CN103979537A - Hemp-stalk activated charcoal and preparation method thereof - Google Patents
Hemp-stalk activated charcoal and preparation method thereof Download PDFInfo
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- CN103979537A CN103979537A CN201410256998.1A CN201410256998A CN103979537A CN 103979537 A CN103979537 A CN 103979537A CN 201410256998 A CN201410256998 A CN 201410256998A CN 103979537 A CN103979537 A CN 103979537A
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Abstract
The invention relates to the field of activated charcoal preparation and particularly relates to hemp-stalk activated charcoal and a preparation method thereof. The method comprises the following steps: (a) kneading and aging: thoroughly mixing hemp stalks and an activator in a kneader, and aging hemp stalk fibers, so as to obtain a mixture, wherein the activator is phosphoric acid; (b) granulating: carrying out extrusion granulation on the mixture obtained in the step (a), so as to obtain a granular material; (c) shaping: shaping the granular material obtained in the step (b) by using a shaping furnace; (d) activating: activating the shaped granular material obtained in the step (c) by using an activation furnace; (e) rinsing and drying, thus obtaining the hemp-stalk activated charcoal. According to the method disclosed by the invention, the phosphoric acid is adopted as the activator and can be partially recovered in an aftertreatment rinsing process, so that the production cost is reduced; the prepared hemp-stalk activated charcoal has the iodine adsorption value of 800-1,100mg/g and the carbon tetrachloride adsorption value of 100-120%.
Description
Technical field
The present invention relates to activated carbon preparation field, be specifically related to a kind of Chinese hemp stalk gac and preparation method thereof.
Background technology
Chinese fiber crops originate from China, have the title of " source is spun by state, 10000 years clothing ancestrals ".The discovery and application of fiber crops occupies first of natural fiber.In China, historical existing more than 8000 year of the plantation of Chinese fiber crops, in Heilungkiang, the Inner Mongol, people are referred to as hemp; In Anhui, people are referred to as cold fiber crops; In Guangxi, people are referred to as fire fiber crops; All being referred to as now Chinese fiber crops (china-hemp), is also the transliteration of English " hemp ".
In recent years, along with Chinese national economy high speed development, textile garment industry is gone on motorway equally.For this reason, the consumption of Chinese fiber crops increases severely every year, and its cultivated area is also increasing year by year, and the Chinese fiber crops plantation planning of millions of mu is set about by domestic relevant department.Because China is industrial, be mainly to utilize china-hemp fibers to manufacture apparel textile or papermaking etc., meanwhile, peasant is after having gathered in china-hemp fibers for a long time, and but a large amount of Chinese hemp stalks being made a fire to cook even abandons, and causes the waste of a large amount of biomass resources.
Nearly one, 20 year, the gac that utilizes various agricultural wastes to prepare high-specific surface area and high absorption property as Pericarppium Armeniacae Amarum, nut-shell, rice husk and waste of flax etc. has caused that people more and more pay close attention to, and as the utilization of the waste of flax class of biomass resource, oneself steps into the process of research and development.Studies have reported that as the employing potassium hydrogen phosphates such as Soheil Aber be that activator is prepared bluish dogbane based active carbon fiber.The employing vapor activations such as Michio Inagaki are prepared the bluish dogbane activated carbon fiber of high-specific surface area.The employings such as Eduardo M.Cuerda Correa be take bluish dogbane and as raw material, are prepared bluish dogbane activated carbon fiber of hole prosperity etc.Equally, in recent years domestic bibliographical information and the publication that also has waste of flax class to prepare gac, the Chinese invention patent that is 200710195717.6 as application number discloses " a kind of kenaf stalk activated charcoal and preparation method thereof ", as publication number Chinese invention patent " a kind of method of preparing gac with waste of flax " that is CN102381703.A etc.The former product form is that gac powdery crude product is granulated active carbon through hydraulic pressure granulation, and the latter's product form is powdered carbon, and gained activated carbon adsorption value is low, has used potassium permanganate in preparation method, can not reclaim, and cost is high.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of employing phosphoric acid as activator, the high Chinese hemp stalk method for preparation of active carbon of charcoal absorption value making.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
The preparation method that a kind of Chinese kenaf stalk activated charcoal is provided, comprises the steps:
A, kneading and slaking: in kneader, the Chinese hemp stalk of crushing drying is fully mixed with activator, the slaking of Chinese hemp stalk fiber obtains compound, and described activator is phosphoric acid;
B, granulation: step 1 gained compound is carried out to extruding pelletization and obtain pellet, gained pellet particle diameter is 1-4mm;
C, sizing: step b gained pellet is placed in to shaping furnace and shapes;
D, activation: the pellet after the sizing of steps d gained is placed in to activation furnace and activates;
E, rinsing and dry: the pellet naturally cooling that step e gained is activated, rinsing to pH be 6-7, dry, obtain Chinese kenaf stalk activated charcoal.
The Chinese kenaf stalk activated charcoal that another technical scheme of the present invention is prepared for a kind of preparation method of above-mentioned Chinese kenaf stalk activated charcoal is provided.
Beneficial effect of the present invention is: the reserves of Chinese hemp stalk are abundant, originate more concentrated, is easy to collect, the present invention be take Chinese hemp stalk as raw material, can rationally utilize agroforestry waste resource, saves or alternative timber resources, expand gac raw material sources, also protected environment simultaneously;
Chinese hemp stalk method for preparation of active carbon technique of the present invention is simple, and without loaded down with trivial details technical process, and to adopt phosphoric acid be activator, in the rinsing process of aftertreatment, can carry out the recovery of part phosphoric acid, reduced production cost, shortens the production cycle, increases work efficiency;
The Chinese hemp stalk activated carbon-iodine adsorptive value that the inventive method makes is 800-1100mg/g, and Penetrating curve 100-120% has the very good characterization of adsorption to volatile organic solvent gas of levying.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, below in conjunction with embodiment, be explained in detail.
The design of most critical of the present invention is: take Chinese hemp stalk as raw material, adopting phosphoric acid is that activator is prepared Chinese hemp stalk gac.
Embodiment 1
The present embodiment provides a kind of preparation method of Chinese kenaf stalk activated charcoal, comprises the steps:
A, kneading and slaking: in kneader, the Chinese hemp stalk of crushing drying is fully mixed with activator, the slaking of Chinese hemp stalk fiber obtains compound, and described activator is phosphoric acid;
B, granulation: step 1 gained compound is carried out to extruding pelletization and obtain pellet, gained pellet particle diameter is 1-4mm; Granulation can be in hydraulic pressure forcing machine or spiral tablets press a kind of carrying out;
C, sizing: step b gained pellet is placed in to shaping furnace and shapes;
D, activation: the pellet after the sizing of steps d gained is placed in to activation furnace and activates;
E, rinsing and dry: the pellet naturally cooling that step e gained is activated, rinsing to pH be 6-7, dry, obtain Chinese kenaf stalk activated charcoal.
Further, in the preparation method of above-mentioned Chinese kenaf stalk activated charcoal, Chinese waste of flax in described step a is through raw material pre-treatment, and described raw material pre-treatment is: will remove the bar core of the Chinese hemp stalk of outer bast, fragmentation is sieved, broken value order is counted 5-10 order, remove the large granular impurity of the inside doping, then the Chinese hemp stalk having sieved is cleaned, remove the tiny trifle in the world matter of the inside doping, after cleaned, dry for standby.
Further, in the preparation method of above-mentioned Chinese kenaf stalk activated charcoal, in described step a, the jacket temperature of kneader is 100-200 ℃, and Chinese hemp stalk fiber curing temperature is controlled as 100-200 ℃, kneading time is 30-150min, and the degree Beaume of described phosphoric acid is 45-55 ° of Be.
Further, in the preparation method of above-mentioned Chinese kenaf stalk activated charcoal, the mass ratio of described Chinese hemp stalk and phosphoric acid is 1:1-3.Chinese hemp stalk dry weight is benchmark.
Further, in the preparation method of above-mentioned Chinese kenaf stalk activated charcoal, the setting temperature in described step c is 120-200 ℃, and shaping time is 8-24h.
Further, in the preparation method of above-mentioned Chinese kenaf stalk activated charcoal, the activation temperature of described steps d is 300-500 ℃, and soak time is 0.1-1h, and the flow that activation employing passes into air is 5-10L/min.
Further, in the preparation method of above-mentioned Chinese kenaf stalk activated charcoal, the rinsing of described step e is boiled (can reuse with rear phosphoric acid), at every turn 30min for being 10-35 ° of Be phosphoric acid with degree Beaume three times to pellet, and then boil 3-5 time with clear water, finally with clear water, rinse 30min.
Further, in the preparation method of above-mentioned Chinese kenaf stalk activated charcoal, the dry middle temperature of described step e is controlled as 110-140 ℃.
According to the Chinese hemp stalk gac of the invention described above preparation method gained, according to standard GB/T/T12496.10-1999 and GB/T12496.5-1999 regulation activated-carbon test method, detect, iodine sorption value 800-1100mg/g, Penetrating curve 100-120%, particle diameter 1-4mm, tap density 0.3-0.4g/m3, intensity is greater than 95%.The present invention is directed to the property brought into play organic solvent gas and there is very good characterization of adsorption.
Embodiment 2
The present embodiment provides a kind of preparation method of Chinese kenaf stalk activated charcoal, comprises the steps:
Chinese hemp stalk is broken, and screening, after cleaning-drying, is added in kneader by mass ratio interpolation Chinese hemp stalk and the phosphoric acid of 1:1.2, and the degree Beaume of described phosphoric acid is 45 ° of Be, mediates 130 ℃ of temperature, kneading time 30min.
Material after slaking is carried out to granulation, particle diameter 2mm.
Pellet is put into shaping furnace, 130 ℃ of design temperatures, shaping time 10h.
Pellet after sizing is packed in activation furnace, in 30min, be warming up to 350 ℃.Soaking time 10min, and pass into pressurized air, the flow of air is 10L/min.
By after the granulate cooling after activation, with 20 ° of Be phosphoric acid, carry out the phosphoric acid in recovered carbon, boil 30min, after three times, with clear water, boil 3-5 time, with clear water, rinse 30min again, 110-140 ℃ dry, the about 2mm of gained activated carbon particle size, iodine sorption value 810mg/g, Penetrating curve 102%, intensity 96%.
Embodiment 3
The present embodiment provides a kind of preparation method of Chinese kenaf stalk activated charcoal, comprises the steps:
Chinese hemp stalk is broken, and screening, after cleaning-drying, adds Chinese hemp stalk and phosphoric acid in kneader by 1:1.5 mass ratio, and described phosphoric acid degree Beaume is 150 ℃ of 55 ° of Be kneading temperature, kneading time 30min.
Material after slaking is carried out to granulation, particle diameter 3mm.
Pellet is put into shaping furnace, 150 ℃ of design temperatures, shaping time 15h.
Pellet after sizing is packed in activation furnace, in 30min, be warming up to 450 ℃.Soaking time 15min, and pass into pressurized air, 10L/min.
By after the granulate cooling after activation, with 26 ° of Be phosphoric acid, carry out the phosphoric acid in recovered carbon, boil 30min, after three times, with clear water, boil 3-5 time, then rinse 30min with clear water, the dry about 3mm of gained activated carbon particle size, iodine sorption value 850mg/g, Penetrating curve 112%, intensity 96.2%.
Embodiment 4
The present embodiment provides a kind of preparation method of Chinese kenaf stalk activated charcoal, comprises the steps:
Chinese hemp stalk is broken, and screening, after cleaning-drying, adds Chinese hemp stalk and phosphoric acid in kneader by 1:3 mass ratio, and described phosphoric acid degree Beaume is 200 ℃ of 50 ° of Be kneading temperature, kneading time 150min.
Material after slaking is carried out to granulation, particle diameter 4mm.
Pellet is put into shaping furnace, 200 ℃ of design temperatures, shaping time 15h.
Pellet after sizing is packed in activation furnace, in 30min, be warming up to 500 ℃.Soaking time 10min, and pass into pressurized air, 10L/min.
By after the granulate cooling after activation, with 35 ° of Be phosphoric acid, carry out the phosphoric acid in recovered carbon, boil 30min, after three times, with clear water, boil 3-5 time, then rinse 30min with clear water, the dry about 4mm of gained activated carbon particle size, iodine sorption value 900mg/g, Penetrating curve 116%, intensity 96.6%.
Embodiment 5
The present embodiment provides a kind of preparation method of Chinese kenaf stalk activated charcoal, comprises the steps:
Chinese hemp stalk is broken, and screening, after cleaning-drying, adds Chinese hemp stalk and phosphoric acid in kneader by 1:1 mass ratio, 100 ℃ of kneading temperature, kneading time 30min.
Material after slaking is carried out to granulation, particle diameter 1mm.
Pellet is put into shaping furnace, 120 ℃ of design temperatures, shaping time 8h.
Pellet after sizing is packed in activation furnace, in 30min, be warming up to 500 ℃.Soaking time 30min, and pass into pressurized air, 10L/min.
By after the granulate cooling after activation, with 10 ° of Be phosphoric acid, carry out the phosphoric acid in recovered carbon, boil 30min, after three times, with clear water, boil 3-5 time, then rinse 30min with clear water, the dry about 1mm of gained activated carbon particle size, iodine sorption value 920mg/g, Penetrating curve 110%, intensity 97%.
In sum, Chinese hemp stalk method for preparation of active carbon technique provided by the invention is simple, without loaded down with trivial details technical process, employing phosphoric acid is activator, in the rinsing process of aftertreatment, can carry out the recovery of part phosphoric acid, has reduced production cost, shorten the production cycle, increase work efficiency; The Chinese hemp stalk activated carbon-iodine adsorptive value making is 800-1100mg/g, and Penetrating curve 100-120% has the very good characterization of adsorption to volatile organic solvent gas of levying.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention to do, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (9)
1. a preparation method for Chinese kenaf stalk activated charcoal, is characterized in that, comprises the steps:
A, kneading and slaking: in kneader, the Chinese hemp stalk of crushing drying is fully mixed with activator, the slaking of Chinese hemp stalk fiber obtains compound, and described activator is phosphoric acid;
B, granulation: step 1 gained compound is carried out to extruding pelletization and obtain pellet, gained pellet particle diameter is 1-4mm;
C, sizing: step b gained pellet is placed in to shaping furnace and shapes;
D, activation: the pellet after the sizing of steps d gained is placed in to activation furnace and activates;
E, rinsing and dry: the pellet naturally cooling that step e gained is activated, rinsing to pH be 6-7, dry, obtain Chinese kenaf stalk activated charcoal.
2. the preparation method of Chinese kenaf stalk activated charcoal according to claim 1, it is characterized in that, Chinese waste of flax in described step a is through raw material pre-treatment, described raw material pre-treatment is: the Chinese hemp stalk fragmentation of removing outer bast is sieved, remove the large granular impurity of the inside doping, again the Chinese hemp stalk having sieved is cleaned, remove the tiny trifle in the world matter of the inside doping, after cleaning, dry.
3. the preparation method of Chinese kenaf stalk activated charcoal according to claim 1, is characterized in that, in described step a, the temperature of Chinese hemp stalk fiber slaking is controlled as 100-200 ℃, and kneading time is 30-150min, and the degree Beaume of described phosphoric acid is 45-55 ° of Be.
4. the preparation method of Chinese kenaf stalk activated charcoal according to claim 3, is characterized in that, the mass ratio of described Chinese hemp stalk and phosphoric acid is 1:1-3.
5. the preparation method of Chinese kenaf stalk activated charcoal according to claim 1, is characterized in that, the setting temperature in described step c is 120-200 ℃, and shaping time is 8-24h.
6. the preparation method of Chinese kenaf stalk activated charcoal according to claim 1, is characterized in that, the activation temperature of described steps d is 300-500 ℃, and soak time is 0.1-1h, adds fluidizing air during activation.
7. the preparation method of Chinese kenaf stalk activated charcoal according to claim 1, it is characterized in that, the rinsing of described step e is is that 10-35 ° of Be phosphoric acid boils three times pellet with degree Beaume, each 30min, and then boil 3-5 time with clear water, finally with clear water, rinse 30min.
8. the preparation method of Chinese kenaf stalk activated charcoal according to claim 1, is characterized in that, the dry middle temperature of described step e is controlled as 110-140 ℃.
9. the Chinese kenaf stalk activated charcoal of preparing according to the preparation method of the Chinese kenaf stalk activated charcoal described in claim 1-8 any one.
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| CN105197926A (en) * | 2015-08-18 | 2015-12-30 | 南京林业大学 | Method for preparing activated carbon with enzymatic hydrolysis lignin as raw material |
| CN106520750A (en) * | 2016-12-08 | 2017-03-22 | 浙江海洋大学 | Immobilized microbial repairing agent for spilled oil and preparation method thereof |
| CN106607007A (en) * | 2015-10-20 | 2017-05-03 | 北京林业大学 | Preparation method for MgO loaded china-hemp stalk activated carbon |
| CN106608622A (en) * | 2015-10-20 | 2017-05-03 | 北京林业大学 | Method for preparing hemp-stem-based active carbon through microwaves |
| CN106608625A (en) * | 2015-10-20 | 2017-05-03 | 北京林业大学 | Preparation method for China hemp stem-tree root mixed active carbon |
| CN110203929A (en) * | 2019-05-13 | 2019-09-06 | 中国地质大学（武汉） | A kind of Chinese hemp stalk pilum shaped activated carbon with wide spectrum characterization of adsorption |
| CN110436461A (en) * | 2018-05-02 | 2019-11-12 | 新奥科技发展有限公司 | A kind of active carbon and preparation method thereof |
| CN111170319A (en) * | 2020-02-15 | 2020-05-19 | 太原理工大学 | Method for preparing high-performance activated carbon for automobile carbon tank by using mycelia |
| CN111672476A (en) * | 2020-06-24 | 2020-09-18 | 黑龙江省科学院大庆分院 | Preparation method and application of modified hemp extraction waste adsorption material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105197926A (en) * | 2015-08-18 | 2015-12-30 | 南京林业大学 | Method for preparing activated carbon with enzymatic hydrolysis lignin as raw material |
| CN106607007A (en) * | 2015-10-20 | 2017-05-03 | 北京林业大学 | Preparation method for MgO loaded china-hemp stalk activated carbon |
| CN106608622A (en) * | 2015-10-20 | 2017-05-03 | 北京林业大学 | Method for preparing hemp-stem-based active carbon through microwaves |
| CN106608625A (en) * | 2015-10-20 | 2017-05-03 | 北京林业大学 | Preparation method for China hemp stem-tree root mixed active carbon |
| CN106608625B (en) * | 2015-10-20 | 2019-01-04 | 北京林业大学 | A kind of technique of Chinese hemp stalk, tree root mixed active charcoal |
| CN106520750A (en) * | 2016-12-08 | 2017-03-22 | 浙江海洋大学 | Immobilized microbial repairing agent for spilled oil and preparation method thereof |
| CN110436461A (en) * | 2018-05-02 | 2019-11-12 | 新奥科技发展有限公司 | A kind of active carbon and preparation method thereof |
| CN110203929A (en) * | 2019-05-13 | 2019-09-06 | 中国地质大学（武汉） | A kind of Chinese hemp stalk pilum shaped activated carbon with wide spectrum characterization of adsorption |
| CN111170319A (en) * | 2020-02-15 | 2020-05-19 | 太原理工大学 | Method for preparing high-performance activated carbon for automobile carbon tank by using mycelia |
| CN111672476A (en) * | 2020-06-24 | 2020-09-18 | 黑龙江省科学院大庆分院 | Preparation method and application of modified hemp extraction waste adsorption material |
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