CN101966990B - Method for preparing activated carbon from kernel of common macrocarpium fruit - Google Patents
Method for preparing activated carbon from kernel of common macrocarpium fruit Download PDFInfo
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- CN101966990B CN101966990B CN201010543235A CN201010543235A CN101966990B CN 101966990 B CN101966990 B CN 101966990B CN 201010543235 A CN201010543235 A CN 201010543235A CN 201010543235 A CN201010543235 A CN 201010543235A CN 101966990 B CN101966990 B CN 101966990B
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- skunk bush
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Abstract
The invention discloses a method for preparing activated carbon from the kernel of common macrocarpium fruit serving as a raw material, which comprises the following steps of: stirring by using an intermittent tank reactor which is treated by an anti-corrosion material to fully knead the pretreated raw material and an active agent, and carbonizing and activating at a certain temperature to obtain an activated material; and recovering the active agent, rinsing, dehydrating, drying and the like to obtain finished activated carbon. The kernel of the common macrocarpium fruit is forest product waste which is not utilized at present, so that the problem of multi-layer composite utilization of the forest product common macrocarpium fruit is solved, the production cost of the activated carbon is greatly reduced; meanwhile, a new resource capable of producing the activated carbon with high adsorption property is found for the activated carbon industry.
Description
Technical field
The present invention relates to a kind of preparation activated carbon technology field.Specifically, the present invention relates to a kind ofly prepare process of active carbon with the skunk bush fruit stone.
Background technology
Skunk bush (cornus officinalis Sieb.et Zucc.) is Cornaceae Macrocarpium dungarunga or shrub, has another name called Fructus Corni, medicine jujube, fructus corni etc. after the fruit stoning after its maturation.Skunk bush is distributed in the north temperate zone, semi-tropical high mountain area.Main product is in countries such as China, Japan, Korea S, Britain, the U.S..In China, main product in Shaanxi, more than 10 province such as little, Gansu in Henan, Zhejiang, Shanxi, Shandong, Sichuan, peace.Wherein, the Fuping of Hanzhong have the laudatory title in " township of skunk bush ", and YO has broken through 1,000,000 kg at present.The dry fruit stone of skunk bush, its weight is about 1/3 of pulp, and relevant skunk bush pulp has had sophisticated product, but less relatively to the research of its fruit stone utilization, a large amount of fruit stones has just wasted valuable biomass resource as can not get effective utilization.Therefore, to the harder characteristics of skunk bush fruit stone, we have developed new technology, and the cornel fruit consideration convey is changed into gac.
Gac is a kind of porous carbon material with flourishing pore texture and bigger serface that utilizes biological organic substance (like timber, coke, refinery coke, various nutshells etc.) preparation.Utilize different raw materials and different processes to prepare, and then obtained the biomass active charcoal of different performance.The preparation that with timber is traditional gac of raw material receives the restriction of ecological environmental protection, more and more is much accounted of so utilize secondary product of forestry to produce gac for raw material.
Utilize the skunk bush fruit stone to prepare gac, do not appear in the newspapers up to now.
Summary of the invention
The purpose of this invention is to provide a kind of is the feedstock production process of active carbon with depleted skunk bush fruit stone; Not only solve the skunk bush fruit stone and prepared the technological difficulties in the gac process; And make full use of discarded skunk bush fruit stone, enlarged the new way in gac source.
Technical scheme: a kind ofly prepare process of active carbon, may further comprise the steps with the skunk bush fruit stone:
(1) the skunk bush fruit stone after will removing the peel is removed impurity, and 105 ± 5 ℃ of oven dry, through pulverizing, 20 purpose powder are processed in screening;
(2) with step 1 gained skunk bush fruit stone powder impregnation in acvator, utilize through the two-way stirring of the tank reactor at intermittence that corrosion resistant material was handled and quicken to mediate, after kneading is abundant, again its suction filtration is gone out, subsequent use;
(3) with the skunk bush fruit stone powder of gained in the step 2, in the rotary kiln of packing into, at a certain temperature, fill heating charcoal activation under shielding gas (like nitrogen) the oxygen barrier condition;
(4) with activated particles in the step 3, carry out pickling, washing, oven dry, pulverize, sieve, prepare the finished product gac.
Described preparation process of active carbon, the employing of acvator described in the said step (2) mass concentration are 30%～65% liquor zinci chloridi.
Described preparation process of active carbon, the solid-liquid ratio of skunk bush fruit stone powder and said acvator is 1: 1～1: 5 described in the said step (2).
Described preparation process of active carbon, the time of immersion described in the said step (2) is 3～9h.
The charcoal activation temperature of skunk bush fruit stone powder is 400～900 ℃ in the described preparation process of active carbon, said step (3).
Described preparation process of active carbon, the charcoal soak time in the said step (3) is 1～5h.
Described preparation process of active carbon, the rotating speed of said step (2) discontinuous tank reactor is 4r/min, and is every at a distance from 2min, changes round about 1 time.
Described preparation process of active carbon uses not condensable gases as a kind of shielding gas in the said charcoal reactivation process in the said step (3).
In charcoal priming reaction process, total system the unloading phase, utilize nitrogen to feed in the activation tube as protection gas, increase a condensation facility in its tail gas outlet and collect wood vinegar, liquid substances such as tar, condensable gases is not collected in the gas tank.After system moves 20 minutes, start vacuum pump, the not condensable gases in the gas tank is fed rotary kiln as protection gas, stop the nitrogen input simultaneously.
Compared with prior art, the advantage and the effect that have of the present invention is following:
The raw material ratio of the preparation gac that (1) the present invention adopted is newer, is that the research of feedstock production gac does not see that as yet report is arranged with the skunk bush fruit stone at present promptly.In addition, use the skunk bush fruit stone to be able to use, can enlarge the raw material sources of preparation gac from the raw materials for production angle as the gac of raw material manufacturing.
The raw material of the preparation gac that (2) the present invention adopted is easy to get, and cost is low.The skunk bush fruit stone is the waste that obtains at present behind the skunk bush pulp, if with its contaminate environment first of directly burning, second wastes forest resourceies.The skunk bush fruit stone is made gac, not only it is turned waste into wealth, and has improved the utility value of skunk bush sub product greatly, and has reduced the manufacturing cost of gac.
(3) utilization of the present invention is quickened to mediate through the two-way stirring of tank reactor at intermittence that corrosion resistant material was handled, and shortens time of immersion greatly, raises the efficiency.
(4) the present invention utilizes the not condensable gases product that produces in the charcoal reactivation process as protection gas, has reduced the loss of shielding gas (like nitrogen), has practiced thrift cost.
(5) the present invention adopts chemical activation method to prepare the technology of skunk bush gac, and its product absorption property all is higher than relevant criterion.
Embodiment
Below in conjunction with specific embodiment, the present invention is elaborated.
Embodiment 1:
Dry: as the skunk bush fruit stone to be removed impurity, 105 ± 5 ℃ of dry 12h dehydrations.
Pulverize: dried raw material was pulverized 20 mesh sieves.
Dipping: according to the liquor zinci chloridi mixing of 1: 1.5 usefulness 60% of weight ratio solid-liquid ratio, utilize, flooded 3 hours, quicken to mediate through the two-way stirring of tank reactor at intermittence that corrosion resistant material was handled.Again its suction filtration is gone out, subsequent use.
The charcoal priming reaction: impregnated raw material is put into rotary kiln, feed shielding gas, for example nitrogen is 550 ℃ of following charcoal activation 4 hours in temperature, make the raw material pore texture gradually prosperity get up and finally become gac.
Pickling: after the activated material cooling, adopt the hydrochloric acid soln of 1mol/L to boil 30～60min.
Washing: the distilled water flushing activated material with heat makes its pH value approach 7.Can reduce iron and other foreign matter contents in the activated material like this, improve product quality.
Dry: after activated material is placed the baking oven oven dry, pulverized 200 mesh sieves, and can obtain the finished product gac.
Embodiment 2:
Dry: as the skunk bush fruit stone to be removed impurity, 105 ± 5 ℃ of dry 12h dehydrations.
Pulverize: dried raw material was pulverized 20 mesh sieves.
Dipping: according to the liquor zinci chloridi mixing of 1: 3 usefulness 50% of weight ratio solid-liquid ratio, utilize through the two-way stirring of tank reactor at intermittence that corrosion resistant material was handled, flooded 6 hours, rotating speed is 4r/min, and every separated 2min changes 1 time round about, quickens to mediate.Again its suction filtration is gone out, subsequent use.
The charcoal priming reaction: impregnated raw material is put into rotary kiln, feed shielding gas, for example nitrogen is 650 ℃ of following charcoal activation 3 hours in temperature, make the raw material pore texture gradually prosperity get up and finally become gac.
Pickling: after the activated material cooling, adopt the hydrochloric acid soln of 1mol/L to boil 30～60min.
Washing: the distilled water flushing activated material with heat makes its pH value approach 7.Can reduce iron and other foreign matter contents in the activated material like this, improve product quality.
Dry: after activated material is placed the baking oven oven dry, pulverized 200 mesh sieves, and can obtain the finished product gac.
Embodiment 3:
Dry: as the skunk bush fruit stone to be removed impurity, 105 ± 5 ℃ of dry 12h dehydrations.
Pulverize: dried raw material was pulverized 20 mesh sieves.
Dipping: according to the liquor zinci chloridi mixing of 1: 4.5 usefulness 35% of weight ratio solid-liquid ratio, utilize through the two-way stirring of tank reactor at intermittence that corrosion resistant material was handled, flooded 9 hours, rotating speed is 4r/min, and every separated 2min changes 1 time round about, quickens to mediate.Again its suction filtration is gone out, subsequent use.
The charcoal priming reaction: impregnated raw material is put into rotary kiln, feed shielding gas, for example nitrogen is 800 ℃ of following charcoal activation 2 hours in temperature, make the raw material pore texture gradually prosperity get up and finally become gac.
Pickling: after the activated material cooling, adopt the hydrochloric acid soln of 1mol/L to boil 30～60min.
Washing: the distilled water flushing activated material with heat makes its pH value approach 7.Can reduce iron and other foreign matter contents in the activated material like this, improve product quality.
Dry: after activated material is placed the baking oven oven dry, pulverized 200 mesh sieves, and can obtain the finished product gac.
Embodiment 4:
In order to further specify the present invention, take by weighing 500g impurity elimination, cross the skunk bush fruit stone of 20 mesh sieves, flood, after the charcoal activation, pickling, washing, oven dry, pulverizing, obtain the finished product gac of 192g according to step of the present invention and processing condition.
Utilize skunk bush fruit stone production process of active carbon according to the present invention, its performance index are compared with standard index and are listed in the table 1
The synopsis of table 1 detected result of the present invention and standard index
Standard index in the table is the Ministry of Chemical Industry of the People's Republic of China that announces according to HG3-1290-80, and gac ministerial standard, detected result are the test event indexs that the present invention detects.Can see the gac that utilizes the skunk bush fruit stone to make from table 1, the main performance index adsorptive capacity is greater than ministerial standard.
Therefore, provided by the present invention perfect with the technical process of skunk bush fruit stone manufacturing active carbon method, quality product surpasses ministerial standard.
Should be understood that, concerning those of ordinary skills, can improve or conversion, and all these improvement and conversion all should belong to the protection domain of accompanying claims of the present invention according to above-mentioned explanation.
Claims (1)
1. one kind prepares process of active carbon with the skunk bush fruit stone, it is characterized in that, may further comprise the steps:
(1) the skunk bush fruit stone after will removing the peel is removed impurity, and 105 ± 5 ℃ of oven dry, through pulverizing, 20 order skunk bush fruit stone powder are processed in screening;
(2) with step 1 gained skunk bush fruit stone powder impregnation in acvator, utilize through the two-way stirring of the tank reactor at intermittence that corrosion resistant material was handled and quicken to mediate, after kneading is abundant, again its suction filtration is gone out, subsequent use; Said acvator employing mass concentration is 30%～65% liquor zinci chloridi; The solid-liquid ratio of said skunk bush fruit stone powder and said acvator is 1: 1～1: 5; Described time of immersion is 3～9h; Intermittently the rotating speed of tank reactor is 4r/min, and is every at a distance from 2min, changes round about 1 time;
(3) with the skunk bush fruit stone powder of gained in the step 2, in the rotary kiln of packing into, at a certain temperature, fill heating charcoal activation under the shielding gas oxygen barrier condition; In charcoal priming reaction process, total system the unloading phase, utilize nitrogen to feed in the activation tube as protection gas, increase a condensation facility in its tail gas outlet and collect the liquid substance that comprises wood vinegar, tar, condensable gases is not collected in the gas tank; After system moves 20 minutes, start vacuum pump, the not condensable gases in the gas tank is fed rotary kiln as protection gas, stop the nitrogen input simultaneously; The charcoal activation temperature of skunk bush fruit stone powder is 400～900 ℃; The charcoal soak time is 1～5h;
(4) with activated particles in the step 3, carry out pickling, washing, oven dry, pulverize, sieve, prepare the finished product gac.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010543235A CN101966990B (en) | 2010-11-15 | 2010-11-15 | Method for preparing activated carbon from kernel of common macrocarpium fruit |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010543235A CN101966990B (en) | 2010-11-15 | 2010-11-15 | Method for preparing activated carbon from kernel of common macrocarpium fruit |
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| Publication Number | Publication Date |
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| CN101966990A CN101966990A (en) | 2011-02-09 |
| CN101966990B true CN101966990B (en) | 2012-08-29 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491325A (en) * | 2011-11-28 | 2012-06-13 | 江西师范大学 | Method for preparing activated carbon from lotus seed shells |
| CN102502630B (en) * | 2011-11-30 | 2013-08-07 | 河北科技大学 | Method for preparing activated carbon from penicillin or terramycin strain residues |
| CN102633252A (en) * | 2012-04-26 | 2012-08-15 | 合肥工业大学 | Method for producing porous carbon for super capacitor by utilizing lignosulfonate |
| CN102745685A (en) * | 2012-07-18 | 2012-10-24 | 太仓市联林活性炭厂 | Process of using dogwood kernel to prepare activated carbon |
| CN103274399B (en) * | 2013-05-07 | 2015-06-17 | 韩城市金太阳花椒油脂药料有限责任公司 | Method for producing active carbon by pyrolysing pepper branches |
| CN104828821B (en) * | 2013-07-25 | 2017-11-14 | 浙江旺林生物科技有限公司 | A kind of activated carbon and its preparation technology |
| CN103566872A (en) * | 2013-09-26 | 2014-02-12 | 蚌埠华纺滤材有限公司 | Dogwood kernel modified active carbon water purifier and preparation method thereof |
| CN106395818A (en) * | 2016-09-04 | 2017-02-15 | 河南科技学院 | Preparation method of dogwood kernel active carbon |
| CN106608628A (en) * | 2016-12-16 | 2017-05-03 | 陕西中医药大学 | Method for preparing Chinese date pit activated carbon by zinc chloride activation |
| CN107866200A (en) * | 2017-10-27 | 2018-04-03 | 湖南科技学院 | A kind of primary cubeb litsen tree seed granular activated carbon and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497439A (en) * | 2009-03-06 | 2009-08-05 | 中南大学 | Method for preparing active carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101497439A (en) * | 2009-03-06 | 2009-08-05 | 中南大学 | Method for preparing active carbon |
Non-Patent Citations (1)
| Title |
|---|
| Sych, N. V..Processing of Cornus mas kernels to obtain highly porous sorbent materials.《Ekotekhnologii i Resursosberezhenie》.2008,第3卷摘要. * |
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