CN100384723C - Method for utilizing purple stem boneset - Google Patents
Method for utilizing purple stem boneset Download PDFInfo
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- CN100384723C CN100384723C CNB2005100110017A CN200510011001A CN100384723C CN 100384723 C CN100384723 C CN 100384723C CN B2005100110017 A CNB2005100110017 A CN B2005100110017A CN 200510011001 A CN200510011001 A CN 200510011001A CN 100384723 C CN100384723 C CN 100384723C
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- eupatorium adenophorum
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- microwave radiation
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Abstract
The present invention relates to a method for utilizing eupatorium adenophorum. After eupatorium adenophorum is crushed to less than or equal to 3mm, water and the crushed eupatorium adenophorum material are mixed according to the weight proportion of 3 to 6: 1, and potassium carbonate or zinc chloride solids and the crushed eupatorium adenophorum material are mixed according to the weight proportion of 0.5 to 4: 1 to carry out ultrasonic wave processing and then carry out heating by microwave radiation, acid wash, water wash and drying to obtain product active carbon. The ultrasonic wave processing is carried out to the mixture material by using the cavatition and the advantage of super mixing agitation of ultrasonic waves; heating activation is carried out by using the microwave radiation to generate large numbers of active carbon points in carbon, effectively promote the formation of pores and increase the adsorbability and the yield of the active carbon. Four sections of preheating, drying, carbonization and activation are integrated to form a process to reduce energy consumption and increase activation efficiency; the adsorbability of the obtained active carbon exceeds the Chinese first level standard of wood activated carbon, eupatorium adenophorum is effectively used for changing harm into benefit, and the present invention finds out a practicable and effective processing method for utilizing eupatorium adenophorum.
Description
One, technical field:
The chemical industry method prepares the gac field.
Two, background technology:
Hemp Eupatorium is a kind of composite family Eupatorium per nnial herb, is a kind of global pernicious poisonous weeds, is commonly called as Herba Eupatorii Odorati, devil's grass.Originate in Mexico, in last century the forties enter south China through Australia, now be distributed widely in provinces such as Yunnan, Hainan, Guangxi, Guizhou, Tibet, Sichuan.Hemp Eupatorium has that the ecological adaptation scope is wide, fast growth, reproductivity is strong, gregariousness is high, aggressiveness and characteristics such as strong stress resistance, mass consumption soil fertility, can breed in a large number at short notice, form the excellent plant community of list of intensive Cheng Cong, cause many plant-growths slow, some species even endangered, and grain, high quality forage etc. drop in production over a large area, and have caused special " the green pollution " to reach " eco-catastrophe ".Simultaneously, Hemp Eupatorium contains toxic substances such as terpene, tonka bean camphor, glucoside, pasture stocks such as horse, ox, sheep is eaten by mistake poisoned even death.Hemp Eupatorium to agricultural, animal husbandry and the forestry etc. on ground caused the massive losses that is difficult to retrieve.Hemp Eupatorium is effectively developed, turn bane into boon, also just be significant.
Known treatment process to Hemp Eupatorium mainly contains:
Liu Shigui etc. disclose " eupatorine sterilant and preparation method thereof " in application number is the patent of 02128010.x, this method is with Hemp Eupatorium cleaning, pulverizing, organic solvent or water mixing immersion, extraction, filtration, extraction, chromatography, is concentrated into the eupatorine extract of flowing soaking paste, obtains product.And the eupatorine extract made the eupatorine pesticide product.
Zhu Zhaoyun etc. disclose " medicine of Cure for insomnia disease " in application number is 03132977.2 patent, this method is to extract water in the Hemp Eupatorium, alcohol, ether, acetic acid second junket, chloroform etc., the medically acceptable oral preparations that is prepared from by its extract and pharmaceutical excipient, preparation has sedative effect, syngignoscism improves significantly to neurasthenia, insomnia.
Flood flame springs etc. disclose " preparation method of shaving board of eupatorium adenophorum spreng " in application number is 02133712.8 patent, this method by Hemp Eupatorium through pre-treatment, flaking, drying, impregnation, applying glue are mated formation, and be hot-forming, aftertreatment technology makes shaving board of eupatorium adenophorum spreng.
Ou Yanghua etc. disclose " preparation method of Hemp Eupatorium biological organic fertilizer " in application number is 02133441.2 patent, this method is to be raw material with the Hemp Eupatorium, by coarse reduction, and detoxification treatment, fermentation, drying is pulverized, and obtains the biological organic fertilizer product.
Ou Yanghua etc. disclose " preparation method of purple eupatoria feed " in application number is 02113759.5 patent, this method is to be raw material with the Hemp Eupatorium, and undergo microbial fermentation detoxification and the comprehensive treating process of Chinese medicine toxicide are dry again, pulverize and promptly make animal and fowl fodder.
The applicant is ZL93114637.2 in the patent No., disclose a kind of method of utilizing wood chip to prepare powdered carbon in " manufacturing powdered activated carbon with microwave radiation method " by name, this method proportioning raw materials is 100 parts of wood chips, phosphoric acid 200-300 part, phosphoric acid concentration 25-81%, dipping time is more than 12 hours; The proportioning of wood chip and zinc chloride is 100 parts of wood chips, and zinc chloride is 200-300 part, and zinc oxide concentration is 8-65%, and dipping time is more than 12 hours; Type of heating is a microwave radiation, microwave frequency 2450MHz, radiated time 5-15 minute, radiation temperature 600-900 ℃.The radiation after product obtains activated carbon product through pickling, oven dry, pulverizing, screening.This method is that wood chip is a raw material, the cost of material height, and be the great cost of cutting down with the forest reserves.Technological process that this method sets and parameter are made at this specified raw material of wood chip.
The applicant is ZL02113270.4 in the patent No., name is called and discloses a kind of tobacco rod solid waste of utilizing in " microwave radiation tobacco rod solid waste prepares process of active carbon " and prepare process of active carbon, and this method is that the tobacco rod solid waste is crushed to length is 1-15mm; With purity is that to be made into concentration expressed in percentage by weight be 50% solder(ing)acid for 98% technical grade zinc chloride; The mass ratio of raw material tobacco rod and solder(ing)acid is 1 during hybrid infusion: 3.5-5, dipping time 8-10 hour; Be made into 10% aqueous hydrochloric acid and carried out pickling 5-10 hour with adding water with 36% hydrochloric acid after the microwave heating, pH reaches 7 then; Descended dry 5-10 hour at 100-120 ℃.Operational path that this method is set and parameter only are fit to this specific raw material of tobacco rod solid waste.
Peaceful equality is 200410022085.x at application number, name is called and discloses a kind of usefulness brown coal slag production process of active carbon in " a kind of with brown coal slag production process of active carbon ", and this method is that carbon content is broken to granularity less than 0.18mm at the brown coal ground-slag more than 28%; The mass ratio of brown coal slag and Ke Xingjia is 0.8-1.2 in the steeping process, and it is that the solution of 25-40% floods dipping time 3-7 hour to brown coal that Ke Xingjia is made into concentration expressed in percentage by weight; Filter cake is by hot gas drying, temperature 100-150 ℃; Dried powder activates in microwave oven, and 800-1000 ℃ of microwave radiation temperature soak time 8-10 minute, prepares coal mass active carbon.This method fixed operational path and parameter be fixed at this specific raw material of brown coal slag.
Handle at present Hemp Eupatorium in the disclosed method, Shang Weijian lives its preparation and is the report of property charcoal.Do not see the report that ultrasonic wave is used in the Preparation of Activated Carbon in dipping yet.Find a kind of effective novel method by the present invention for handling Hemp Eupatorium.
Three, summary of the invention:
The object of the present invention is to provide a kind of novel method of utilizing purple stem boneset.With the Hemp Eupatorium is raw material, with salt of wormwood or zinc chloride solid is activator, by fragmentation, ultrasonication, microwave radiation, pickling, washing and drying process, obtain activated carbon product, utilize cavitation effect of ultrasonic waves, super mix the advantage that stirs, and microwave radiation is rapidly heated, inner heating, the easy advantage of automatization control etc., shortens the process time, cuts down the consumption of energy.For the resource utilization of Hemp Eupatorium provides a kind of method of effective utilization, product charcoal absorption performance is good, the specific surface area height.
The present invention realizes that by following processing step Fig. 1 is its process flow sheet.
(1) Hemp Eupatorium is crushed to the particle of particle diameter≤3mm;
(2) be 3～6: 1 with water and Hemp Eupatorium broken material by the ratio of quality, salt of wormwood or zinc chloride solid and Hemp Eupatorium broken material are 0.5～4: 1 by mass ratio, mix;
(3) compound being put into the ultra-sonic oscillation device, is 60KHz or 200KHz in ultrasonic frequency, and power is to carry out ultrasonication 5～60min under the 50W;
(4) compound after the ultrasonication is put into the preheating of carry out microwave radiation heating device, drying, charing and the activation that power is 100W～20kW (microwave irradiation power is adjustable continuously), 6～20 minutes radiation heating time, radiation temperature is 600～950 ℃, obtains the primary activity charcoal;
(5) be that the hydrochloric acid of 10-15% carries out pickling with the primary activity charcoal concentration expressed in percentage by weight that obtains, being washed to the pH value with tap water then is 5.5～7;
(6) the later gac of washing is under 80～140 ℃ temperature dry 1～4 hour, obtains the product gac.
Ultrasonic wave is meant that range of frequency is 20～10
6The mechanical wave of kHz, velocity of wave generally are about 1500m/s, and wavelength is 10～0.01cm, in solution with a kind of form transmission of spherical wave.Ultrasonic wave itself is being carried concentrated energy, and it is when the liquid medium, when the sound pressure amplitude of sound wave negative pressure semi-period surpasses inside static pressure when strong, the cavitation nucleus that is present in the liquid will increase rapidly, the malleation that comes one after the other mutually in, cavitation nucleus is compressed suddenly again, up to collapse.When cavitation nucleus collapses, in the circumnuclear little space of inherent cavitation of extremely short time, will produce thousands of degree high temperature of reaching of moment and normal atmosphere high pressure up to a hundred in the part, and produce the microjet that speed is about 110m/s, has intense impact power, make liquid be in the HF oscillation state simultaneously, make liquid medium produce " supercavitation phenomenon ".Ultrasonic wave also has the super special efficacy that stirs that mixes, and ultrasonic wave is being carried out stirring, added the effect of " supercavitation phenomenon " transmitting medium with thousands of times pulsation p.s. in transmittance process, and making whole system be tending towards homogenizing fast.
The present invention has the following advantages:
(1) utilizing purple stem boneset, it is good to obtain absorption property, the activated carbon product that specific surface area is high, its absorption property reaches the requirement of the country-level standard of wood activated charcoal;
(2) turn bane into boon for the development and use of Hemp Eupatorium and found a new approach, created certain economic and be worth and social value;
(3) utilize cavitation effect of ultrasonic waves and the super advantage that stirs of mixing, compound is carried out ultrasonication, shorten greatly than time of common impregnation technology;
(4) utilize microwave can be directly to the heating of material inside, be rapidly heated, inner heating, easy advantages such as automatization control, the activating process time is greatly shortened, energy consumption reduces;
(5) adopt microwave radiation to carry out heat-activated, make to produce big carbon content active point in the charcoal, effectively promoted the formation of hole, improved the absorption property and the yield of gac;
(6) preheating, drying, charing and activation four-stage are integrated into a process, and the operating time is short, and product cost is low;
(7) by method utilizing purple stem boneset of the present invention, technology is simple, and is easy to operate, and condition is easy to control.
Four, description of drawings:
Fig. 1 is a process flow sheet.
Five, embodiment:
Embodiment 1: the 100g Hemp Eupatorium is crushed to≤particle of 3mm, with the ratio of water and the quality of Hemp Eupatorium broken material is 4: 1, potash solid and Hemp Eupatorium broken material are to mix at 1: 1 by mass ratio, in frequency is 60KHz, power is to carry out ultrasonication under the 50W after 15 minutes, put into microwave device, under the microwave power of 700W, carried out carry out microwave radiation heating 12 minutes, 900 ℃ of radiation temperatures, it is that 10% hydrochloric acid carries out pickling that gac after the radiation adopts concentration expressed in percentage by weight, being washed to the pH value with tap water then is 5.5～7, and drying is 4 hours under 80 ℃ temperature, obtains the recycling treatment product: gac.(requirement of GB12496.1～22-1999) is analyzed activated carbon product, and main quality index-methylene blue adsorption value is 30mL/0.1g, and iodine sorption value is 1485.37mg/g by national standard.And the methylene blue adsorption value of gac first grade is 9ml/0.1g in the national standard (GB/T13803.3-1999), and iodine sorption value is 1000mg/g.And adopting nitrogen adsorption that gac is carried out the pore structure sign, its surface-area is 1640.97m
2/ g, total pore volume is 0.7393mL/g, its micropore and mesopore are all flourishing.
Embodiment 2: the 200g Hemp Eupatorium is crushed to≤particle of 3mm, with the mass ratio of water and Hemp Eupatorium broken material is 3: 1, zinc chloride and Hemp Eupatorium broken material are to mix at 2: 1 by mass ratio, in frequency is 60KHz, power is to carry out ultrasonication under the 50W after 20 minutes, put into microwave device, carry out microwave radiation heating is 8 minutes under the microwave power of 1200W, 700 ℃ of radiation temperatures, it is that 15% hydrochloric acid carries out pickling that gac after the radiation adopts concentration expressed in percentage by weight, being washed to the pH value with tap water then is 5.5～7, and drying is 2 hours under 110 ℃ temperature, obtains the recycling treatment product: gac.(requirement of GB12496.1～22-1999) is analyzed activated carbon product, and main quality index-methylene blue adsorption value is 22mL/0.1g, and iodine sorption value is 1112.05mg/g by national standard.And the methylene blue adsorption value of gac first grade is 9ml/0.1g in the national standard (GB/T13803.3-1999), and iodine sorption value is 1000mg/g.And adopting nitrogen adsorption that gac is carried out the pore structure sign, its surface-area is 1304.57m
2/ g, total pore volume is 0.5982mL/g, wherein based on micropore, mesopore is also comparatively flourishing.
Embodiment 3: the 5kg Hemp Eupatorium is crushed to≤particle of 3mm, with the ratio of water and the quality of Hemp Eupatorium broken material is 6: 1, zinc chloride and Hemp Eupatorium broken material are to mix at 4: 1 by mass ratio, in frequency is 200KHz, power is to carry out ultrasonication under the 50W after 50 minutes, put into microwave device, carry out microwave radiation heating is 11 minutes under the microwave power of 6KW, 750 ℃ of radiation temperatures, it is that 13% hydrochloric acid carries out pickling that gac after the radiation adopts concentration expressed in percentage by weight, being washed to the pH value with tap water then is 5.5～7, and drying is 1.5 hours under 130 ℃ temperature, obtains the recycling treatment product: gac.(requirement of GB12496.1～22-1999) is analyzed activated carbon product, and main quality index-methylene blue adsorption value is 25mL/0.1g, and iodine sorption value is 1237.61mg/g by national standard.And the methylene blue adsorption value of gac first grade is 9ml/0.1g in the national standard (GB/T13803.3-1999), and iodine sorption value is 1000mg/g.And adopting nitrogen adsorption that gac is carried out the pore structure sign, its surface-area is 1467.92m
2/ g, total pore volume is 0.6538mL/g, wherein based on micropore, mesopore is also comparatively flourishing.
Claims (1)
1. the method for a utilizing purple stem boneset is after the fragmentation of raw material Hemp Eupatorium, with activator and water mixing, through ultrasonication, send into the microwave radiation device heat-activated again and obtain the primary activity charcoal, carry out pickling, washing, oven dry then and obtain activated carbon product, it is characterized in that:
1). described fragmentation to the raw material Hemp Eupatorium is the particle that it is broken into particle diameter≤3mm;
2). described activator is salt of wormwood or zinc chloride solid, and it is 0.5～4 with broken raw material by mass ratio: 1 mixes;
3). heat in the described carry out microwave radiation heating device, activation condition be microwave irradiation power at 100W～20kW, 6～20 minutes radiation heating time, radiation temperature is 600～950 ℃;
4). the employing concentration expressed in percentage by weight is that the hydrochloric acid of 10-15% carries out pickling.
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| CNB2005100110017A CN100384723C (en) | 2005-09-05 | 2005-09-05 | Method for utilizing purple stem boneset |
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| CNB2005100110017A CN100384723C (en) | 2005-09-05 | 2005-09-05 | Method for utilizing purple stem boneset |
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| CN101597055B (en) * | 2009-05-26 | 2011-04-20 | 中国科学院武汉植物园 | Method for preparing active carbon by seed cases of Jatropha curcas |
| CN102897760A (en) * | 2011-07-29 | 2013-01-30 | 中国科学院过程工程研究所 | Method for preparing activated carbon by using eupatorium adenophorum |
| CN102431993A (en) * | 2011-09-22 | 2012-05-02 | 安徽工业大学 | Method for preparing mesoporous carbon material for electrochemical capacitor by using rice hulls as raw materials |
| 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 |
| CN102862981A (en) * | 2012-09-24 | 2013-01-09 | 昆明理工大学 | Method for simultaneously producing activated carbon and medium heating value (MHV) fuel gas by using eupatorium adenophorum |
| CN103694020B (en) * | 2013-12-11 | 2015-06-10 | 攀枝花市西宇生物科技有限公司 | Comprehensive utilization process for ageratina adenophora |
| CN104692380A (en) * | 2015-02-04 | 2015-06-10 | 昆明理工大学 | Preparation method of Ageratina-adenophora-base high-specific-area activated carbon |
| CN106315579B (en) * | 2016-08-23 | 2019-04-09 | 昆明理工大学 | A kind of Eupatorium adenophorum base prepares micropore-mesopore activated carbon method |
| CN116022768A (en) * | 2023-02-16 | 2023-04-28 | 宁国海螺生物质能有限公司 | Method for uniformly dispersing powder carbon fixing agent in biomass material |
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| CN1102399A (en) * | 1993-11-10 | 1995-05-10 | 昆明工学院 | Manufacturing powdered activated carbon with microwave radiation method |
| CN1229055A (en) * | 1998-03-18 | 1999-09-22 | 邓健郎 | Method for preparing active carbon using carbon black |
| CN1362359A (en) * | 2002-01-21 | 2002-08-07 | 昆明理工大学 | Mocrowave radiation process of producing active carbon with waste tobacco stalk |
| CN1562739A (en) * | 2004-03-19 | 2005-01-12 | 昆明理工大学 | Method for producing active carbon by using cinder of brown coal |
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