CN101643207A - Method for preparing active carbon based on mulberry branch - Google Patents

Method for preparing active carbon based on mulberry branch Download PDF

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CN101643207A
CN101643207A CN200910034737A CN200910034737A CN101643207A CN 101643207 A CN101643207 A CN 101643207A CN 200910034737 A CN200910034737 A CN 200910034737A CN 200910034737 A CN200910034737 A CN 200910034737A CN 101643207 A CN101643207 A CN 101643207A
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active carbon
mulberry branch
ramulus mori
carbon based
preparation
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CN101643207B (en
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王俊
吴福安
王蒙
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Jiangsu University of Science and Technology
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Abstract

The invention relates to a method for preparing active carbon by a mulberry branch, which comprises the following concrete steps: removing dust and impurities of the mulberry branch, drying at 100-140DEG C and pulverizing and screening to prepare mulberry branch powder in 60 meshes; soaking the mulberry branch fine powder in an activating agent, wherein the activating agent is an acetic acid solution, a phosphoric acid solution or a potassium hydroxide solution; heating, activating and then filtering for standby; shifting the activated mulberry branch fine powder to a muffle furnace or a pipefurnace and heating and carbonizing under the conditions of filling nitrogen and insulating oxygen; washing carbonized particles by distilled water till the pH value is 6 to 7 and drying at 100 DEG Cfor 12 hours to obtain the active carbon based on the mulberry branch. The invention prepares the mulberry branch active carbon by a chemical method, has simple preparation process, high efficiency and low cost, belongs to the waste utilization of agricultural and sideline products, is beneficial to environmental protection and can obtain the mulberry branch active carbon with large specific surface area and high adsorption capacity.

Description

The preparation method of active carbon based on mulberry branch
Technical field
The invention belongs to the manufacturing technology field of gac, particularly a kind of is the feedstock production process of active carbon with the ramulus mori.
Background technology
Mulberry cultivation is with a long history, and about 1,000 ten thousand mu of China's mulberry field area is wherein concentrated with main producing regions such as Jiangsu, Zhejiang, Sichuan.Ramulus mori is to be only second to mulberry leaf, the higher part of biological yield in the mulberry tree tissue.In actual silkworm and mulberry are produced, owing to need to produce a large amount of high-quality mulberry leaf satisfying the current demand of the agricultural of breeding silkworms, the mulberry field needs regularly cut every year in the production mulberry leaf process of routine to cut down branch, and these ramulus moris are often piled up on the spot, and underuse, cause the significant wastage of this biomass resource.In addition, the main parasitic place that ramulus mori is a mulberry disease insect is cut down in cutting of arbitrarily stacking in the mulberry field, and untimely processing ramulus mori can cause the large-area disease and pest in mulberry field, thereby in time handles the need of work that ramulus mori also is the prevention and control of mulberry tree insect disease.
Gac is a kind of porous carbon material with flourishing pore texture and bigger serface that utilizes biological organic substance (as timber, coke, refinery coke, various nutshells etc.) preparation.Utilize different raw materials to be prepared, and then obtained the biomass active charcoal of different performance with different technology.The preparation that with timber is traditional gac of raw material has been subjected to the restriction of forest development, more and more is much accounted of so utilize multiple alternative biomass to produce gac for raw material.At present, various biomass are produced the research of gac and are constantly being carried out, and some is large-scale production.Utilize the natural structure of plant class raw material (as timber, coconut husk, nut-shell, straw, corn cob, tobacco rod, straw, rice straw etc.), can make the gac that specific surface area is big, micropore is flourishing, physical strength is high, thereby utilize ramulus mori to possess advantageous resources advantage for the feedstock production gac: wide material sources, with low cost, added value is high, the comprehensive utilization.Under this situation, the present invention utilizes ramulus mori to be the feedstock production gac first, not only can control the source of mulberry field insect disease, the more important thing is, make full use of the abundant carbon resource of mulberry field waste, avoided its environmental pollution that causes, widened the raw material sources channel that China's high performance active carbon is produced, to satisfy, have bigger economic worth and social effect both at home and abroad to the ever-increasing market requirement of high performance active carbon.
Active carbon based on mulberry branch does not appear in the newspapers up to now.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of is the feedstock production process of active carbon with the ramulus mori, realizes the higher value application of the discarded ramulus mori in mulberry field.
Technical scheme: a kind ofly prepare process of active carbon with ramulus mori, concrete steps comprise:
(1) ramulus mori is removed dust impurity, 100~140 ℃ of oven dry, by pulverizing, 60 order ramulus mori powder are made in screening;
(2) step 1 gained ramulus mori fine powder is flooded in activator, described activator is acetic acid solution, phosphoric acid solution or potassium hydroxide solution, after the heat-activated, its suction filtration is gone out again, and is standby;
(3) with the ramulus mori fine powder after the activation of gained in the step 2, move in retort furnace or the tube furnace, under inflated with nitrogen oxygen barrier condition, heat carbonization;
(4) particle after the carbonization in the step 3 is washed with distilled water to pH 6~7, dry 12h under 100 ℃ can get active carbon based on mulberry branch.
Described activator acetic acid solution concentration is 20~60wt%.
Described activator phosphoric acid solution concentration is 30~70wt%.
Described activator potassium hydroxide solution concentration is 0.5~3.0mol/L.
The impregnating ratio of pretreated ramulus mori powder and activator is 1: 1~5: 1 (W/V).
The activation temperature scope of pretreated ramulus mori powder is 60~95 ℃.
The soak time scope of pretreated ramulus mori powder is 6~20h.
The carbonization temperature scope of the ramulus mori powder after the activation is 300~1200 ℃.
The carbonization time scope of the ramulus mori powder after the activation is 1~10h.
Beneficial effect: the present invention adopts chemical method to prepare the ramulus mori gac, and preparation process is simple, the efficient height, and cost is low, and belongs to the agricultural byproducts utilization of waste material, is beneficial to environment protection, can obtain the ramulus mori gac that specific surface area is big, loading capacity is high.
Description of drawings
Preparation technology's schema of Fig. 1 active carbon based on mulberry branch
The scanning electron microscope picture a of Fig. 2 active carbon based on mulberry branch
The scanning electron microscope picture b of Fig. 3 active carbon based on mulberry branch
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Among the embodiment of the present invention, chemical method prepares the notion that gac generally adopts yield, i.e. the ratio of product quality and raw materials quality, and its calculating formula is:
Figure G2009100347374D00031
Wherein, m Product, m Raw materialBe respectively the quality of product and raw material.
Measure iodine sorption value: with reference to GB (National Quality ﹠ Technology Inspection Bureau. the mensuration of wood activated charcoal iodine sorption value [S], 1999.)
Embodiment 1
Ramulus mori is cleaned, removed behind the dust, be crushed to 60 orders 100 ℃ of oven dry down.Be soaked in the acetic acid solution of 20wt%, 60 ℃ flood 20h down, and impregnating ratio is 5: 1 (W/V).Behind the suction filtration, be placed in the retort furnace, 300 ℃ of temperature and fill carbonization 1h under the nitrogen oxygen barrier condition, take out behind the powered-down, be washed with distilled water to the pH value and be 6-7, dry 12h under 100 ℃, oven dry, promptly get the ramulus mori activated carbon, yield is 31.23%, and the mensuration iodine sorption value is 756.42mg/g.
Embodiment 2
Ramulus mori is cleaned, removed behind the dust, be crushed to 60 orders 140 ℃ of oven dry down.Be soaked in the acetic acid solution of 50wt%, 95 ℃ flood 6h down, and impregnating ratio is 1: 1 (W/V).Behind the suction filtration, be placed in the tube furnace, 1200 ℃ of temperature and fill carbonization 10h under the nitrogen oxygen barrier condition, take out behind the powered-down, be washed with distilled water to the pH value and be 6-7, dry 12h under 100 ℃, oven dry, promptly get the ramulus mori activated carbon, yield is 34.23%, and the mensuration iodine sorption value is 781.25mg/g.
Embodiment 3
Ramulus mori is cleaned, removed behind the dust, be crushed to 60 orders 140 ℃ of oven dry down.Be soaked in the phosphoric acid solution of 40wt%, 95 ℃ flood 20h down, and impregnating ratio is 1: 1 (W/V).Behind the suction filtration, be placed in the retort furnace, 1200 ℃ of temperature and fill carbonization 10h under the nitrogen oxygen barrier condition, take out behind the powered-down, be washed with distilled water to the pH value and be 6-7, dry 12h under 100 ℃, oven dry, promptly get the ramulus mori activated carbon, yield is 36.16%, and the mensuration iodine sorption value is 856.37mg/g.
Embodiment 4
Ramulus mori is cleaned, removed behind the dust, be crushed to 60 orders 100 ℃ of oven dry down.Be soaked in the phosphoric acid solution of 30wt%, 60 ℃ flood 6h down, and impregnating ratio is 5: 1 (W/V).Behind the suction filtration, be placed in the tube furnace temperature programming 300 ℃ of temperature and fill carbonization 1h under the nitrogen oxygen barrier condition, take out behind the powered-down, be washed with distilled water to the pH value and be 6-7, dry 12h under 100 ℃, oven dry promptly gets the ramulus mori activated carbon, yield is 32.57%, and the mensuration iodine sorption value is 759.18mg/g.
Embodiment 5
Ramulus mori is cleaned, removed behind the dust, be crushed to 60 orders 100 ℃ of oven dry down.Be soaked in the potassium hydroxide solution of 40wt%, 60 ℃ flood 20h down, and impregnating ratio is 5: 1 (W/V).Behind the suction filtration, be placed in the retort furnace temperature programming 300 ℃ of temperature and fill carbonization 1h under the nitrogen oxygen barrier condition, take out behind the powered-down, be washed with distilled water to the pH value and be 6-7, dry 12h under 100 ℃, oven dry promptly gets the ramulus mori activated carbon, yield is 30.47%, and the mensuration iodine sorption value is 746.22mg/g.
Embodiment 6
Ramulus mori is cleaned, removed behind the dust, be crushed to 60 orders 140 ℃ of oven dry down.Be soaked in the potassium hydroxide solution of 60wt%, 95 ℃ flood 6h down, and impregnating ratio is 1: 1 (W/V).Behind the suction filtration, be placed in the tube furnace, 1200 ℃ of temperature and fill carbonization 10h under the nitrogen oxygen barrier condition, take out behind the powered-down, be washed with distilled water to the pH value and be 6-7, dry 12h under 100 ℃, oven dry, promptly get the ramulus mori activated carbon, yield is 33.14%, and the mensuration iodine sorption value is 814.36mg/g.
Embodiment 7
Ramulus mori is cleaned, removed behind the dust, be crushed to 60 orders 120 ℃ of oven dry down.Be soaked in the phosphoric acid solution of 48wt%, 85 ℃ flood 14h down, and impregnating ratio is 2.1: 1 (W/V).Behind the suction filtration, be placed in the tube furnace, 500 ℃ of temperature and fill carbonization 2h under the nitrogen oxygen barrier condition, take out behind the powered-down, be washed with distilled water to the pH value and be 6-7, dry 12h under 100 ℃, oven dry, promptly get the ramulus mori activated carbon, yield is 38.93%, and the mensuration iodine sorption value is 889.93mg/g.

Claims (9)

1, a kind ofly prepare process of active carbon, it is characterized in that concrete steps comprise with ramulus mori:
(1) ramulus mori is removed dust impurity, 100~140 ℃ of oven dry, by pulverizing, 60 ramulus mori powder are made in screening;
(2) step 1 gained ramulus mori fine powder is flooded in activator, described activator is acetic acid solution, phosphoric acid solution or potassium hydroxide solution, after the heat-activated, its suction filtration is gone out again, and is standby;
(3) with the ramulus mori fine powder after the activation of gained in the step 2, move in retort furnace or the tube furnace, under inflated with nitrogen oxygen barrier condition, heat carbonization;
(4) particle after the carbonization in the step 3 is washed with distilled water to pH 6~7, dry 12h under 100 ℃ can get active carbon based on mulberry branch.
2, the preparation method of a kind of active carbon based on mulberry branch according to claim 1 is characterized in that activator acetic acid solution concentration is 20~60wt%.
3, the preparation method of a kind of active carbon based on mulberry branch according to claim 1 is characterized in that activator phosphoric acid solution concentration is 30~70wt%.
4, the preparation method of a kind of active carbon based on mulberry branch according to claim 1 is characterized in that activator potassium hydroxide solution concentration is 0.5~3.0mol/L.
5, the preparation method of a kind of active carbon based on mulberry branch according to claim 1, the impregnating ratio that it is characterized in that pretreated ramulus mori powder and activator are 1: 1~5: 1 (W/V).
6, the preparation method of a kind of active carbon based on mulberry branch according to claim 1, the activation temperature scope that it is characterized in that pretreated ramulus mori powder is 60~95 ℃.
7, the preparation method of a kind of active carbon based on mulberry branch according to claim 1, the soak time scope that it is characterized in that pretreated ramulus mori powder is 6~20h.
8, the preparation method of a kind of active carbon based on mulberry branch according to claim 1, the carbonization temperature scope of the ramulus mori powder after it is characterized in that activating is 300~1200 ℃.
9, the preparation method of a kind of active carbon based on mulberry branch according to claim 1, the carbonization time scope of the ramulus mori powder after it is characterized in that activating is 1~10h.
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102653402A (en) * 2012-05-29 2012-09-05 马宗华 Method for preparing active carbon
CN103579640A (en) * 2012-07-25 2014-02-12 中国科学院大连化学物理研究所 Anode material for lithium-air battery and preparation method thereof
CN104176736A (en) * 2014-08-18 2014-12-03 福建师范大学泉港石化研究院 Method for preparing activated carbon from ionic liquid pretreated raw material
CN104326471A (en) * 2014-10-20 2015-02-04 宁夏医科大学 Method for preparing active carbon from licorice waste residue
CN106241797A (en) * 2016-07-29 2016-12-21 句容市百诚活性炭有限公司 A kind of preparation method of phragmites communis matrix activated carbon
CN108217645A (en) * 2018-02-13 2018-06-29 平南县亿翔环保能源有限公司 A kind of method that activated carbon is prepared using eucalyptus
CN108275680A (en) * 2018-02-13 2018-07-13 平南县亿翔环保能源有限公司 A method of preparing activated carbon using ramulus mori
CN108821284A (en) * 2018-09-08 2018-11-16 佛山市森昂生物科技有限公司 A kind of preparation method of sand sagebrush (Artemisia filifolia) charcoal
CN108962625A (en) * 2018-06-22 2018-12-07 东莞理工学院 A kind of supercapacitor carbon material and preparation method thereof prepared using humin as raw material
CN110817869A (en) * 2019-12-04 2020-02-21 山东建筑大学 Zinc phosphate-organic acid composite activator and method for preparing activated carbon by using same
CN115532034A (en) * 2022-10-22 2022-12-30 潍坊金信达生物化工有限公司 Method and device for treating biodiesel mixed tail gas
CN116282340A (en) * 2023-05-15 2023-06-23 广东省农业科学院动物科学研究所 Method for treating aquaculture water by adding mulberry twig biochar

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* Cited by examiner, † Cited by third party
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CN101249960B (en) * 2008-03-11 2010-12-01 山东大学 Preparation technique of read catkins or silvergrass activated carbon

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102653402A (en) * 2012-05-29 2012-09-05 马宗华 Method for preparing active carbon
CN103579640A (en) * 2012-07-25 2014-02-12 中国科学院大连化学物理研究所 Anode material for lithium-air battery and preparation method thereof
CN104176736A (en) * 2014-08-18 2014-12-03 福建师范大学泉港石化研究院 Method for preparing activated carbon from ionic liquid pretreated raw material
CN104326471A (en) * 2014-10-20 2015-02-04 宁夏医科大学 Method for preparing active carbon from licorice waste residue
CN106241797A (en) * 2016-07-29 2016-12-21 句容市百诚活性炭有限公司 A kind of preparation method of phragmites communis matrix activated carbon
CN108275680A (en) * 2018-02-13 2018-07-13 平南县亿翔环保能源有限公司 A method of preparing activated carbon using ramulus mori
CN108217645A (en) * 2018-02-13 2018-06-29 平南县亿翔环保能源有限公司 A kind of method that activated carbon is prepared using eucalyptus
CN108962625A (en) * 2018-06-22 2018-12-07 东莞理工学院 A kind of supercapacitor carbon material and preparation method thereof prepared using humin as raw material
CN108821284A (en) * 2018-09-08 2018-11-16 佛山市森昂生物科技有限公司 A kind of preparation method of sand sagebrush (Artemisia filifolia) charcoal
CN110817869A (en) * 2019-12-04 2020-02-21 山东建筑大学 Zinc phosphate-organic acid composite activator and method for preparing activated carbon by using same
CN115532034A (en) * 2022-10-22 2022-12-30 潍坊金信达生物化工有限公司 Method and device for treating biodiesel mixed tail gas
CN116282340A (en) * 2023-05-15 2023-06-23 广东省农业科学院动物科学研究所 Method for treating aquaculture water by adding mulberry twig biochar
CN116282340B (en) * 2023-05-15 2023-07-21 广东省农业科学院动物科学研究所 Method for treating aquaculture water by adding mulberry twig biochar

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