CN109721053A - A kind of preparation method of fast-growing eucalyptus leather activated char - Google Patents

A kind of preparation method of fast-growing eucalyptus leather activated char Download PDF

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CN109721053A
CN109721053A CN201910062523.1A CN201910062523A CN109721053A CN 109721053 A CN109721053 A CN 109721053A CN 201910062523 A CN201910062523 A CN 201910062523A CN 109721053 A CN109721053 A CN 109721053A
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eucalyptus
fast
preparation
activated char
growing
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刘峥
韦梦琴
冯庆革
孙翔
马大朝
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Guangxi University
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Guangxi University
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Abstract

The invention belongs to prepare technical field of active carbon using abandoned biomass, and in particular to a kind of preparation method of fast-growing eucalyptus leather activated char.A kind of preparation method of fast-growing eucalyptus leather activated char, comprises the following steps that (1) cleans eucalyptus barks, dries, and crushes, dry, is sealed;(2) it will impregnate, clean by the eucalyptus barks of step (1) processing, drying obtains pretreatment sample;(3) pretreatment sample for obtaining step (2), pyrolysis carbonization, takes out, rinses after being cooled to room temperature, and dries, and grinds to get the fast-growing eucalyptus leather activated char.The active carbon that the present invention is prepared has more rich central hole structure and surface functional group, and the active carbon that adsorption capacity is prepared with other methods compares favourably, and preparation method of the invention, simple to operate, with preferable industrial application value.

Description

A kind of preparation method of fast-growing eucalyptus leather activated char
Technical field
The invention belongs to prepare technical field of active carbon using abandoned biomass, and in particular to a kind of fast-growing eucalyptus barks activity The preparation method of charcoal.
Background technique
Acticarbon has huge specific surface area, flourishing pore structure, surface functional group abundant and excellent Different physicochemical property is widely used in the fields such as soil, wastewater treatment, gas purification, electrode material and catalyst carrier.Through Research report, the raw material of traditional commercial activated carbons are usually based on coal base, such as lignite, bituminous coal;The work of biological material Property charcoal usually using timber as raw material, such as timber, bamboo compare using coal base as the active carbon of raw material, and biological material comes Source is extensive, cheap easy acquisition.In recent years, due to coal resource it is continuous reduction and it is non-renewable, and country to natural What woods was felled orders within a certain time, is that raw material prepares active carbon as an important project using discarded biomass resource.
Guangxi is that Chinese fast-growing eucalyptus plants area, the largest province, and according to statistics, 2001 so far, and the fast-growing woods gross area will be added to 2000000 hm2, artificial forest area reach ten thousand hm2 more than 3000, the half of the Zhan Quanguo eucalyptus gross area, year forest pathogen reach 3681.8 ten thousand m3, are the first in the nation.But annual generate largely discards fast-growing eucalyptus barks disposal options mostly based on burning, The processing mode of this extensive style causes greatly pollution and the unreasonable utilization to biomass resource to natural environment. The carbon content of fast-growing eucalyptus barks is higher, is found according to the analysis of the organic principle to eucalyptus barks, cellulose, hemicellulose, wood Ratio contained by quality is respectively 46.81%, 32.72%, 19.69%, can be used as the high-quality predecessor for preparing absorbent charcoal material. More importantly the invention can solve the handling problems of rural area of Guangxi fast-growing eucalyptus barks waste, it is allowed to turn waste into wealth, Clean energy resource has prevented to realize the minimizing and " with pollution treatment of giving up " of agricultural wastes because of the environmental pollution caused by burning every year Resource utilization, have significant environmental benefit, Social benefit and economic benefit.
Active carbon is mainly determined the suction-operated of pollutant by pore structure and surface chemical property.Wherein, hole Structure plays an important role to the conveying of pollutant and offer adsorption site.Studies have shown that activated carbon capillary is main Suction-operated, mesoporous, macropore carry out absorption in assistant micropore and play considerable effect, it was reported that mesoporous not only contributes to The transmission of small molecule contaminants can also occur capillary condensation in certain condition and carry out suction-operated.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
To solve above-mentioned existing issue, the present invention provides a kind of preparation method of fast-growing eucalyptus leather activated char.
The technical solution of the present invention is as follows:
A kind of preparation method of fast-growing eucalyptus leather activated char, comprises the following steps that
(1) eucalyptus barks cleaned, are dried, be put into pulverizer and be ground into clast, be placed in freeze-day with constant temperature 12h in drying box, It is cooled to room temperature, is sealed;
(2) it will be mixed by the eucalyptus barks of step (1) processing with the deionized water solution of activator, impregnate, dried after cleaning It is dry, obtain pretreatment sample;
(3) pretreatment sample that step (2) obtains is placed in tube furnace, carbonization, Temperature fall is pyrolyzed under nitrogen atmosphere It is taken out to 200 DEG C or less, is rinsed with deionized water to neutrality after being cooled to room temperature, be placed in drying box and dry, ground to get institute State fast-growing eucalyptus leather activated char.
Preferably, the sieve that clast can be all 5-10mm by aperture in step (1).
Preferably, the temperature in step (1) and step (2) in drying box is 105 DEG C.
Preferably, activator selects potassium pyrophosphate in step (2).
Preferably, the mass ratio of eucalyptus barks and activator is 1:0.5-2 in step (2).
Preferably, dip time is 12h in step (2).
Preferably, being pyrolyzed Carbonization Conditions in step (3) are as follows: nitrogen flow rate 0.4L/min, heating rate 10-30 DEG C/min, it is warming up to 550-750 DEG C, and keep temperature 30-90min.
Compared with prior art, the invention has the following beneficial effects:
(1) it is raw material that the preparation method of fast-growing eucalyptus leather activated char of the present invention, which is using discarded eucalyptus barks, no Only consuming cost is low, economizes on resources, and the Resource Rationalization for realizing discarded eucalyptus barks to a certain extent utilizes, and also solves discarded Eucalyptus barks are to environment bring pressure.
(2) active carbon being prepared using preparation method of the invention is had pore structure abundant, biggish compares table Area and more rich surface functional group.
(3) preparation method of the invention, simple to operate.And under suitable activators dipping and carbonization condition, reaction Speed is fast, has saved time and the energy, has preferable industrial application value.
Detailed description of the invention
Fig. 1 is nitrogen adsorption-desorption curve figure and the hole BJH of fast-growing eucalyptus leather activated char obtained by 1-4 of the embodiment of the present invention Diameter distribution map;
Fig. 2 is the infrared spectrogram of fast-growing eucalyptus leather activated char obtained by 1-4 of the embodiment of the present invention;
Fig. 3 is the LR laser raman analysis chart of fast-growing eucalyptus leather activated char obtained by 1-4 of the embodiment of the present invention;
Fig. 4 is the X-ray diffraction analysis figure of fast-growing eucalyptus leather activated char obtained by 1-4 of the embodiment of the present invention;
Explanation in relation to attached drawing are as follows:
1- embodiment 1,2- embodiment 2,3- embodiment 3,4- embodiment 4.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention Shield range is not limited by the specific implementation.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " includes " or its change Changing such as "comprising" or " including " etc. will be understood to comprise stated element or component, and not exclude other members Part or other component parts.
Embodiment 1
A kind of preparation method of fast-growing eucalyptus leather activated char, comprises the following steps that
(1) eucalyptus barks cleaned, dried, be put into pulverizer and be ground into clast, be placed in freeze-day with constant temperature in 105 DEG C of drying boxes 12h is cooled to room temperature, and is sealed;
(2) it will be mixed by the eucalyptus barks of step (1) processing with the deionized water solution of potassium pyrophosphate, impregnate 12h, clean It is placed on freeze-day with constant temperature 12h in 105 DEG C of drying boxes, obtains pretreatment sample;
(3) pretreatment sample that step (2) obtains is placed in tube furnace, carbonization, Temperature fall is pyrolyzed under nitrogen atmosphere To 200 DEG C take out, rinsed with deionized water to neutrality after being cooled to room temperature, be placed in 105 DEG C of drying boxes and dry, grinding to get The fast-growing eucalyptus leather activated char;
Wherein, the sieve that clast can be all 5mm by aperture in step (1);Eucalyptus barks and potassium pyrophosphate in step (2) Mass ratio be 1:0.5;Carbonization Conditions are pyrolyzed in step (3) are as follows: nitrogen flow rate 0.4L/min, heating rate is 20 DEG C/ Min is warming up to 750 DEG C, and keeps temperature 60min.
Embodiment 2
A kind of preparation method of fast-growing eucalyptus leather activated char, comprises the following steps that
(1) eucalyptus barks cleaned, dried, be put into pulverizer and be ground into clast, be placed in freeze-day with constant temperature in 105 DEG C of drying boxes 12h is cooled to room temperature, and is sealed;
(2) it will be mixed by the eucalyptus barks of step (1) processing with the deionized water solution of potassium pyrophosphate, impregnate 12h, clean It is placed on freeze-day with constant temperature 12h in 105 DEG C of drying boxes, obtains pretreatment sample;
(3) pretreatment sample that step (2) obtains is placed in tube furnace, carbonization, Temperature fall is pyrolyzed under nitrogen atmosphere To 180 DEG C take out, rinsed with deionized water to neutrality after being cooled to room temperature, be placed in 105 DEG C of drying boxes and dry, grinding to get The fast-growing eucalyptus leather activated char;
Wherein, the sieve that clast can be all 7mm by aperture in step (1);Eucalyptus barks and potassium pyrophosphate in step (2) Mass ratio be 1:2;Carbonization Conditions are pyrolyzed in step (3) are as follows: nitrogen flow rate 0.4L/min, heating rate are 20 DEG C/min, 750 DEG C are warming up to, and keeps temperature 60min.
Embodiment 3
A kind of preparation method of fast-growing eucalyptus leather activated char, comprises the following steps that
(1) eucalyptus barks cleaned, dried, be put into pulverizer and be ground into clast, be placed in freeze-day with constant temperature in 105 DEG C of drying boxes 12h is cooled to room temperature, and is sealed;
(2) it will be mixed by the eucalyptus barks of step (1) processing with the deionized water solution of potassium pyrophosphate, impregnate 12h, clean It is placed on freeze-day with constant temperature 12h in 105 DEG C of drying boxes, obtains pretreatment sample;
(3) pretreatment sample that step (2) obtains is placed in tube furnace, carbonization, Temperature fall is pyrolyzed under nitrogen atmosphere To 150 DEG C take out, rinsed with deionized water to neutrality after being cooled to room temperature, be placed in 105 DEG C of drying boxes and dry, grinding to get The fast-growing eucalyptus leather activated char;
Wherein, the sieve that clast can be all 8mm by aperture in step (1);Eucalyptus barks and potassium pyrophosphate in step (2) Mass ratio be 1:1;Carbonization Conditions are pyrolyzed in step (3) are as follows: nitrogen flow rate 0.4L/min, heating rate are 30 DEG C/min, 750 DEG C are warming up to, and keeps temperature 60min.
Embodiment 4
A kind of preparation method of fast-growing eucalyptus leather activated char, comprises the following steps that
(1) eucalyptus barks cleaned, dried, be put into pulverizer and be ground into clast, be placed in freeze-day with constant temperature in 105 DEG C of drying boxes 12h is cooled to room temperature, and is sealed;
(2) it will be mixed by the eucalyptus barks of step (1) processing with the deionized water solution of potassium pyrophosphate, impregnate 12h, clean It is placed on freeze-day with constant temperature 12h in 105 DEG C of drying boxes, obtains pretreatment sample;
(3) pretreatment sample that step (2) obtains is placed in tube furnace, carbonization, Temperature fall is pyrolyzed under nitrogen atmosphere To 130 DEG C take out, rinsed with deionized water to neutrality after being cooled to room temperature, be placed in 105 DEG C of drying boxes and dry, grinding to get The fast-growing eucalyptus leather activated char;
Wherein, the sieve that clast can be all 10mm by aperture in step (1);Eucalyptus barks and pyrophosphoric acid in step (2) The mass ratio of potassium is 1:2;Carbonization Conditions are pyrolyzed in step (3) are as follows: nitrogen flow rate 0.4L/min, heating rate is 10 DEG C/ Min is warming up to 650 DEG C, and keeps temperature 60min.
The obtained eucalyptus leather activated char of embodiment 1-4 is to the adsorptive value such as table 1 of methylene blue and iodine, specific surface area and hole Gap structure parameter such as table 2, nitrogen adsorption-desorption curve such as Fig. 1, infrared spectrum analysis such as Fig. 2, Laser Roman spectroscopic analysis of composition is as schemed 3, X-ray diffraction analysis such as Fig. 4.
The methylene blue adsorption value and iodine sorption value of fast-growing eucalyptus leather activated char obtained by 1 1-4 of the embodiment of the present invention of table
As can be seen from Table 1, eucalyptus leather activated char obtained by 1-4 of the embodiment of the present invention has preferable suction to methylene blue and iodine Attached effect, wherein iodine sorption value is up to 1077.22, illustrates that there are more rich mesoporous and micro- using active carbon prepared by the present invention Pore structure.
The specific surface area and gap structure parameter of fast-growing eucalyptus leather activated char obtained by 2 1-4 of the embodiment of the present invention of table
As can be seen from Table 2, the specific surface area of eucalyptus leather activated char obtained by 1-4 of the embodiment of the present invention reaches as high as 619m2/ G, total hole volume reach as high as 0.7766cm3/ g illustrates there is biggish specific surface area using active carbon prepared by the present invention.
As seen from Figure 3, there is eucalyptus barks activated carbon surface obtained by 1-4 of the embodiment of the present invention-OH, C-O, C=O etc. to contain Oxygen functional group illustrates using the more rich surface functional group of active carbon prepared by the present invention.
As seen from Figure 4, eucalyptus leather activated char obtained by 1-4 of the embodiment of the present invention is undefined structure, and disordering journey It spends larger, forms more defects, increase pore structure and specific surface area, this is corresponding to the resulting result of Tables 1 and 2.
In conclusion the active carbon being prepared using preparation method of the invention, there is pore structure abundant, larger Specific surface area and more rich surface functional group.
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.

Claims (7)

1. a kind of preparation method of fast-growing eucalyptus leather activated char, which is characterized in that comprise the following steps that
(1) eucalyptus barks cleaned, dried, be put into pulverizer and be ground into clast, be placed in freeze-day with constant temperature 12h in drying box, it is cooling To room temperature, it is sealed;
(2) will mix, impregnate with the deionized water solution of activator by the eucalyptus barks of step (1) processing, it is clean be placed on it is dry Freeze-day with constant temperature 12h, obtains pretreatment sample in dry case;
(3) pretreatment sample that step (2) obtains is placed in tube furnace, carbonization is pyrolyzed under nitrogen atmosphere, is naturally cooling to 200 DEG C or less take out, rinsed with deionized water to neutrality after being cooled to room temperature, be placed in drying box and dry, grind to get the speed Raw eucalyptus leather activated char.
2. the preparation method of fast-growing eucalyptus leather activated char according to claim 1, which is characterized in that clast in step (1) The sieve that can be all 5-10mm by aperture.
3. the preparation method of fast-growing eucalyptus leather activated char according to claim 1, which is characterized in that step (1) and step (2) temperature in drying box is 105 DEG C.
4. the preparation method of fast-growing eucalyptus leather activated char according to claim 1, which is characterized in that activation in step (2) Potassium pyrophosphate is selected in agent.
5. the preparation method of fast-growing eucalyptus leather activated char according to claim 1, which is characterized in that eucalyptus in step (2) The mass ratio of skin and activator is 1:0.5-2.
6. the preparation method of fast-growing eucalyptus leather activated char according to claim 1, which is characterized in that dipping in step (2) Time is 12h.
7. the preparation method of fast-growing eucalyptus leather activated char according to claim 1, which is characterized in that pyrolysis in step (3) Carbonization Conditions are as follows: nitrogen flow rate 0.4L/min, heating rate are 10-30 DEG C/min, are warming up to 550-750 DEG C, and keep temperature Spend 30-90min.
CN201910062523.1A 2019-01-23 2019-01-23 A kind of preparation method of fast-growing eucalyptus leather activated char Pending CN109721053A (en)

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