CN108715446A - A kind of preparation method of more mesoporous Lignin-Based Activated Carbons - Google Patents
A kind of preparation method of more mesoporous Lignin-Based Activated Carbons Download PDFInfo
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- CN108715446A CN108715446A CN201810721828.4A CN201810721828A CN108715446A CN 108715446 A CN108715446 A CN 108715446A CN 201810721828 A CN201810721828 A CN 201810721828A CN 108715446 A CN108715446 A CN 108715446A
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- C01B32/318—Preparation characterised by the starting materials
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- C—CHEMISTRY; METALLURGY
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Abstract
The present invention provides a kind of preparation method of more mesoporous Lignin-Based Activated Carbons, including step：(1) acid precipitation method separation and Extraction alkali lignin powder from pulping and paper-making is used；(2) alkali lignin powder is heated to 500 DEG C~900 DEG C from room temperature, stops heating after being kept for 1~2 hour, obtains alkali lignin base charcoal；(3) it under the conditions of gas shield, uses vapor and zinc chloride for activator, activates alkali lignin base charcoal at being 600 DEG C~900 DEG C in temperature, obtain alkali lignin matrix activated carbon.Preparation method proposed by the present invention, the alkali lignin matrix activated carbon of gained has excellent physicochemical property, mesoporous greatly increases, adsorption and desorption ability is improved, and can be widely applied to the fields such as environmental protection, electronics, medical sanitary, chemical industry with its special surface chemical structure and physical adsorption characteristic.Also, the method for the present invention is easy to operate, less energy consumption, time-consuming short, has preferable prospects for commercial application.
Description
Technical field
The invention belongs to activated carbon preparing technical fields, and in particular to a kind of to utilize plant pulping and paper-making waste liquid for raw material system
The method of standby high mesoporosity activated carbon.
Background technology
As one of most important industrial adsorbents, activated carbon, which is one kind, having high specific surface area, flourishing pore structure,
It is easy after a variety of surface functional groups (such as hydroxyl, carboxyl, carbonyl), preferable mechanical strength and heat-resisting, acidproof, alkaline-resisting, failure
The carbonaceous material for the characteristics such as regenerating and utilizing, can be widely applied to liquid phase processing, gas phase purifying, organic solvent recycling, aviation,
Military affairs, food, catalyst carrier, electrode material etc..Currently, the raw material for preparing activated carbon mostlys come from fossil class resource
(bituminous coal, lignite, pitch etc.) and biomass resource (timber, shell, bamboo wood etc.).However, it is increasingly in short supply with petroleum resources,
And exploitation and use during caused by environmental disruption with pollution, and country to wildwood business felling forbid, in height
Degree advocates today of energy greenization, and the raw material that can be used for green production activated carbon gradually decreases, and how to use sustainable life
Physical obsolescence resource is that raw material prepares activated carbon as an important topic.
Lignin is the second largest abundant biomass resource in the world, is only second to cellulose.Currently, domestic pulp and paper making
Up to 50,000,000 tons/year of content of lignin in the black liquor of discharge, and 5% of the part being used effectively less than total amount, it is remaining
Part is discharged discarded or burning.The functional materials such as activated carbon are prepared into using lignin and high-valued processing, can not only be reached
To turn waste into wealth and realize activated carbon raw material sustainability purpose, but also can be to avoid polluting the environment and break
It is bad, therefore, there is great strategic importance in resources reserve and environmental protection etc..
The raw material for being presently used for preparing Lignin-Based Activated Carbon is concentrated mainly on lignosulfonates, sulfate-reducing conditions
With acid-hydrolysis lignin etc., and the research that activated carbon is prepared using alkali lignin is less.Meanwhile preparing Lignin-Based Activated Carbon
Method, which mainly uses, has many advantages, such as low reaction temperature, specific surface area and the high chemical activation method of yield, but the activity obtained
Charcoal mesoporous is relatively low.Therefore, for high-valued sharp lignin, and the mesoporous of activated carbon is improved, widens answering for activated carbon
With efficiency and range, there is an urgent need to a kind of preparations that can effectively prepare the Lignin-Based Activated Carbon containing larger proportion mesoporous
Method.
Invention content
For this field there are the problem of, the purpose of the present invention is to provide it is a kind of using re-activation alkali lignin prepare
The preparation method of high mesoporosity activated carbon.
Another object of the present invention is to provide a kind of alkali lignin matrix activated carbons with more mesoporous.
Realize that the technical solution of the object of the invention is：
A kind of preparation method of more mesoporous Lignin-Based Activated Carbons, which is characterized in that including step：
(1) black liquor powder is mixed with water, is filtered using filter paper after stirring evenly, remove the insoluble matter in black liquor；Take filter
Hydrochloric acid is gradually added in liquid, and is centrifuged and precipitated using low speed centrifuge, then suitable quantity of water is added into precipitation and stirs evenly, then
Final gained pellet frozen is dried, finally obtains alkali lignin powder by secondary centrifugation.
(2) under the conditions of gas shield, alkali lignin powder is heated to 600 DEG C~900 DEG C from room temperature, holding 1~2 is small
When after stop heating, alkali lignin base charcoal is made in natural cooling；
(3) under the conditions of gas shield, use vapor and zinc chloride for activator, in the case where temperature is 500 DEG C~900 DEG C
Alkali lignin base charcoal is activated, alkali lignin matrix activated carbon is obtained；
Gas in step (2) and step (3) for protecting is one or more in nitrogen, argon gas, helium.Step
(3) activation process activation sequence changes in.
Gas in step (2) and step (3) for protecting is one or more in nitrogen, argon gas, helium.
Wherein, the alkali lignin powder is the lignin isolated from pulping and paper-making waste liquid, dry and levigate to grain
Diameter 0.5mm or less.
Further, the method for separating lignin is from pulping and paper-making waste liquid：Pulping and paper-making waste liquid is adjusted to contain admittedly
The solution of amount 10~18%, filtering remove the insoluble matter in solution, and the pH value that hydrochloric acid is added to solution is 2.0~3.0, solid-liquid point
From taking precipitation dry and levigate.
Preferably, in the step (2), the temperature of alkali lignin powder charing is 600 DEG C, time 1h.
Wherein, in the step (2), the heating rate that 600 DEG C~900 DEG C are heated to from room temperature is 4~10 DEG C/min.
Wherein, in the step (3), as water vapour and the gas mixing for protection of activator, for protection
The flow velocity of gas is 200mL/min, and the flow of vapor is 4g/min-5g/min.Zinc chloride as activator it is a concentration of
Between 15%-45%, ratio when being mixed with raw material is 1:1-1:Between 5.
Further, in activation process, activation method has the difference of sequence twice, has first steam activation in activation
Steam activation or vapor are carried out at the same time with zinc chloride activation again after zinc chloride activation, or first zinc chloride activation again afterwards.
The alkali lignin matrix activated carbon that preparation method of the present invention is prepared.
By many experiments, in conjunction with as a result, inventor has found in three steps, alkali lignin powder is in charing
The flow of activator vapor when carbonization temperature, carbonization time and heating rate, activation process, activator chlorination zinc concentration,
The sequence of activation method is key factor when the mixed proportion of zinc chloride and raw material, soak time and activation.Alkali lignin powder
In charing, carbonization temperature is higher, is more conducive to the discharge of non-carbon element, the carbon content of obtained alkali lignin base charcoal is higher；It rises
Warm rate is lower, is more conducive to carbonize；The amount and chlorination zinc concentration of vapor are bigger, are more conducive to activate, and obtain more
Mesoporous, activation process processing time is longer, and alkali lignin base charcoal is activated the more severe of agent water vapor encroachment, the poroid knot of formation
Structure is also more, and final mesoporous is also higher.
By controlling the above key factor, the maximum specific surface area of the alkali lignin matrix activated carbon of gained can reach
1513m2/ g, total pore volume can reach 1.187mL/g, and mesoporous can reach 73.3%, be more than the previous water using conventional procedures
The specific surface area of the alkali lignin matrix activated carbon of steam activation research (is less than 100m2/ g) with mesoporous (48-56%) and existing
Specific surface area (700~1500m of activated carbon in the market2/ g) and mesoporous (45-60%).
The beneficial effects of the present invention are：
The alkali lignin matrix activated carbon of preparation method proposed by the present invention, gained has excellent physicochemical property, mesoporous
Rate greatly increases, and adsorption and desorption ability is improved, and with its special surface chemical structure and physical adsorption characteristic
It can be widely applied to the fields such as environmental protection, electronics, medical sanitary, chemical industry.Also, the method for the present invention is easy to operate, less energy consumption, consumption
When it is short, have preferable prospects for commercial application.
Description of the drawings
Fig. 1 is nitrogen adsorption-desorption curve figure of activated carbon prepared by the embodiment of the present invention 1.Wherein, relative pressure is nitrogen
Qi leel presses the ratio with the saturated vapor pressure of nitrogen under liquid nitrogen temperature.
Fig. 2 is nitrogen adsorption-desorption curve figure of activated carbon prepared by the embodiment of the present invention 2.
Fig. 3 is nitrogen adsorption-desorption curve figure of activated carbon prepared by the embodiment of the present invention 3.
Fig. 4 is nitrogen adsorption-desorption curve figure of activated carbon prepared by the embodiment of the present invention 4.
Fig. 5 is nitrogen adsorption-desorption curve figure of activated carbon prepared by reference examples 1 of the present invention.
Specific implementation mode
Technical solution is further illustrated the present invention with specific embodiment below.Those skilled in the art are it is to be understood that reality
It applies example and is merely to illustrate the present invention, be not used in and limit the scope of the invention.
In embodiment, unless otherwise instructed, technological means used is this field conventional technology.In embodiment, add
Each raw material entered is commercially available convenient source unless otherwise indicated.
Embodiment 1：
400g black liquor powder and suitable water are mixed, the solution that concentration is about 15% is configured to, after stirring evenly
The qualitative filter paper for being 10~15 μm with aperture filters, and removes the insoluble matter in black liquor.Filtered filtrate is taken to be added several times dense
Degree is that the hydrochloric acid of 6mol/L, with magnetic stirrer 20min, then uses until after the pH value of solution is adjusted to 2.5 or so
Aperture is that 10~15 μm of qualitative filter paper is filtered solution, and precipitation is taken out and is dried in vacuo, sample is completely dried again
Grinding after 60 mesh sieve by that can obtain alkali lignin powder.
The liquor zinci chloridi of alkali lignin powder and a concentration of 30% is pressed 1:3 ratio mixing, using magnetic stirring apparatus
2h is stirred, after being dried in electric drying oven with forced convection, then the raw material after drying is placed in activation furnace, is 99.9% in purity
It under nitrogen protection, keeps 20min to drain retort inner air in room temperature, then from room temperature is heated to 800 DEG C and in the temperature
Lower heat preservation 1h；The alkali lignin powder after chemical activation is obtained after cooled to room temperature；Using the hydrochloric acid pair of 1mol/L
It is washed, and reuses tap water and its pH value is washed till neutrality, and finally drying obtains alkali lignin matrix activated carbon.
Alkali lignin matrix activated carbon obtained is heated to 900 DEG C from room temperature, whole process is in the atmosphere of nitrogen, nitrogen
Using flow velocity be 200mL/min, use vapor flow be 4g/min activation alkali lignin base charcoal 60min, it is wooden to obtain alkali
Plain matrix activated carbon.
The Autosorb-1 nitrogen adsorption instrument provided using Quantachrome instrument companies, obtained nitrogen adsorption desorption
Curve graph is shown in Fig. 1, use multiple spot BET method survey the specific surface area for the alkali lignin matrix activated carbon that institute the present embodiment obtains for
1458m2/ g measures total pore volume using the corresponding nitrogen capacity of nitrogen adsorption curve relative pressure peak and has reached 1.101mL/
G uses the mesopore volume rate that BJH methods measure for 64.2%.
Embodiment 2
Alkali lignin powder is prepared using the method in embodiment 1.Alkali lignin powder is placed in closed retort,
In the case where purity is 99.9% nitrogen protection, keep 20min to drain retort inner air in room temperature, then with 4 DEG C/min's
Heating rate is heated to 600 DEG C from room temperature and keeps the temperature 1h at such a temperature；After being carbonized after cooled to room temperature
Alkali lignin powder.
Alkali lignin powder after charing is heated to 900 DEG C from room temperature, whole process in the atmosphere of nitrogen, nitrogen
The use of flow velocity is 200mL/min, uses vapor flow to activate alkali lignin base charcoal 60min for 5g/min, obtain alkali lignin
Matrix activated carbon.The liquor zinci chloridi of alkali lignin matrix activated carbon obtained and a concentration of 35% is pressed 1:2 ratio mixing, uses
Magnetic stirrer 2h after being dried in electric drying oven with forced convection, then the raw material after drying is placed in activation furnace, in purity
Under 99.9% nitrogen protection, to keep 20min to be heated to 800 DEG C to drain retort inner air, then from room temperature in room temperature
And 1h is kept the temperature at such a temperature；The alkali lignin powder after chemical activation is obtained after cooled to room temperature；Using 1mol/
The hydrochloric acid of L washs it, reuses tap water and its pH value is washed till neutrality, and finally drying obtains alkali lignin base activity
Charcoal.
The Autosorb-1 nitrogen adsorption instrument provided using Quantachrome instrument companies, obtained nitrogen adsorption desorption
Curve graph is shown in Fig. 2, use multiple spot BET method survey the specific surface area for the alkali lignin matrix activated carbon that institute the present embodiment obtains for
1147m2/ g measures total pore volume using the corresponding nitrogen capacity of nitrogen adsorption curve relative pressure peak and has reached 0.693mL/
G uses the mesopore volume rate that BJH methods measure for 61.2%.
Embodiment 3
Alkali lignin powder is prepared using the method in embodiment 1.By alkali lignin powder and a concentration of 40% chlorination
Zinc solution presses 1:5 ratio mixing, using magnetic stirrer 2h, after being dried in electric drying oven with forced convection, then will drying
Raw material afterwards is placed in activation furnace, in the case where purity is 99.9% nitrogen protection, keeps 20min to drain in retort in room temperature
Portion's air, then 900 DEG C are heated to from room temperature, for whole process in the atmosphere of nitrogen, nitrogen is 200mL/min using flow velocity,
Vapor flow is used to activate alkali lignin base charcoal 60min for 5g/min, after cooled to room temperature, using 1mol/L's
Hydrochloric acid washs it, reuses tap water and its pH value is washed till neutrality, and finally drying obtains alkali lignin matrix activated carbon.
The Autosorb-1 nitrogen adsorption instrument provided using Quantachrome instrument companies, obtained nitrogen adsorption desorption
Curve graph is shown in Fig. 3, use multiple spot BET method survey the specific surface area for the alkali lignin matrix activated carbon that institute the present embodiment obtains for
1481m2/ g measures total pore volume using the corresponding nitrogen capacity of nitrogen adsorption curve relative pressure peak and has reached 1.187mL/
G uses the mesopore volume rate that BJH methods measure for 73.3%.
Embodiment 4：
Alkali lignin powder is prepared using the method in embodiment 1.Alkali lignin powder is placed in closed retort,
In the case where purity is 99.9% nitrogen protection, keep 20min to drain retort inner air in room temperature, then with 6 DEG C/min's
Heating rate is heated to 600 DEG C from room temperature and keeps the temperature 1h at such a temperature；After being carbonized after cooled to room temperature
Alkali lignin powder.
By after charing alkali lignin powder with a concentration of 25% liquor zinci chloridi press 1:4 ratio mixing, using magnetic
Power blender stirs 2h, after being dried in electric drying oven with forced convection, then the raw material after drying is placed in activation furnace, is in purity
Under 99.9% nitrogen protection, 20min is kept to be heated to 900 DEG C simultaneously to drain retort inner air, then from room temperature in room temperature
1h is kept the temperature at such a temperature；The alkali lignin powder after chemical activation is obtained after cooled to room temperature；Using 1mol/L
Hydrochloric acid it is washed, reuse tap water and its pH value be washed till neutrality, finally drying obtain alkali lignin matrix activated carbon.
Alkali lignin matrix activated carbon obtained is heated to 900 DEG C from room temperature, whole process is in the atmosphere of nitrogen, nitrogen
Using flow velocity be 200mL/min, use vapor flow be 4g/min activation alkali lignin base charcoal 60min, it is wooden to obtain alkali
Plain matrix activated carbon.
The Autosorb-1 nitrogen adsorption instrument provided using Quantachrome instrument companies, obtained nitrogen adsorption desorption
Curve graph is shown in Fig. 4, use multiple spot BET method survey the specific surface area for the alkali lignin matrix activated carbon that institute the present embodiment obtains for
1057m2/ g measures total pore volume using the corresponding nitrogen capacity of nitrogen adsorption curve relative pressure peak and has reached 0.614mL/
G uses the mesopore volume rate that BJH methods measure for 56.1%.
Embodiment 5
In the present embodiment, the temperature of steam activation is 800 DEG C, and vapor flow is that 5g/min activates alkali lignin base charcoal
90min obtains alkali lignin matrix activated carbon.Other operations are the same as embodiment 1.
The specific surface area that the alkali lignin matrix activated carbon that institute's the present embodiment obtains is surveyed with multiple spot BET method is 1252m2/ g, is adopted
Total pore volume is measured with the corresponding nitrogen capacity of nitrogen adsorption curve relative pressure peak and has reached 0.792mL/g, using BJH methods
The mesopore volume rate measured is 68.6%.
Embodiment 6
In the present embodiment, the conjunction a concentration of 40% mixed with zinc chloride when zinc chloride activation, mixing ratio 1:2.Other operations
With embodiment 1.
The specific surface area that the alkali lignin matrix activated carbon that institute's the present embodiment obtains is surveyed with multiple spot BET method is 922m2/ g is used
The corresponding nitrogen capacity of nitrogen adsorption curve relative pressure peak measures total pore volume and has reached 0.813mL/g, is surveyed using BJH methods
The mesopore volume rate obtained is 59.6%.
Comparative example 1
Alkali lignin powder is prepared using the method in embodiment 1.Alkali lignin powder is heated to 900 DEG C from room temperature,
For whole process in the atmosphere of nitrogen, nitrogen is 200mL/min using flow velocity, and vapor flow is used to activate alkali for 5g/min
Lignin-base charcoal 60min, obtains alkali lignin matrix activated carbon.
The Autosorb-1 nitrogen adsorption instrument provided using Quantachrome instrument companies, obtained nitrogen adsorption desorption
Curve graph is shown in Fig. 5, and multiple spot BET method is used to survey the specific surface area for the alkali lignin matrix activated carbon that institute's the present embodiment obtains as 730m2/
G measures total pore volume using the corresponding nitrogen capacity of nitrogen adsorption curve relative pressure peak and has reached 0.590mL/g, uses
The mesopore volume rate that BJH methods measure is 41.8%.
It is compared to embodiment 1,2,3 and 4, only carries out the specific surface of the alkali lignin matrix activated carbon of steam-activation treatment
Product, total pore volume and mesoporous will be much smaller than re-activation treated alkali lignin matrix activated carbon.
Above embodiment be only to the present invention specific implementation mode be described, not to the scope of the present invention into
Row limits, and those skilled in the art can also do numerous modifications and variations, be set not departing from the present invention on the basis of existing technology
Under the premise of meter spirit, all variations and modifications that this field ordinary engineering and technical personnel makes technical scheme of the present invention,
It should all fall into the protection domain of claims of the present invention determination.
Claims (7)
1. a kind of preparation method of more mesoporous Lignin-Based Activated Carbons, which is characterized in that including step：
(1) black liquor powder is mixed with water, is filtered using filter paper after stirring evenly, remove the insoluble matter in black liquor；Take filtrate by
Secondary addition hydrochloric acid, and centrifuge and precipitated using low speed centrifuge, then toward addition suitable quantity of water in precipitation and stir evenly, again from
The heart detaches, and final gained pellet frozen is dried, alkali lignin powder is finally obtained；
(2) under the conditions of gas shield, alkali lignin powder is heated to 600 DEG C~900 DEG C from room temperature, after being kept for 1~2 hour
Stop heating, alkali lignin base charcoal is made in natural cooling；
(3) it under the conditions of gas shield, uses vapor and zinc chloride for activator, is activated at being 500 DEG C~900 DEG C in temperature
Alkali lignin base charcoal, obtains alkali lignin matrix activated carbon；
Gas in step (2) and step (3) for protecting is one or more in nitrogen, argon gas, helium；In step (3)
The sequence of steam activation and zinc chloride activation used by activation process is different.
2. preparation method according to claim 1, which is characterized in that step (1) the alkali lignin powder is from slurrying
The lignin isolated in papermaking wastewater, it is dry and levigate to grain size 0.5mm or less.
3. preparation method according to claim 2, which is characterized in that the method for separating lignin from pulping and paper-making waste liquid
For：Pulping and paper-making waste liquid is adjusted to the solution of solid content 10~18%, hydrochloric acid is added extremely in the insoluble matter in filtering removal solution
The pH value of solution is 2.0~3.0, is separated by solid-liquid separation, and takes precipitation dry and levigate.
4. preparation method according to claim 1, which is characterized in that in the step (2), 600 DEG C are heated to from room temperature
~900 DEG C of heating rate is 4~10 DEG C/min.
5. according to Claims 1 to 4 any one of them preparation method, which is characterized in that in the step (3), as activation
The water vapour of agent and the gas mixing for protection, the flow velocity of the gas for protection is 200mL/min, and the flow of vapor is
4g/min-5g/min；Between a concentration of 15%-45% of zinc chloride as activator, ratio when being mixed with raw material is 1:
1-1:Between 5.
6. according to Claims 1 to 4 any one of them preparation method, which is characterized in that in the step (3), in activation
Have after first steam activation after zinc chloride activation, or first zinc chloride activation again that steam activation or vapor are lived with zinc chloride again
Change is carried out at the same time.
7. the alkali lignin matrix activated carbon that any preparation method of claim 1~6 is prepared.
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| CN110142026A (en) * | 2019-05-27 | 2019-08-20 | 湖南农业大学 | The alkali lignin base charcoal efficient absorption material of cadmium, preparation method and applications in adsorbed water body |
| CN110577217A (en) * | 2019-10-16 | 2019-12-17 | 中国矿业大学 | Honeycomb porous carbon, preparation method thereof and electrode plate of supercapacitor |
| CN111285367A (en) * | 2018-12-06 | 2020-06-16 | 香港理工大学 | Porous carbon anode based on alkali lignin and ionic capacitor adopting same |
| CN111760549A (en) * | 2020-06-10 | 2020-10-13 | 昆明理工大学 | Method for preparing porous carbon-based adsorbent from papermaking black liquor |
| CN113816374A (en) * | 2021-09-29 | 2021-12-21 | 海南金海浆纸业有限公司 | Method for preparing high-adsorption-performance activated carbon by using pulping black liquor |
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| CN110577217A (en) * | 2019-10-16 | 2019-12-17 | 中国矿业大学 | Honeycomb porous carbon, preparation method thereof and electrode plate of supercapacitor |
| CN111760549A (en) * | 2020-06-10 | 2020-10-13 | 昆明理工大学 | Method for preparing porous carbon-based adsorbent from papermaking black liquor |
| CN113816374A (en) * | 2021-09-29 | 2021-12-21 | 海南金海浆纸业有限公司 | Method for preparing high-adsorption-performance activated carbon by using pulping black liquor |
| CN115445588A (en) * | 2022-08-15 | 2022-12-09 | 东南大学 | Biomass-based porous carbon composite material, preparation method thereof and application thereof in CO 2 Application in adsorption |
| CN115445588B (en) * | 2022-08-15 | 2023-10-17 | 东南大学 | Biomass-based porous carbon composite material, preparation and CO production 2 Application in adsorption |
| CN115594163A (en) * | 2022-09-22 | 2023-01-13 | 青岛农业大学（Cn） | Columnar lignin-based capsule foam carbon and preparation method and application thereof |
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