CN109019590A - Lignin-base multi-stage porous carbon material and preparation method thereof - Google Patents
Lignin-base multi-stage porous carbon material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of lignin-base multi-stage porous carbon materials and preparation method thereof, the preparation method includes: lignin pretreatment, eutectic solvent is prepared, the eutectic solvent heat of lignin is carbonized, the preparation of solvent heat carbonized product, the activation of solvent heat carbonized product and the preparation of lignin-base multi-stage porous carbon material.The present invention selects eutectic solvent dissolved lignin raw material, and preparation is simple, green non-poisonous.Lignin-base multi-stage porous carbon material of the invention has foramen magnum-mesoporous-microcellular structure abundant, and is evenly distributed rationally, has good absorption property.It can be used for the fields such as electrode material for super capacitor, lithium ion battery negative material, adsorbent material.
Description
Technical field
The invention belongs to carbon material fields, and in particular to a kind of lignin-base multi-stage porous carbon material and preparation method thereof.
Background technique
Active carbon has flourishing porous structure, and internal specific surface area can reach 500 to 3000m2/ g, high temperature stable
And chemical stabilization, and abundance, the above property make it be widely used in the fields such as absorption, catalysis, energy storage.The hole of porous material
Gap structure can be divided into according to its size: macropore (>50nm), mesoporous or mesoporous (2-50nm) and micropore (<2nm), in general living
For the pore structure of property charcoal based on macropore and micropore, meso-hole structure is less.But in the numerous areas such as energy storage, absorption, filtering,
The meso-hole structure of multi-stage porous carbon material plays a crucial role, thus prepare foramen magnum-mesoporous-micropore be reasonably distributed it is more
Grade hole carbon material has great significance.
Lignin phosphorus content is high, and oxygen content is low, there is a large amount of benzene ring structure, is highly suitable as the raw material of carbon material.
And the application requires lignin type, structural integrity lower, is that lignin realizes high-valued, industrial applications have
Imitate one of path.Using the porous carbon materials that lignin is prepared as raw material, following a few classes are broadly divided into according to its method.
(1) Lignin-Based Activated Carbon, method are broadly divided into physically activated and chemical activation.Physically activated finger is in hot environment
Under activated using vapor or carbon dioxide as activator；Chemical activation refers to the activators such as alkali, phosphoric acid, alkali metal salt and wood
Quality mixing is activated at high temperature.Lignin-Based Activated Carbon pore structure is mainly based on micropore and macropore, it is extremely difficult to obtain
Mesoporous carbon material abundant.
(2) lignin-base template carbon, method are broadly divided into hard template method and soft template method.Hard template includes nanometer silica gel
Grain, zeolite etc. pass through confinement carbon if Chinese patent CN201610362526 discloses one kind using monodisperse silica as template
Change, etching template and KOH in-situ activation prepare three-dimensional continuous multi-stage hole carbon material.Soft template includes surfactant, colloid
Polymer etc..In such method, hard mold version method, which needs to etch using strong acid (such as hydrofluoric acid), goes removing template, higher cost and danger
Dangerous, the soft template in soft template method not can be recycled, higher cost.
(3) lignin-base carbon fiber, such material preparation method are first prepared using the methods of melt spinning, electrostatic spinning
Porous carbon fiber is being prepared in conjunction with activation by heat treatment in lignin fibre, such method is complex.
(4) hydrothermal carbonization, lignin are mixed with water, are tentatively carbonized under high-temperature and high-pressure conditions, by subsequent activation
The carbon material of pore structure prosperity can be made afterwards.The advantages of hydrothermal carbonization technology is adjustment aperture to be distributed to a certain extent, molten
Agent is environmentally protective, and carbon yield is high.But its disadvantage is mainly that system vapour pressure is high, needs special installation and product grain larger,
Meso-hole structure is few.Ionic liquid at room temperature is a kind of substance for being in a liquid state at a temperature of room temperature or near room temperature, being made of ion,
There is the features such as vapour pressure is small, dissolubility is good, it is made to be widely used to every field.Occurs ion heat carbonization skill in recent years
Art, i.e., the solvent heat carbonization technology for replacing water to carry out under the conditions of class hydrothermal carbonization with ionic liquid at room temperature.It is steamed needed for this method
Vapour pressure is low, and biomass material solubility in suitable ion liquid system is high, and obtained carbon material has meso-hole structure abundant.
But its shortcoming is that ionic liquid prepares complex, at high price, ionic liquid removes difficulty from product.
Eutectic solvent (DES) be it is a kind of be cross-linked with each other by hydrogen bond action the liquid formed by two kinds of chemical components,
Fusing point is lower than any one constituent, is only made of ion, is often considered as a kind of novel ion liquid.Compared to ionic liquid
Body, DES have some exclusive advantages, such as Atom economy is more preferable, good biocompatibility, toxicity are low；Most of all,
DES preparation is simple, low in cost, and large-scale use feasibility is high.This technical field is still in blank at present.
Summary of the invention
It is an object of the invention to use the solvent heat carbonization technology based on eutectic solvent, knot using lignin as raw material
It closes subsequent high temperature activation and produces the multi-stage porous carbon material that foramen magnum-mesoporous-micropore is reasonably distributed.It can be used for electrode of super capacitor
The fields such as material, lithium ion battery negative material, adsorbent material.
The object of the invention to solve the technical problems adopts the following technical solutions to realize:
A kind of lignin-base multi-stage porous carbon material proposed according to the present invention and preparation method thereof, comprising the following steps:
Lignin pretreatment: raw material wood element is air-dried, crushing is placed in baking oven, carries out the first drying, cold after dry
But to room temperature, lignin sample is obtained, it is spare；
Eutectic solvent is prepared: anhydrous choline chloride and formic acid uniformly being mixed, the first reaction is carried out, obtains clear
Liquid is placed in airtight oven, carries out the second drying, removes excessive moisture, and sealing obtains eutectic solvent after being cooled to room temperature,
It is spare；
The eutectic solvent heat of lignin is carbonized: eutectic solvent uniformly being mixed with lignin sample, is placed in closed baking
In case, the second reaction is carried out, the first product is obtained；
The preparation of solvent heat carbonized product: under stirring, the instillation of the first product is heated to going for third reaction temperature
In ionized water, third reaction is carried out.Mixed liquor is centrifuged, is washed, cryogenic vacuum freeze-drying obtains the second product；
The activation of solvent heat carbonized product: the second product uniformly being mixed with potassium hydroxide, a small amount of deionized water dissolving is added,
It is dry that mixture is subjected to third.Mixture is carried out in tube furnace to the first activation under nitrogen atmosphere after drying, obtains the
Three products；
The preparation of lignin-base multi-stage porous carbon material: after third product salt acid soak, sufficiently washing to neutrality, after filtering
The 4th drying is carried out in airtight oven, obtains lignin-base multi-stage porous carbon material.
The object of the invention to solve the technical problems also can be used following technical measures and further realize:
Preferably, preparation method above-mentioned, wherein the molar ratio of the anhydrous choline chloride and formic acid is 1:1-5, it is described
The solid-to-liquid ratio that lignin is mixed with eutectic solvent is 1:1-15, and the volume ratio of first product and deionized water is 1:10-
50, the mass ratio of second product and potassium hydroxide is 1:1-4, and the hydrochloric acid is that the hydrochloric acid of mass concentration 10%-20% is molten
Liquid.
Preferably, preparation method above-mentioned, wherein the described first dry drying condition are as follows: 80-100 DEG C of temperature, the time
1-3h；Described second dry drying condition are as follows: 60-80 DEG C of temperature, time 4-6h；The dry drying condition of the third are as follows:
100-120 DEG C of temperature；Described 4th dry drying condition are as follows: 80-110 DEG C of temperature.
Preferably, preparation method above-mentioned, wherein the reaction condition of first reaction are as follows: 50-80 DEG C of temperature, the time
1h；The reaction condition of second reaction are as follows: 160-190 DEG C of temperature, time 3-24h；The reaction condition of the third reaction are as follows:
60-90 DEG C of temperature；The third reaction temperature is 60-90 DEG C；The activation condition of first activation are as follows: temperature 700-1000
DEG C, time 1-4h.
Preferably, preparation method above-mentioned, wherein the lignin is alkali lignin, lignosulfonates, sulfate
At least one of lignin, prehydrolysis lignin, organic solvent lignin.
Also the following technical solution is employed for the object of the invention to solve the technical problems to realize.
A kind of lignin-base multi-stage porous carbon material proposed according to the present invention and preparation method thereof, the lignin-base is more
Grade hole carbon material is prepared by method described in any of the above embodiments.
By above-mentioned technical proposal, lignin-base multi-stage porous carbon material of the invention is at least had the advantage that
(1) solvent of the ionic liquid as solvent-thermal method being replaced using eutectic solvent (DES) system, preparation is easy, at
This is cheap.After solvent heat carbonization, DES is easy removing.
(2) it is rich by the solvent heat carbonization method based on eutectic system to be prepared for foramen magnum-mesoporous-microcellular structure by the present invention
Rich multi-stage porous carbon material, increases the specific surface area and mesoporous volume of carbon material.It can be used for supercapacitor, lithium-ion electric
The fields such as pond, absorption.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to a kind of lignin-base multi-stage porous carbon material proposed according to the present invention and preparation method thereof its specific embodiment party
Formula, feature and its effect, detailed description is as follows.In the following description, different " embodiment " or " embodiment " refers to different
It surely is the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any suitable form groups
It closes.
The embodiment of the present invention proposes a kind of lignin-base multi-stage porous carbon material and preparation method thereof.
The preparation method the following steps are included:
Lignin pretreatment: raw material wood element is air-dried, crushing is placed in baking oven, the dry 1-3h at 80-100 DEG C,
It is cooled to room temperature after drying, obtains lignin sample, it is spare；
Eutectic solvent is prepared: anhydrous choline chloride and formic acid uniformly being mixed with molar ratio 1:1-5, at 50-80 DEG C
1h is stirred, clear liquid is obtained, is placed in airtight oven, the dry 4-6h at 60-80 DEG C removes excessive moisture, sealing
Eutectic solvent is obtained after being cooled to room temperature, it is spare；
The eutectic solvent heat of lignin is carbonized: eutectic solvent uniformly being mixed with lignin sample, is placed in closed baking
In case, 3-24h is reacted at 60-190 DEG C, obtains heat carbonization mixed liquor；
The preparation of solvent heat carbonized product: under stirring, heat carbonization mixed liquor is added dropwise in 60-90 DEG C of deionized water
The volume ratio of reaction, heat carbonization mixed liquor and deionized water is 1:10-50.Mixed liquor is centrifuged, is washed, cryogenic vacuum freezing is dry
It is dry, obtain solvent heat carbonized product；
The activation of solvent heat carbonized product: solvent heat carbonized product is uniformly mixed with potassium hydroxide with mass ratio 1:1-4, is added
Enter a small amount of deionized water dissolving, mixture is dried at 100-120 DEG C.By mixture under nitrogen atmosphere in tubular type after drying
It is activated in furnace, activation temperature is 700-1000 DEG C, keeps the temperature 1-4h, obtains activation products；
The preparation of lignin-base multi-stage porous carbon material: the activation products hydrochloric acid solution of mass concentration 10%-20% is impregnated
Afterwards, activation products to be taken out, are sufficiently washed with deionized water to neutrality, filtering is placed in airtight oven, it is dried at 80-110 DEG C,
Obtain lignin-base multi-stage porous carbon material.
In the present embodiment, lignin includes but is not limited to: alkali lignin, lignosulfonates, sulfate-reducing conditions, pre- water
Solve at least one of lignin, organic solvent lignin.
With specific embodiment, the present invention will be further described below, but not as the limitation of the invention.
Embodiment 1
(1) prehydrolysis lignin is placed in 90 DEG C of baking ovens dry 2h, taking-up is cooled to room temperature, spare.
(2) it is weighed respectively with molar ratio for the ratio of 1:2 in anhydrous choline chloride and formic acid, in 80 DEG C of stirred in water bath 1h
With mixing, clear liquid is obtained, 6h is placed in 80 DEG C of airtight oven, removes excessive moisture, is taken out, sealing is cooled to
Eutectic solvent is obtained after room temperature.
(3) it weighs 0.5g prehydrolysis lignin to be placed in polytetrafluoroethyllining lining container, 5g eutectic solvent is added, to pre-
It after hydrolytic lignin is completely dissolved, is placed in closed container, 6h is reacted in 160 DEG C of baking oven, taking-up is cooled to room temperature opening.
(4) under stirring, the mixed solution that generation is reacted in closed container is instilled in 80 DEG C of deionized water, with
The revolving speed of 8000rpm is centrifuged 5min, is washed with deionized twice, solvent heat carbonized product is obtained after freeze-drying.
(5) in mass ratio it is that 1:3 is weighed respectively with potassium hydroxide by solvent heat carbonized product, the two is mixed, is added few
Deionized water is measured, is placed in 105 DEG C of baking oven and dries, mixture is transferred in crucible, in the tube furnace for having nitrogen atmosphere
900 DEG C are heated to, heat preservation 2h is activated.
(6) activation products are impregnated using 10% hydrochloric acid solution, takes out activation products, is cleaned using deionized water
To neutrality, filtering is placed in airtight oven, is dried at 80 DEG C to get lignin-base multi-stage porous carbon material is arrived.
Surface sweeping Electronic Speculum, nitrogen adsorption test are carried out to preparation-obtained lignin-base multi-stage porous carbon material.As a result it is listed in
Attached drawing.
Table 1 be according to nitrogen adsorption test data, it is more after calculating solvent heat carbonized product obtained and activation
Grade hole carbon material pore structure data.
1 embodiment of table, 1 multi-stage porous carbon material pore structure data
Embodiment 2
(1) sulfate-reducing conditions are placed in 90 DEG C of baking ovens dry 2h, taking-up is cooled to room temperature, spare.
(2) it is weighed respectively with molar ratio for the ratio of 1:3 in anhydrous choline chloride and formic acid, in 80 DEG C of stirred in water bath 1h
With mixing, clear liquid is obtained, 1h is placed in 80 DEG C of airtight oven, removes excessive moisture, is taken out, sealing is cooled to
Eutectic solvent is obtained after room temperature.
(3) 1g sulfate-reducing conditions are weighed to be placed in polytetrafluoroethyllining lining container, 5g eutectic solvent is added, to pre- water
It after solution lignin is completely dissolved, is placed in closed container, 12h is reacted in 175 DEG C of baking oven, taking-up is cooled to room temperature opening.
(4) under stirring, the mixed solution that generation is reacted in closed container is instilled in 70 DEG C of deionized water, with
The revolving speed of 8000rpm is centrifuged 5min, is washed with deionized twice, solvent heat carbonized product is obtained after freeze-drying.
(5) in mass ratio it is that 1:4 is weighed respectively with potassium hydroxide by solvent heat carbonized product, the two is mixed, is added few
Deionized water is measured, is placed in 105 DEG C of baking oven and dries, mixture is transferred in crucible, in the tube furnace for having nitrogen atmosphere
700 DEG C are heated to, heat preservation 4h is activated.
(6) activation products are impregnated using 20% hydrochloric acid solution, takes out activation products, is cleaned using deionized water
To neutrality, filtering is placed in airtight oven, is dried at 80 DEG C to get lignin-base multi-stage porous carbon material is arrived.
To preparation-obtained lignin-base multi-stage porous carbon material, inhaled using surface sweeping Electronic Speculum same as Example 1, nitrogen
Attached test, it is as a result substantially the same manner as Example 1.
Embodiment 3
(1) alkali lignin is placed in 100 DEG C of baking ovens dry 3h, taking-up is cooled to room temperature, spare.
(2) it is weighed respectively with molar ratio for the ratio of 1:5 in anhydrous choline chloride and formic acid, in 80 DEG C of stirred in water bath 1h
With mixing, clear liquid is obtained, 1h is placed in 60 DEG C of airtight oven, removes excessive moisture, is taken out, sealing is cooled to
Eutectic solvent is obtained after room temperature.
(3) it weighs 1g alkali lignin to be placed in polytetrafluoroethyllining lining container, 15g eutectic solvent is added, to prehydrolysis
It after lignin is completely dissolved, is placed in closed container, is reacted in 190 DEG C of baking oven for 24 hours, taking-up is cooled to room temperature opening.
(4) under stirring, the mixed solution that generation is reacted in closed container is instilled in 60 DEG C of deionized water, with
The revolving speed of 8000rpm is centrifuged 5min, is washed with deionized three times, solvent heat carbonized product is obtained after freeze-drying.
(5) in mass ratio it is that 1:2 is weighed respectively with potassium hydroxide by solvent heat carbonized product, the two is mixed, is added few
Deionized water is measured, is placed in 105 DEG C of baking oven and dries, mixture is transferred in crucible, in the tube furnace for having nitrogen atmosphere
1000 DEG C are heated to, heat preservation 1h is activated.
(6) activation products are impregnated using 10% hydrochloric acid solution, takes out activation products, is cleaned using deionized water
To neutrality, filtering is placed in airtight oven, is dried at 80 DEG C to get lignin-base multi-stage porous carbon material is arrived.
To preparation-obtained lignin-base multi-stage porous carbon material, inhaled using surface sweeping Electronic Speculum same as Example 1, nitrogen
Attached test, it is as a result substantially the same manner as Example 1.
Detailed description of the invention
Fig. 1 is the SEM figure of solvent heat carbonized product and the multi-stage porous carbon material after activation in embodiment 1, wherein (a), (b)
Be solvent heat carbonized product SEM figure, (c), (d) be activation after multi-stage porous carbon material SEM figure.
Fig. 2 is the nitrogen adsorption isotherm figure of solvent heat carbonized product and the multi-stage porous carbon material after activation in embodiment 1.
Fig. 3 is the graph of pore diameter distribution of the multi-stage porous carbon material after activating in embodiment 1.
Fig. 1 is the SEM figure of solvent heat carbonized product and the multi-stage porous carbon material after activation in embodiment 1, wherein (a), (b)
It is the SEM figure of solvent heat carbonized product, shows that solvent heat carbonized product granular size is 70-120nm, is (d) after activation (c)
Multi-stage porous carbon material SEM figure, show that multi-stage porous carbon is formed with nano-scale carbon microballoon, granular size is about 10-30nm.
Fig. 2 is the nitrogen adsorption isotherm figure of solvent heat carbonized product and the multi-stage porous carbon material after activation in embodiment 1,
The nitrogen adsorption isotherm of solvent heat carbonized product shows that its pore structure is less, greatly increases through overactivation metapore gap structure,
Risen rapidly in low-pressure area curve and illustrate that material has micropore, and in curve the appearance of winding illustrate to have in material mutually together with
Meso-hole structure.
Fig. 3 is the graph of pore diameter distribution of the multi-stage porous carbon material after activating in embodiment 1, shows that multi-stage porous carbon material has greatly
Measure mesoporous material.
Claims (5)
1. a kind of lignin-base multi-stage porous carbon material and preparation method thereof, which comprises the following steps:
Lignin pretreatment: raw material wood element is air-dried, crushing is placed in baking oven, is carried out the first drying, is cooled to after dry
Room temperature obtains lignin sample, spare；
Eutectic solvent is prepared: anhydrous choline chloride and formic acid uniformly being mixed, the first reaction is carried out, obtains clear liquid
Body is placed in airtight oven, carries out the second drying, removes excessive moisture, sealing obtains eutectic solvent after being cooled to room temperature, standby
With；
The eutectic solvent heat of lignin is carbonized: eutectic solvent uniformly mixed with lignin sample, is placed in airtight oven,
The second reaction is carried out, the first product is obtained；
The preparation of solvent heat carbonized product: under stirring, the first product is instilled to the deionization for being heated to third reaction temperature
In water, third reaction is carried out；Mixed liquor is centrifuged, is washed, cryogenic vacuum freeze-drying obtains the second product；
The activation of solvent heat carbonized product: the second product is uniformly mixed with potassium hydroxide, a small amount of deionized water dissolving is added, will mix
It closes object and carries out third drying；Mixture is carried out in tube furnace to the first activation under nitrogen atmosphere after drying, obtains third production
Object；
The preparation of lignin-base multi-stage porous carbon material: after third product salt acid soak, sufficiently washing is to neutrality, close after filtering
It closes in baking oven and carries out the 4th drying, obtain lignin-base multi-stage porous carbon material.
2. preparation method according to claim 1, which is characterized in that
The molar ratio of the anhydrous choline chloride and formic acid is 1:1-5,
The solid-to-liquid ratio that the lignin is mixed with eutectic solvent is 1:1-15,
The volume ratio of first product and deionized water is 1:10-50,
The mass ratio of second product and potassium hydroxide is 1:1-4,
The hydrochloric acid is the hydrochloric acid solution of mass concentration 10%-20%.
3. preparation method according to claim 1, which is characterized in that
Described first dry drying condition are as follows: 80-100 DEG C of temperature, time 1-3h；
Described second dry drying condition are as follows: 60-80 DEG C of temperature, time 4-6h；
The dry drying condition of the third are as follows: 100-120 DEG C of temperature；
Described 4th dry drying condition are as follows: 80-110 DEG C of temperature.
4. preparation method according to claim 1, which is characterized in that
The reaction condition of first reaction are as follows: 50-80 DEG C of temperature, time 1h；
The reaction condition of second reaction are as follows: 160-190 DEG C of temperature, time 3-24h；
The reaction condition of the third reaction are as follows: 60-90 DEG C of temperature；
The third reaction temperature is 60-90 DEG C；
The activation condition of first activation are as follows: 700-1000 DEG C of temperature, time 1-4h.
5. preparation method according to claim 1, which is characterized in that
The lignin is alkali lignin, lignosulfonates, sulfate-reducing conditions, prehydrolysis lignin, organic solvent wood
At least one of quality.
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