CN104386693B - A kind of method that activated carbon prepared by Chinese crude drug waste residue - Google Patents
A kind of method that activated carbon prepared by Chinese crude drug waste residue Download PDFInfo
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- CN104386693B CN104386693B CN201410648295.3A CN201410648295A CN104386693B CN 104386693 B CN104386693 B CN 104386693B CN 201410648295 A CN201410648295 A CN 201410648295A CN 104386693 B CN104386693 B CN 104386693B
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Abstract
The invention discloses a kind of method that activated carbon prepared by Chinese crude drug waste residue, it is characterised in that comprise the following steps: Feedstock treating, once physically activated, chemical impregnation, secondary chemical activation；The present invention is by selecting the Chinese crude drug waste residue that self moisture is different to prepare activated carbon, it may be achieved the micropore regulation and control of Chinese crude drug waste residue activated carbon, makes the activated carbon of preparation have good micropore and central hole structure；Chinese crude drug waste residue need not be dried early stage process, and it is physically activated to utilize self contained humidity to carry out, and has saved and has passed into this operation of steam, has simplified technological process, reduced energy consumption.
Description
Technical field
The present invention relates to the method that Chinese crude drug waste residue resource utilizes, in particular to a kind of method utilizing Chinese crude drug waste residue to prepare activated carbon.
Background technology
China is production of crude drugs state maximum in the world.Cultivated drug face product million hectares, the annual sale tens million of ton of medical material；The prepared slices of Chinese crude drugs and the nearly family more than 3000 of Health Products Enterprises；2000 Duo Jia pharmaceutical factories (include part Western medicine factory) produce thousands of kinds of Chinese patent medicines.All tuberses, leaf, flos materia medica, in Processing methods process, all can produce Chinese crude drug waste residue.At present, the process of Chinese crude drug waste residue based on landfill and is abandoned by domestic most of Chinese crude drug factories as solid waste.The easy polluted-water of above-mentioned processing mode and air；This exopathogenic factor Chinese crude drug waste residue amount is big, landfill disposal can cause large stretch of plough loss and energy waste.For this, Chengdu Inst. of Biology, Chinese Academy of Sciences has carried out " the resource technology research of Chinese herbal medicine dregs ", with Chinese herbal medicine dregs for raw material, and selection-breeding microbial function bacterial strain, produce Organic biological compound fertilizer.
But, Chinese crude drug slag is a kind of desirably regenerative resource, has recyclability and CO2The features such as zero-emission.If Chinese crude drug slag being converted into high-grade energy, it is possible to reduce Fossil fuel consumption, Chinese society sustainable development, utilization of energy and environmental conservation and ecological balance etc. are had important practical significance.
For achieving the above object, Chinese invention patent ZL200910272464.7 proposes a kind of method utilizing Chinese crude drug waste residue to produce combustible gas.This invention is primarily characterized in that employing thermochemical method, Chinese crude drug waste residue pyrolytic gasification is made fuel gas in gasification furnace directly as industry fuel gas heat supply or can as fuel gas after further purification.This Land use systems had both reduced energy waste, solved again the problem of environmental pollution produced because Chinese crude drug waste residue abandons.But in actual application, having that Chinese crude drug waste residue kind is different from source causes that its gasifying furnace device is less strong to raw material versatility adaptive capacity, its product also there is also the shortcomings such as added value is less high.
Therefore, exploitation number of ways recycles Chinese crude drug waste residue, it is thus achieved that the product that added value more highlights becomes inevitable.Chinese crude drug waste residue carbon content is high, content of organics is low, source is wide, cost is low, quantity is big.Chinese crude drug waste residue is made function admirable, activated carbon that added value is higher is to utilize solid waste resource recovery preferably to annotate.Not only economize on resources, and more can promote other environmental protection industry development, be the right way complying with social sustainable development.
Published, adopt Chinese crude drug waste residue to prepare the patent of activated carbon nothing more than as raw material: will carrying out after dehydrate crushes and screens process under Chinese crude drug waste residue low temperature, dipping chemical activating agent carries out activated carbon to be prepared；By again carbonized material is passed into after the Chinese crude drug waste residue pyrolysis charring under an inert atmosphere of dehydrate under low temperature steam carry out physically activated or dipping chemical activating agent carry out chemical activation and then prepare activated carbon.
Chinese invention patent " Chinese medicine slag prepares the method for activated carbon " (application publication number: CN102092711A) discloses, with Chinese invention patent " utilizing the method that Chinese medicine slag produces activated carbon " (application publication number: CN200910059178), the method that activated carbon prepared by Chinese crude drug waste residue.Its common trait is first to be dried by activated carbon, then impregnates different chemical activating agents and carries out activated carbon and prepare.Method disclosed in " Chinese medicine slag prepares the method for activated carbon " is: carry out chemical impregnation by after Chinese medicine slag drying and crushing, places into carbonization-activation in microwave oven, and passing into steam in carbonization-activation process will increase the specific surface area of activated carbon.But steam activation needs to increase process equipment, and consuming time longer, is unfavorable for industrialized production.
Chinese invention patent " a kind of with Chinese medicine slag be raw material heavy metal adsorption activated carbon and method for making and application " (application publication number: CN103949214A), disclose a kind of method and application preparing heavy metal adsorption activated carbon with Chinese medicine slag for raw material.After it is characterized in that just Chinese medicine slag is classified by rhizome mass of residue percentage composition, respectively through high temperature carbonization and steam activation, it is modified preparing activated carbon with methacrylic acid then through after oxidation reaction.This invention, when preparing Chinese crude drug waste residue activated carbon, must will prepare raw material as activated carbon after mixing by a certain percentage after its categorized process of Chinese crude drug waste residue again.But, Chinese medicine preparation factory of China also exists, when medical material extracts active ingredients, the problem that medical material kind mixes always.Therefore, in actual mechanical process, it has been difficult to the classification of Chinese crude drug waste residue.Secondly, carbonization process and the devolatilization process of the Chinese crude drug waste residue that this invention describes are to carry out under an inert atmosphere, this process easily makes the tar blocking carbonized material hole generated in devolatilization process, so that dipping effect is not good during carbonized material dipping chemical activating agent.According to interpretation: carbonized material during under an inert atmosphere or without chemical activating agent, activated carbon raw material carbonization obtained, its specific surface area is usually the scope of several square metres.It is obvious that the carbonized material of this order of magnitude is certain to cause that the dipping effect of the chemical activating agent in later stage is bad, thus finally affecting the Properties of Activated Carbon of preparation.
Patent of invention " a kind of with Chinese medicine slag be raw material antibiotic absorption activated carbon and method for making and application " (application publication number: CN103949214A), Chinese invention patent " a kind of with Chinese medicine slag be raw material heavy metal adsorption activated carbon and method for making and application " (application publication number: CN103949214A), Chinese invention patent " a kind of method utilizing nutgall dreg to prepare mesopore activated carbon " (application publication number: CN102757046A) is all reprocess after raw material Chinese medicine slag is dried, carbonization process utilize steam can accelerate the decomposition of tar, the characteristic reducing the amorphous carbon blocking carbonized material hole that tar deposition generates passes into steam activation, but the method time is long, energy consumption is big, add production cost, it is unfavorable for saving energy and reduce the cost.
Summary of the invention
Present invention aim to solve the deficiency of above-mentioned background technology, it is provided that a kind of method that activated carbon prepared by Chinese crude drug waste residue
The technical scheme is that a kind of method that activated carbon prepared by Chinese crude drug waste residue, it is characterised in that comprise the following steps:
A. Feedstock treating
Chinese crude drug waste residue carries out pulverizing, being sieved into granule, and in wherein said Chinese crude drug waste residue, the mass fraction of contained humidity is 40%-80%；
B. once physically activated
The Chinese crude drug waste particle that contained humidity mass fraction is 40%-80% is placed in vacuum heating apparatus, with 20-100 DEG C/min ramp to after 500-900 DEG C, insulation 20-90min forms material at the beginning of activated carbon, in activation process, Chinese crude drug waste particle is continuously stirred；
C. chemical impregnation
Being immersed in chemical activating agent after the dipping of 4-10h and dry to obtain impregnant by material at the beginning of activated carbon, in dipping process, activated carbon is 1:1.7-4.5 with the mass ratio of chemical activating agent；
D. two chemical activations
Being placed in activation furnace by impregnant, under inert atmosphere, after being warming up to 500 DEG C-1000 DEG C with heating rate 5-30 DEG C/min, insulation 15-30min obtains activated carbon first product, after using deionized water cyclic washing, and drying activated carbon.
Preferably, in described step a, the mass fraction of Chinese crude drug waste residue contained humidity is 50%-70%.
Preferably, Chinese crude drug waste particle is incubated 30-70min by described step b under 600-800 DEG C of vacuum condition and forms material at the beginning of activated carbon.
Preferably, in described step b, mixing speed is 3-6r/min.
Preferably, in described step c, chemical activating agent is the one in hydrochloric acid, potassium hydroxide solution or solution of potassium carbonate.
Further, described chemical activating agent is mass fraction is the solution of potassium carbonate of 30-70%.
Further, in described step c, the mass ratio of activated carbon and chemical activating agent is 1:1.7-3.0.
Preferably, in described step c, activated carbon dip time is 6-8h.
Preferably, after being warming up to 700 DEG C-900 DEG C with heating rate 10-20 DEG C/min in described step d, insulation 20-30min obtains activated carbon first product.
Preferably, in described step d, inert atmosphere uses gas to be nitrogen, argon or helium.
The invention have the advantages that
(1) present invention utilizes the contained high-moisture of Chinese crude drug waste residue self, at high temperature carries out pyrolysis under the steam atmosphere of Chinese crude drug waste residue (being called physically activated), so that material has the specific surface area of up to hundreds of square meters at the beginning of the activated carbon of preparation.At the beginning of the activated carbon that this processing method obtains, material can impregnate chemical activating agent better, reduces dip time, the final manufacturing cycle shortening activated carbon.The effect of steam shows the elimination contributing to part volatile matter, by the steam reforming reaction of tar, accelerates the decomposition that carbonization process is coal-tar middle oil, decreases the chance of the amorphous carbon blocking carbonized material hole that tar deposition generates.The heating rate of 20-100 DEG C/min had both inhibited the generation of tar, has promoted the quick release of steam activated carbon yield to be made again higher.
(2) the Chinese crude drug waste residue particle diameter that the present invention selects is in 15mm, and compared to other patent, Chinese crude drug waste particle particle size range is relatively big, reduces the requirement to grain diameter refinement.This is due in airtight heating furnace, and the high Chinese crude drug waste residue of moisture content is in pyrolysis charring process, and its contained moisture increasing temperature and pressure gradually, so that Chinese crude drug waste particle expands.Form the fluff structure of similar " puffed rice " in door opened moment, expect at the beginning of short grained activated carbon thus bigger Chinese crude drug waste particle can be made to break down into.
(3) present invention is by selecting the Chinese crude drug waste residue that self moisture is different to prepare activated carbon, it may be achieved the micropore regulation and control of Chinese crude drug waste residue activated carbon, makes the activated carbon of preparation have good micropore and central hole structure.
(4) Chinese crude drug waste residue early stage need not be dried process by the present invention, and it is physically activated to utilize self contained humidity to carry out, and has saved and has passed into this operation of steam, has simplified technological process, reduced energy consumption.
Accompanying drawing explanation
Fig. 1 is activated carbon and the once nitrogen adsorption desorption isothermal curve of material at the beginning of physically activated rear activated carbon of embodiment 1,2,3 preparation
Fig. 2 is the activated carbon sample SEM figure of example 1 preparation
Fig. 3 is the activated carbon sample SEM figure of example 2 preparation
Detailed description of the invention
The present invention is described in further detail for embodiment in detail below.
Embodiment 1
It is 75wt% (mass fraction) by moisture content, particle diameter Chinese crude drug waste residue in 15mm heat in airtight heating furnace carry out once physically activated, carry out being warming up to 750 DEG C with 50 DEG C/min, physically activated time 40min, once physically activated process is continuously stirred with 3r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the solution of potassium carbonate Immesion active carbon that mass fraction is 50%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:2.0, dip time 8h.Being placed in activation furnace by impregnant, under nitrogen atmosphere, with 30 DEG C/min heating rate to activation temperature 800 DEG C, soak time 15min carries out secondary chemical activation and prepares activated carbon semi-finished product, obtains activated carbon product after washing and drying repeatedly.Activated carbon yield is 38.19%, and the pattern in the activated carbon sample hole of preparation is as shown in Figure 2.
Embodiment 2
It is 65wt% by moisture content, particle diameter Chinese crude drug waste residue in 15mm heats in airtight heating furnace and carries out once physically activated, carries out being warming up to 750 DEG C with 50 DEG C/min, physically activated time 40min, once physically activated process is continuously stirred with 4r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the solution of potassium carbonate Immesion active carbon that mass fraction is 60%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:1.7, dip time 7h.Impregnant is placed in activation furnace, under helium atmosphere, with 20 DEG C/min heating rate to activation temperature 800 DEG C, when soak time 20min, prepares activated carbon.Activated carbon yield is 36.51%, and the pattern in the activated carbon sample hole of preparation is as shown in Figure 3.
Embodiment 3
It is 80wt% by moisture content, particle diameter Chinese crude drug waste residue in 15mm heats in airtight heating furnace and carries out once physically activated, carries out being warming up to 850 DEG C with 80 DEG C/min, physically activated time 60min, once physically activated process is continuously stirred with 5r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the solution of potassium carbonate Immesion active carbon that mass fraction is 40%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:2.5, dip time 7h.Being placed in activation furnace by impregnant, under argon gas atmosphere, with 10 DEG C/min heating rate to activation temperature 750 DEG C, prepare activated carbon when soak time 30min, activated carbon yield is 33.12%.The nitrogen adsorption desorption isothermal curve of the activated carbon of example 1,2,3 preparation and once material at the beginning of physically activated rear activated carbon is as it is shown in figure 1, the activated carbon of example 1,2,3 preparation and the active carbon pore structure parameter of once material at the beginning of physically activated rear activated carbon are as shown in table 1.
Embodiment 4
It is 70wt% by moisture content, particle diameter Chinese crude drug waste residue in 15mm heats in airtight heating furnace and carries out once physically activated, carries out being warming up to 900 DEG C with 100 DEG C/min, physically activated time 70min, once physically activated process is continuously stirred with 6r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the solution of potassium carbonate Immesion active carbon that mass fraction is 70%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:3.0, dip time 10h.Being placed in activation furnace by impregnant, under nitrogen atmosphere, with 5 DEG C/min heating rate to activation temperature 950 DEG C, prepare activated carbon when soak time 25min, activated carbon yield is 32.43%.
Embodiment 5
It is 50wt% by moisture content, particle diameter Chinese crude drug waste residue in 15mm heats in airtight heating furnace and carries out once physically activated, carries out being warming up to 900 DEG C with 90 DEG C/min, physically activated time 35min, once physically activated process is continuously stirred with 5r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the hydrochloric acid solution Immesion active carbon that mass fraction is 30%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:2.5, dip time 6h.Being placed in activation furnace by impregnant, under nitrogen atmosphere, with 25 DEG C/min heating rate to activation temperature 650 DEG C, prepare activated carbon when soak time 25min, activated carbon yield is 30.83%.
Embodiment 6
It is 65wt% by moisture content, particle diameter Chinese crude drug waste residue in 15mm heats in airtight heating furnace and carries out once physically activated, carries out being warming up to 800 DEG C with 60 DEG C/min, physically activated time 30min, once physically activated process is continuously stirred with 5r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the sodium hydroxide solution Immesion active carbon that mass fraction is 30%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:3.5, dip time 10h.Impregnant is placed in activation furnace, under nitrogen atmosphere, with 30 DEG C/min heating rate to activation temperature 800 DEG C, when soak time 30min, prepares activated carbon.Activated carbon yield is 36.87%.
Embodiment 7
It is 45wt% by moisture content, particle diameter Chinese crude drug waste residue in 15mm heats in airtight heating furnace and carries out once physically activated, carries out being warming up to 900 DEG C with 80 DEG C/min, physically activated time 20min, once physically activated process is continuously stirred with 5r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the solution of potassium carbonate Immesion active carbon that mass fraction is 70%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:1.7, dip time 8h.Being placed in activation furnace by impregnant, under nitrogen atmosphere, with 30 DEG C/min heating rate to activation temperature 500 DEG C, prepare activated carbon when soak time 20min, activated carbon yield is 31.73%.
Embodiment 8
It is 80wt% by moisture content, particle diameter Chinese crude drug waste residue in 15mm heats in airtight heating furnace and carries out once physically activated, carries out being warming up to 500 DEG C with 50 DEG C/min, physically activated time 90min, once physically activated process is continuously stirred with 5r/min mixing speed, prepares material at the beginning of activated carbon.To expect at the beginning of the solution of potassium carbonate Immesion active carbon that mass fraction is 40%, impregnating ratio (mass ratio of activated carbon and chemical activating agent) is 1:4.5, dip time 4h.Being placed in activation furnace by impregnant, under nitrogen atmosphere, with 25 DEG C/min heating rate to activation temperature 1000 DEG C, prepare activated carbon when soak time 30min, activated carbon yield is 32.16%.
The active carbon pore structure parameter of table 1 preparation
Claims (10)
1. the method that activated carbon prepared by a Chinese crude drug waste residue, it is characterised in that comprise the following steps:
A. Feedstock treating
Chinese crude drug waste residue carries out pulverizing, being sieved into granule, and in wherein said Chinese crude drug waste residue, the mass fraction of contained humidity is 40%-80%；
B. once physically activated
The Chinese crude drug waste particle that contained humidity mass fraction is 40%-80% is placed in vacuum heating apparatus, with 20-100 DEG C/min ramp to after 500-900 DEG C, insulation 20-90min forms material at the beginning of activated carbon, in activation process, Chinese crude drug waste particle is continuously stirred；
C. chemical impregnation
Being immersed in chemical activating agent after the dipping of 4-10h and dry to obtain impregnant by material at the beginning of activated carbon, in dipping process, activated carbon is 1:1.7-4.5 with the mass ratio of chemical activating agent；
D. two chemical activations
Being placed in activation furnace by impregnant, under inert atmosphere, after being warming up to 500 DEG C-1000 DEG C with heating rate 5-30 DEG C/min, insulation 15-30min obtains activated carbon first product, after using deionized water cyclic washing, and drying activated carbon.
2. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 1, it is characterised in that in described step a, the mass fraction of Chinese crude drug waste residue contained humidity is 50%-70%.
3. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 1, it is characterised in that in described step b, Chinese crude drug waste particle is warming up under 600-800 DEG C of vacuum condition and is incubated 30-70min forms material at the beginning of activated carbon.
4. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 1, it is characterised in that in described step b, mixing speed is 3-6r/min.
5. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 1, it is characterised in that in described step c, chemical activating agent is the one in hydrochloric acid, potassium hydroxide solution or solution of potassium carbonate.
6. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 5, it is characterised in that described chemical activating agent is mass fraction is the solution of potassium carbonate of 30-70%.
7. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as described in claim 1 or 6, it is characterised in that in described step c, activated carbon is 1:1.7-3.0 with the mass ratio of chemical activating agent.
8. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 1, it is characterised in that in described step c, activated carbon dip time is 6-8h.
9. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 1, it is characterised in that after being warming up to 700 DEG C-900 DEG C with heating rate 10-20 DEG C/min in described step d, insulation 20-30min obtains activated carbon first product.
10. the method that activated carbon prepared by a kind of Chinese crude drug waste residue as claimed in claim 1, it is characterised in that in described step d, inert atmosphere uses gas to be the one in nitrogen, argon or helium.
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| CN105110328A (en) * | 2015-08-18 | 2015-12-02 | 丘璇 | Activated carbon physicochemical modification method |
| CN105197924A (en) * | 2015-08-18 | 2015-12-30 | 丘璇 | Method for processing active carbon |
| CN107285314A (en) * | 2017-08-14 | 2017-10-24 | 河南圣玛斯科技有限公司 | A kind of activated carbon and preparation method thereof |
| CN109529847A (en) * | 2018-11-21 | 2019-03-29 | 江汉大学 | A kind of method and application preparing carbon base catalyst using waste residue of Chinese herbs |
| CN110467181A (en) * | 2019-08-15 | 2019-11-19 | 石河子大学 | A kind of classifying porous charcoal of liquorice dregs base and its preparation method and application |
| CN110436438A (en) * | 2019-09-10 | 2019-11-12 | 西京学院 | A kind of CO2Modified Chinese medicine slag charcoal and its preparation method and application |
| CN115520973A (en) * | 2021-06-25 | 2022-12-27 | 神美科技有限公司 | Preparation method of biological activated carbon loaded with microbial inoculum |
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| CN101544370A (en) * | 2009-05-04 | 2009-09-30 | 成都信息工程学院 | Method for producing active carbon by using traditional Chinese medicine dregs |
| CN102092711A (en) * | 2011-01-13 | 2011-06-15 | 山东大学 | Method for preparing activated carbon from Chinese medicinal dregs |
| CN102757046A (en) * | 2012-06-27 | 2012-10-31 | 昆明理工大学 | Method for preparing mesoporous activated carbon from nutgall dregs |
| CN103303917B (en) * | 2013-07-25 | 2015-05-06 | 程俊校 | Activated carbon and preparation process thereof |
| CN103496698B (en) * | 2013-10-14 | 2016-03-23 | 中国林业科学研究院林产化学工业研究所 | The method of active carbon with high specific surface area is prepared in spontaneous pressure activation |
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