with pH 2,95 ℃ of aqueous hydrochloric acid washings of temperature dezincify; separate with the whizzer solid-liquid, and it is clean to neutral to add washing the solid materials drying and dehydrating; last crushing and classification obtains broken kernel gac, powdered carbon.
Embodiment 2
Chestnut shell Activated Carbon Production process is as follows: with foreign material such as chestnut shell flush away dust; 105~140 ℃ of oven dry; being ground into granularity is the following fine powder of 0.043mm; mix with powerful mixer with the liquor zinci chloridi of concentration 0.45mol; the add-on of solder(ing)acid is 60% of a chestnut shell fine powder quality; make the peloid of diameter 4~5mm; drying removes moisture content; move in the charring furnace; charing is 210 minutes under 380~680 ℃ of temperature and oxygen barrier condition; earlier be warmed up to 680 ℃ with 200 ℃ speed per hour from 380 ℃, 680 ℃ of insulations 120 minutes, the pellet after the charing changed vertical activation furnace over to; through 550~650 ℃ of temperature; activation is 45 minutes in the overfire air stream of pressure 0.08~0.15MPa, uses pH 2.5 then; 85 ℃ of hydrochloric acid soln washing dezincifys separate with the whizzer solid-liquid; and it is clean to neutral to add washing; the solid materials drying and dehydrating, last crushing and classification obtains the broken kernel gac; powdered carbon.
Embodiment 3
The preparation of chestnut shell broken kernel gac and powdered carbon
Production process is as follows: with foreign material such as chestnut shell flush away dust, 105~140 ℃ of oven dry, being ground into granularity is the following fine powder of 0.038mm, mix with powerful mixer with the solder(ing)acid of concentration 0.45mol, the add-on of liquor zinci chloridi is 75% of a chestnut shell fine powder quality, make the granular of diameter 4~5mm, drying removes moisture content, move in the charring furnace, charing is 200 minutes under 380~680 ℃ of temperature and oxygen barrier condition, earlier be warmed up to 680 ℃ from 380 ℃, 680 ℃ of insulations 110 minutes with 200 ℃ speed per hour.Pellet after the charing changes vertical activation furnace over to; 550~650 ℃ of temperature; activation is 45 minutes in the superheated vapour air-flow of pressure 0.08~0.15MPa; then with pH 2,90 ℃ of hydrochloric acid soln washings of temperature dezincify; separate with the whizzer solid-liquid, and it is clean to neutral to add washing the solid materials drying and dehydrating; last crushing and classification obtains broken kernel gac, powdered carbon.
Embodiment 4
The preparation of chestnut shell peloid gac
Production process is as follows: with foreign material such as chestnut shell flush away dust; 105~140 ℃ of oven dry; being ground into 90% granularity is the following fine powder of 0.043mm; mix with powerful mixer with the solder(ing)acid of concentration 0.15mol; the add-on of solder(ing)acid is 45% of a chestnut shell fine powder quality, is made the spherical grain that needs specification by tablets press.The pellet drying removes moisture content, moves in the charring furnace, and charing is 240 minutes under 380~680 ℃ of temperature and oxygen barrier condition, is warmed up to 680 ℃ with 200 ℃ speed per hour from 380 ℃ earlier, 680 ℃ of insulations 150 minutes.Pellet after the charing changes vertical activation furnace over to, 550~650 ℃ of temperature, activation is 30 minutes in the superheated vapour air-flow of pressure 0.08~0.15MPa, then with pH 2,85 ℃ of hydrochloric acid soln washings of temperature dezincify, separate with the whizzer solid-liquid, and it is clean to neutral to add washing the solid materials drying and dehydrating, last crushing and classification obtains the ball shape gac.
Embodiment 5
The preparation of chestnut shell peloid gac
Production process is as follows: with foreign material such as chestnut shell flush away dust; 105~140 ℃ of oven dry; being ground into granularity is the following fine powder of 0.038mm; mix with powerful mixer with the solder(ing)acid of concentration 0.45mol; the add-on of liquor zinci chloridi is 75% of a chestnut shell fine powder quality, is made the spherical grain that needs specification by tablets press.The pellet drying removes moisture content, moves in the charring furnace, and charing is 200 minutes under 380~680 ℃ of temperature and oxygen barrier condition, is warmed up to 680 ℃ with 200 ℃ speed per hour from 380 ℃ earlier, 680 ℃ of insulations 110 minutes.Pellet after the charing changes vertical activation furnace over to, 550~650 ℃ of temperature, activation is 30 minutes in the superheated vapour air-flow of pressure 0.08~0.15MPa, then with pH 2.5,90 ℃ of hydrochloric acid soln washings of temperature dezincify, separate with the whizzer solid-liquid, and it is clean to neutral to add washing the solid materials drying and dehydrating, last crushing and classification obtains the ball shape gac.

Claims (2)

1, a kind of is the feedstock production process of active carbon with the chestnut shell, it is characterized in that step is as follows:
1st, chestnut shell is removed the dust foreign material, 105~140 ℃ of oven dry, be ground into the fine powder of granularity for<0.053mm, with concentration be that 0.15~0.45mol solder(ing)acid mixes, the add-on of liquor zinci chloridi is 45~75% of a chestnut shell fine powder quality, make the granular of diameter 4~5mm, perhaps directly make the peloid of specification with tablets press, drying removes moisture content;
2nd, the pellet that step 1 drying is removed behind the water moves in the charring furnace, and charing is 200~240 minutes under 380~680 ℃ of temperature and oxygen barrier condition;
3rd, change the pellet after step 2 charing over to activation furnace,, activate 30~45 minutes in the superheated vapour air-flow of pressure 0.08~0.15MPa 550~650 ℃ of temperature;
4th, with the HCl solution washing dezincify of the pellet after step 3 activation with pH2-2.5, temperature 85-95 ℃, solid-liquid separates again, and it is clean to neutral to add washing; the solid materials drying and dehydrating; last crushing and classification obtains broken kernel gac, powdered carbon, or the spherulitic gac.
2, as claimed in claim 1 is the feedstock production process of active carbon with the chestnut shell, and when it is characterized in that doing the spherulitic charcoal, chestnut shell powder degree 90% is by 0.043~0.038mm; When doing broken granulated carbon and powdery carbon, chestnut shell powder degree 70% is by 0.053~0.043mm.
CNB2005100191194A 2005-07-19 2005-07-19 Production of active carbon with Chinese chestnut Expired - Fee Related CN100335408C (en)

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CN100509143C (en) 2006-05-19 2009-07-08 张大伟 Method for treating saturated active coke
CN101892106B (en) * 2010-07-01 2013-05-08 东华大学 Method for preparing chestnut shell-based biomass charcoal with loose and porous structure
CN102774835A (en) * 2012-07-16 2012-11-14 太仓市联林活性炭厂 Preparation method of chestnut shell activated carbon
CN102745688A (en) * 2012-07-18 2012-10-24 太仓市联林活性炭厂 Process for preparing bamboo shoot shell based activated carbon by means of zinc chloride activation method
CN103165910A (en) * 2013-03-28 2013-06-19 中国科学院城市环境研究所 Method for preparing bioelectrochemistry system electrode by utilizing chestnut shells
CN103641118B (en) * 2013-12-26 2015-06-17 南京林业大学 Production method of producing active carbon with high specific surface area by composite activator
CN104087326B (en) * 2014-07-26 2016-06-22 安徽科技学院 A kind of method preparing charcoal for raw material wet method thermal cracking with agricultural organic solid waste
CN105776203A (en) * 2014-12-22 2016-07-20 重庆雪瑞盛泉农业开发有限公司 Method for preparing chestnut shell activated carbon
CN105602589A (en) * 2015-11-16 2016-05-25 湖南莎丽袜业股份有限公司 Preparation method of high-activity machine-made bamboo charcoal
CN106276890A (en) * 2016-07-14 2017-01-04 旌德县龙强净化材料厂 A kind of be raw material production activated carbon with Semen Caryae Cathayensis shell method
CN106241796A (en) * 2016-07-14 2016-12-21 旌德县龙强净化材料厂 A kind of method utilizing Exocarpium cocois (Cocos nucifera L) to prepare activated carbon
CN106179207A (en) * 2016-07-14 2016-12-07 旌德县龙强净化材料厂 A kind of method utilizing agriculture and forestry organic waste material Semen Castaneae thorn shell to prepare activated carbon
CN111972706A (en) * 2020-08-27 2020-11-24 广西中烟工业有限责任公司 Preparation method of chestnut shell activated carbon binary composite flavored filter stick
CN113178339A (en) * 2021-05-14 2021-07-27 西南大学 Broad bean shell derived activated carbon material for super capacitor and preparation method and application thereof

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