CN104003386A - Method for preparing powder active carbon by taking cow dung as raw material - Google Patents

Method for preparing powder active carbon by taking cow dung as raw material Download PDF

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Publication number
CN104003386A
CN104003386A CN201410248431.XA CN201410248431A CN104003386A CN 104003386 A CN104003386 A CN 104003386A CN 201410248431 A CN201410248431 A CN 201410248431A CN 104003386 A CN104003386 A CN 104003386A
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China
Prior art keywords
cow dung
raw material
activating agent
composite activating
gac
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CN201410248431.XA
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Chinese (zh)
Inventor
沈泽文
曹奥运
刘廷凤
陈文栋
陈亚南
甘瑜威
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Nanjing Institute of Technology
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Nanjing Institute of Technology
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Abstract

The invention discloses a method for preparing powder active carbon by taking cow dung as a raw material. The method is as follows: by taking the cow dung as the raw material, carrying out activation for 24 hours by a composite activator formed by mixing phosphoric acid and phosphate, and then carbonizing at a high temperature. According to the invention, livestock breeding waste-cow dung is mainly utilized as the raw material, and is sufficient in source, easy to purchase and low in price; the composite activator is relatively low in price and can be recycled in different degrees; the method for using the activator to activate the cow dung and then carbonizing radically solves influences and damage of the cow dung on environment; the prepared active carbon can be directly and practically applied to satisfy various needs on active carbon, so that waste is changed into things of value, and therefore, the method has remarkable social and economic benefits, and very good commercial application prospect.

Description

A kind of method of preparing powdered carbon taking cow dung as raw material
Technical field
The invention belongs to the preparation field of gac, it is particularly related to a kind of multiplicity reactivation method that adopts and processes cow dung, is prepared into the method for gac.
Background technology
Along with the fast development of livestock breeding industry, the movement of animal is on the rise to the pollution situation of environment, and particularly the element environmental pollution such as the nitrogen in movement, phosphorus, iron, zinc and copper is especially serious.And above-mentioned material has certain long-term accumulation to the pollution of environment, in the time that they run up to certain degree in environment, can cause Soil degradation, crop yield declines, and by by runoff, leaching loss effect polluted surface water and underground water, ecotope is caused to great harm.And wherein cow dung is one of main movement, a head of cattle approximately 20 kg that will void excreta for a day, will have 7000 kg many for 1 year, and output is huge.Caused from government at this point, dairy cow farm owner, the showing great attention to and paying attention to of the each side such as researcher, in succession develop multiple different countermeasure, but different countermeasures has certain limitation suitability for different plants, therefore select the processing mode of correct livestock and poultry cultivation ight soil just to become the key point that solves its environmental pollution problem.
Gac is a kind of traditional carbon material, it has flourishing pore texture and huge specific surface area, and contain the properties such as good decolouring, deodorizing, absorption, be therefore subject to people to pay close attention to for a long time, and gac is all applied widely in all fields.Along with expanding economy, countries in the world are increasing to the demand of gac, and development prospect is very wide.
Summary of the invention
The object of this invention is to provide one taking cow dung as raw material, adopt multiplicity reactivation method to be prepared into the method for powdered carbon.Realize the recycling that cow dung is turned waste into wealth.
The present invention is achieved through the following technical solutions:
A method of preparing powdered carbon taking cow dung as raw material, comprises the following steps:
(1) cow dung is shone after dry doubling sieves and put into container, for subsequent use;
(2) by the cow dung of drying and composite activating agent hybrid infusion, the mass ratio of cow dung and this composite activating agent is 0.14:1 ~ 0.1:1, dipping time 24 hours; Wherein composite activating agent is the mixture of phosphoric acid and potassium primary phosphate;
(3) cow dung of dipping composite activating agent is carried out to burning carbonate 1-3 hour under the oxygen free condition of 400 ~ 800 DEG C, obtain gac;
(4) gac of acquisition is filtered to filtrate pH with distilled water wash and is neutral, then 105 DEG C of oven dry, then grind, sieve and obtain 100 ~ 200 object powdered active carbons.
Wherein described in step (1), cow dung is shone to dry doubling and can be screened to 0.9mm.
Cow dung described in step (2) can be 1:9 with the impregnating effect ratio of composite activating agent.
The phosphoric acid of composite activating agent and the mass ratio of potassium primary phosphate described in step (2) can be 20:1.
The temperature of carrying out burning carbonate described in step (3) under oxygen free condition can be 700 DEG C.
The burning carbonate time described in step (3) can be 1.5 hours.
The temperature of the distilled water described in step (4) can be room temperature.
beneficial effect
(1) the present invention uses cow dung as starting material, substitutes that existing other is wooden, the raw materials such as coal.Not only raw material sources are extensive, be easy to get, and also with low cost, both fundamentally solve the problem of environmental pollution of cow dung, reduce again the consumption of the disposable energy.
(2) raw materials for production of gac are cow dung, the activator using for phosphoric acid and phosphoric acid be the composite activating agent that thing is mixed into, compare the gac that generally the business gac of use and alone phosphoric acid are made as activator at present and there is higher yield and better absorption property, determine the best applications ratio of component in composite activating agent simultaneously, made the cow dung Properties of Activated Carbon finally obtaining obtain further raising.
(3) cost of the present invention is low, and corrodibility is low, and environmental pollution is little, is the recycling of refuse; Technical process is simple, can carry out suitability for industrialized production, both be livestock waste-cow dung, new recycling approach is provided, the disposable energy such as coal are saved again, also open up new source direction for the preparation of gac, can meet each side to the ever-increasing market requirement of gac, there is higher economic benefit and social benefit; Gac prepared by cow dung can decolour rapidly and adsorbent solution in the pollutent such as heavy metal ion, can fundamentally solve cow dung and pile up the pollution problem to environment, have a good application prospect.
brief description of the drawings:
Fig. 1 is raw material cow dung scanning electron microscope (SEM) photograph;
Fig. 2 is the cow dung gac scanning electron microscope (SEM) photograph that phosphoric acid method makes;
Fig. 3 is the cow dung gac scanning electron microscope (SEM) photograph that embodiment 3 composite activator methods make.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Yield in example of the present invention, is the ratio of product quality and raw materials quality, and its formula is:
Wherein, m productand m raw materialrepresent respectively the quality of product and raw material.
Iodine number in example of the present invention according to: National Standard of the People's Republic of China GB/T12496.8-1999 mono-wood activated charcoal measuring method is measured iodine sorption value.
Methylene blue value in example of the present invention according to: National Standard of the People's Republic of China's GB/T12496.10-1999-wood activated charcoal measuring method is measured methylene blue adsorption value.
Described in embodiment 4, contrast in other gac, other gac is prepared cow dung gac under business gac and the phosphoric acid method optimum process that openly searches.The data of surveying all under equal conditions complete.
The chromium solution being adsorbed in example of the present invention is that chromium content concn is the potassium bichromate solution of 100mg/L, and the dye solution being adsorbed is that concentration is the reactive brilliant blue solution of 300mg/L.
Adsorption conditions in example of the present invention: dosage is 6g/L, pH is 6, temperature is 25 DEG C of room temperatures.
In following examples, composite activating agent is 20:1 composition by the mass ratio of phosphoric acid and potassium primary phosphate.
Embodiment 1
Choose the cow dung of 0.5kg as raw material, shining dry doubling is screened to after 0.9 mm, put it in container and carry out hybrid infusion with composite activating agent, wherein the dipping ratio of cow dung and composite activating agent is 1:9, after 24 hours flood, container is transferred in retort furnace, anaerobic charing 1 h at the temperature of 700 DEG C, the distilled water that is room temperature by temperature is more afterwards dry in 105 DEG C after being washed till neutrality, then grinding and be sized to 200 orders, is 56% cow dung gac thereby obtain yield.Measuring its iodine number is 775.97mg/g, and methylene blue adsorption value is 127mg/g.Being 95.67% to the clearance of chromium solution, is 94.30% to the percent of decolourization of dyestuff.
Embodiment 2
Choose the cow dung of 0.5kg as raw material, shining dry doubling is screened to after 0.9 mm, put it in container and carry out hybrid infusion with composite activating agent, wherein the dipping ratio of cow dung and composite activating agent is 1:10, container was transferred in retort furnace after dipping through 24 hours, be washed till neutrality with the distilled water that temperature is room temperature again after anaerobic charing 1.5 h at the temperature of 600 DEG C after in 105 DEG C dry, then grind and be sized to 200 orders, be 50% cow dung gac thereby obtain yield.Measuring its iodine number is 792.48mg/g, and methylene blue adsorption value is 136.25mg/g.Being 98.53% to the clearance of chromium solution, is 98.15% to the percent of decolourization of dyestuff.
Embodiment 3
Choose the cow dung of 0.5kg as raw material, shining dry doubling is screened to after 0.9 mm, put it in container and carry out hybrid infusion with composite activating agent, wherein the dipping ratio of cow dung and composite activating agent is 1:9, after dipping, container is transferred in retort furnace through 24 hours, anaerobic charing 1.5 h at the temperature of 700 DEG C, are washed till after neutrality and are dried in 105 DEG C with the distilled water that temperature is room temperature more afterwards, then grinding and be sized to 200 orders, is 52% cow dung gac thereby obtain yield.Measuring its iodine number is 862.33mg/g, and methylene blue adsorption value is 145.86mg/g.Being 100% to the clearance of chromium solution, is 99.84% to the percent of decolourization of dyestuff.
Embodiment 4
Choose the cow dung of 1kg as raw material, shining dry doubling is screened to after 0.9 mm, put it in container and carry out hybrid infusion with composite activating agent, wherein the dipping ratio of cow dung and composite activating agent is 1.4:10, after dipping, container is transferred in retort furnace through 24 hours, anaerobic charing 3 h at the temperature of 600 DEG C, are washed till after neutrality and are dried in 105 DEG C with the distilled water that temperature is room temperature more afterwards, then grinding and be sized to 100 orders, is 55% cow dung gac thereby obtain yield.Measuring its iodine number is 851.62mg/g, and methylene blue adsorption value is 132.53mg/g.Being 98.76% to the clearance of chromium solution, is 97.84% to the percent of decolourization of dyestuff.
Embodiment 5
Choose the cow dung of 1kg as raw material, shining dry doubling is screened to after 0.9 mm, put it in container and carry out hybrid infusion with composite activating agent, wherein the dipping ratio of cow dung and composite activating agent is 1:8, after 24 hours flood, container is transferred in retort furnace, anaerobic charing 2 h at the temperature of 800 DEG C, are washed till neutral dry afterwards again with the distilled water that temperature is room temperature, grinding is sized to 180 orders, is 54% cow dung gac thereby obtain yield.Measuring its iodine number is 846.58mg/g, and methylene blue adsorption value is 126.47mg/g.Being 98.25% to the clearance of chromium solution, is 97.65% to the percent of decolourization of dyestuff.
Can be drawn by above embodiment, the cow dung Properties of Activated Carbon that embodiment 3 prepares is best, the most optimum embodiment.
Comparative example 1
Preparation method and process be with embodiment 3, only changed the mass ratio of phosphoric acid and potassium primary phosphate in composite activating agent.
Choose the cow dung of 0.5kg as raw material, shining dry doubling is screened to after 0.9 mm, put it in container and carry out hybrid infusion with composite activating agent, wherein in composite activating agent, the mass ratio of phosphoric acid and potassium primary phosphate is 10:1, the dipping ratio of cow dung and composite activating agent is 1:9, container was transferred in retort furnace after dipping through 24 hours, anaerobic charing 1.5 h at the temperature of 700 DEG C, after being washed till neutrality with the distilled water that temperature is room temperature more afterwards, be dried in 105 DEG C, then grinding and be sized to 200 orders, is 46% cow dung gac thereby obtain yield.Measuring its iodine number is 728.55mg/g, and methylene blue adsorption value is 119.32mg/g.Being 89% to the clearance of chromium solution, is 92.16% to the percent of decolourization of dyestuff.
Comparative example 2
Preparation method and process be with embodiment 3, only changed the mass ratio of phosphoric acid and potassium primary phosphate in composite activating agent.
Choose the cow dung of 0.5kg as raw material, shining dry doubling is screened to after 0.9 mm, put it in container and carry out hybrid infusion with composite activating agent, wherein in composite activating agent, the mass ratio of phosphoric acid and potassium primary phosphate is 25:1, the dipping ratio of cow dung and composite activating agent is 1:9, container was transferred in retort furnace after dipping through 24 hours, anaerobic charing 1.5 h at the temperature of 700 DEG C, after being washed till neutrality with the distilled water that temperature is room temperature more afterwards, be dried in 105 DEG C, then grinding and be sized to 200 orders, is 49% cow dung gac thereby obtain yield.Measuring its iodine number is 741.20mg/g, and methylene blue adsorption value is 121.68mg/g.Being 90% to the clearance of chromium solution, is 93.68% to the percent of decolourization of dyestuff.
Can be found out by above two simultaneous tests, after the component ratio in composite activating agent changes, the cow dung Properties of Activated Carbon obtaining has obtained larger decline, and as can be seen here, in composite activating agent, the ratio of component has very important impact to the finished product performance.
Carry out simultaneous test with other gac:
Business gac iodine number is 652.94mg/g, and methylene blue adsorption value is 103.75mg/g, is 65.72% to the clearance of chromium solution, and dye decolored rate is 83.52%.
The yield of the prepared cow dung gac of phosphoric acid method is 47%, and iodine number is 734.19mg/g, and methylene blue adsorption value is 108.20mg/g, is 75.84% to the clearance of chromium solution, and dye decolored rate is 92.75%.
Can find out from above testing data, cow dung gac provided by the invention is compared the gac that generally the business gac of use and alone phosphoric acid are made as activator at present and is had higher yield and better absorption property.
Fig. 1 is the scanning electron microscope (SEM) photograph of raw material cow dung, can find out that cow dung surface is dense, can play adsorbing aperture very little; Fig. 2 is the prepared cow dung gac of above phosphoric acid method scanning electron microscope (SEM) photograph, can obviously find out, its surface exists polynuclear plane, but cellular less, and arrangement is more mixed and disorderly, there is no rule; Fig. 3 is the cow dung gac scanning electron microscope (SEM) photograph that embodiment 3 composite activator methods make, can find out that its surface exists evenly distributed polynuclear plane, and surface is cellular, therefore can find out by contrast, the cow dung gac that embodiment 3 makes by composite activator method has better adsorption.

Claims (7)

1. a method of preparing powdered carbon taking cow dung as raw material, is characterized in that, comprises the following steps:
(1) cow dung is shone after dry doubling sieves and put into container, for subsequent use;
(2) by the cow dung of drying and composite activating agent hybrid infusion, the mass ratio of cow dung and this composite activating agent is 0.14:1 ~ 0.1:1, dipping time 24 hours; Wherein composite activating agent is the mixture of phosphoric acid and potassium primary phosphate;
(3) cow dung of dipping composite activating agent is carried out to burning carbonate 1-3 hour under the oxygen free condition of 400 ~ 800 DEG C, obtain gac;
(4) gac of acquisition is filtered to filtrate pH with distilled water wash and is neutral, then 105 DEG C of oven dry, then grind, sieve and obtain 100 ~ 200 object powdered active carbons.
2. a kind of method of preparing powdered carbon taking cow dung as raw material according to claim 1, is characterized in that, described in step (1), cow dung is shone to dry doubling and is screened to 0.9mm.
3. a kind of method of preparing powdered carbon taking cow dung as raw material according to claim 1, is characterized in that, cow dung described in step (2) is 1:9 with the impregnating effect ratio of composite activating agent.
4. a kind of method of preparing powdered carbon taking cow dung as raw material according to claim 1, is characterized in that, described in step (2), the phosphoric acid of composite activating agent and the mass ratio of potassium primary phosphate are 20:1.
5. a kind of method of preparing powdered carbon taking cow dung as raw material according to claim 1, is characterized in that, the temperature of carrying out burning carbonate described in step (3) under oxygen free condition is 700 DEG C.
6. a kind of method of preparing powdered carbon taking cow dung as raw material according to claim 1, is characterized in that, the burning carbonate time described in step (3) is 1.5 hours.
7. a kind of method of preparing powdered carbon taking cow dung as raw material according to claim 1, is characterized in that, the temperature of the distilled water described in step (4) is room temperature.
CN201410248431.XA 2014-06-06 2014-06-06 Method for preparing powder active carbon by taking cow dung as raw material Pending CN104003386A (en)

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Cited By (6)

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CN104355357A (en) * 2014-11-25 2015-02-18 中南林业科技大学 Filter unit for fecal wastewater treatment of farm
CN104801306A (en) * 2015-03-26 2015-07-29 中国科学院生态环境研究中心 Powdered activated carbon catalyst prepared from turf used as raw material and preparation method
CN107572519A (en) * 2017-08-22 2018-01-12 青海民族大学 A kind of method of intensive milk cow factory clean manufacturing
CN110755991A (en) * 2018-07-27 2020-02-07 中国石油化工股份有限公司 Styrene waste gas treatment method
CN112295386A (en) * 2019-08-02 2021-02-02 中国石油化工股份有限公司 Activating agent for manganese dioxide generated in styrene waste gas treatment and application thereof
CN115140735A (en) * 2022-05-27 2022-10-04 桂林理工大学 Preparation method and application of passion fruit peel-based activated carbon

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104355357A (en) * 2014-11-25 2015-02-18 中南林业科技大学 Filter unit for fecal wastewater treatment of farm
CN104355357B (en) * 2014-11-25 2017-06-13 中南林业科技大学 A kind of filter for plant's excrement and urine water treatment
CN104801306A (en) * 2015-03-26 2015-07-29 中国科学院生态环境研究中心 Powdered activated carbon catalyst prepared from turf used as raw material and preparation method
CN107572519A (en) * 2017-08-22 2018-01-12 青海民族大学 A kind of method of intensive milk cow factory clean manufacturing
CN110755991A (en) * 2018-07-27 2020-02-07 中国石油化工股份有限公司 Styrene waste gas treatment method
CN110755991B (en) * 2018-07-27 2021-12-24 中国石油化工股份有限公司 Styrene waste gas treatment method
CN112295386A (en) * 2019-08-02 2021-02-02 中国石油化工股份有限公司 Activating agent for manganese dioxide generated in styrene waste gas treatment and application thereof
CN115140735A (en) * 2022-05-27 2022-10-04 桂林理工大学 Preparation method and application of passion fruit peel-based activated carbon

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Application publication date: 20140827