CN107010622B - The modified microwave of medium barrier plasma activates lignin-base carbon resistance rod preparation method - Google Patents
The modified microwave of medium barrier plasma activates lignin-base carbon resistance rod preparation method Download PDFInfo
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Abstract
The present invention is the modified microwave activation lignin-base carbon resistance rod preparation method of medium barrier plasma, belongs to biological material field.Its technique is to be purified using alkaline aqueous solution extraction to industrial lignin, Lignin-Based Activated Carbon is obtained after microwave-assisted activation again, it mixes, roll with ptfe emulsion and acetylene black, drying after being modified with medium barrier plasma to it, being compressed in nickel foam and carbon resistance rod is made.After medium barrier plasma is handled, the specific surface area of Lignin-Based Activated Carbon is set to improve 5~30% in 1~5 minute, micropore ratio increases to 80% or more, and oxygen element, nitrogen element content improve 2~5 times, with the carbon resistance rod specific capacitance of its preparation compared with raising 15~45% before corona treatment.
Description
Technical field
The present invention relates to the systems that a kind of medium barrier plasma is quickly modified microwave-assisted activation lignin-base carbon resistance rod
Preparation Method belongs to biological material field.
Background technique
Lignin is the unformed shape polymer that plant kingdom's content is only second to cellulose, is primarily present in plant cell wall
In.Lignin is distributed widely in higher plant, is chemical component specific to gymnosperm and angiosperm.It is estimated that every
Year whole world lignin reserves as made of plant growth are up to 150,000,000,000 tons, and wherein industrial lignin yield is up to 1.5~1.8 hundred million
Ton.Main component of the industrial lignin as pulping and paper-making industry waste liquid, is only utilized effectively less than 2%, and major part is all
It is discharged into rivers or burn-up, not only environment is caused seriously to pollute, but also waste of resource, making full use of industrial lignin, this is huge
Large resource has become one of hot spot of Recent study.Due to lignin not only charcoal yield with higher, cheap, source
It is abundant, and the porous activated carbon specific surface area of its preparation is high, and pore-size distribution is suitable for, it is considered to be before the ideal for preparing active carbon
Body is driven, is widely used in capacitor electrode material.But traditional charing and activating process need by complicated heating,
Heat preservation, cooling step, cause the production cycle too long (3~5 hours), production efficiency is low, and industrialization promotion is greatly limited
System.However, microwave-assisted activation can (10~30 minutes) prepare high-specific surface area within a short period of time active carbon, compare
In traditional heating activating process, microwave-assisted activating process greatly shortens activation time.
Currently, active carbon is one kind that is earliest in the supercapacitor for making electrode with carbon-based material and most being applied extensively
Material.The aperture structure and chemically active surface functional group content of active carbon are the carbon resistance rod chemical properties for influencing its preparation
Key factor.The chemical property modification of active carbon is usually to carry out 2~4 hours in the aqueous solution for place it in target compound
Heat treatment (250~450 DEG C), modification will be by complicated heating, and the process of heat preservation and cooling, energy consumption is big, and time-consuming, leads
High production cost is caused, the production cycle is long, and production efficiency is low, and industrialization promotion is extremely limited.However, plasma is
It is a kind of by a large amount of electronics, the ion of either polarity, the high energy gaseous atom in the form of ground state or any excitation state and molecule and
The molecular gaseous state complex of light quantity, the energy of particle is about from several electron volts to several kiloelectron-volts, with these high energy activity
Particle acts on activated carbon surface, its original chemical bond can be made to be broken in several minutes, introduces specific objective chemistry official
It can roll into a ball, while using the corrasion of plasma, be formed on its surface a large amount of nanoscale holes, improving raw material of wood-charcoal blanking aperture knot
Structure increases substantially specific surface area.
Plasma can pass through glow discharge, corona discharge, dielectric barrier discharge, radio frequency discharge and microwave discharge etc.
Mode generates.Dielectric barrier discharge is a kind of nonequilibrium state gas discharge for having dielectric insertion discharge space.It is put at two
It is full of certain working gas between electrode, and wherein one or two electrode is covered with dielectric, it can also be by medium
Be hung directly from discharge space or using granular media filler wherein, when applying sufficiently high alternating voltage between two electrodes
When, interelectrode gas can be breakdown and generation is discharged, that is, produces dielectric barrier discharge plasma.Dielectric impedance plasma
Body can carry out the quick modification in surface to material under low pressure even normal pressure, and modification is at low cost, and treatment effeciency is high.
The present invention uses medium barrier plasma modification technology, quickly and efficiently enhances microwave-assisted activation lignin-base
The chemical property of carbon resistance rod, makes lignin turn waste into wealth, and increases substantially Lignin-Based Activated Carbon in carbon resistance rod preparation field
The market competitiveness, for promoting the industrial applications of China's Lignin-Based Activated Carbon to have important practical significance.
Summary of the invention
The purpose of the present invention is using medium barrier plasma (i.e. by electronics, either polarity ion, with ground state or appoint
The high energy gaseous atom and molecule and the molecular gaseous state complex of light quantity of what excitation state form) physics and chemical action,
A large amount of nanoscale holes are formed on microwave-assisted activation Lignin-Based Activated Carbon surface (in several minutes) in a very short period of time, substantially
Degree increases its specific surface area, and introduces target chemical functional group on surface, significantly improves its specific capacitance, it is excellent to obtain chemical property
Different lignin-base carbon resistance rod.
Technical solution of the invention: the modified microwave of medium barrier plasma activates lignin-base carbon resistance rod preparation side
Method is completed by the following steps:
One, Lignin pufification:
Industrial lignin is purified using alkaline aqueous solution extraction, removes impurity, to reduce to subsequent activation mistake
The influence of journey.
Lignin pufification specific steps described in step 1 are as follows: mix lignin with the NaOH solution that concentration is 3%, wood
Quality and the ratio of NaOH are 1: 10, after stirring 1 hour at 65 DEG C, keep the temperature 30min, hot mixing liquid is filtered by vacuum,
The dilution heat of sulfuric acid that concentration is 2% is slowly added in filtrate, it is lasting to stir, pH to 3 is adjusted, 30 points of the heat preservation agglutination at 70 DEG C
Clock, until observing that graininess lignin floats, stirring makes lignin sink, and staticly settles 12 hours, is poured out in beaker
Layer clear liquid, the graininess lignin of precipitating is centrifuged with remaining supernatant liquor, is cleaned with deionized water
Sediment is in neutrality up to pH, is then dried at 60 DEG C to constant weight, is obtained lignin after purification.
Two, microwave-assisted activation prepares Lignin-Based Activated Carbon；
Using KOH solution as activator, be directly placed into after being mixed by lignin with KOH mass ratio 1: 3 in microwave reactor into
Row is activated, and obtains Lignin-Based Activated Carbon.
Microwave-assisted activation described in step 2 prepares Lignin-Based Activated Carbon specific steps are as follows: will purify in proportion wooden
Element is added in the KOH solution that concentration is 53%, and mechanical stirring 30min is then directly placed into microwave reactor and carries out at activation
Reason, microwave frequency are 2450 ± 50MHz, processing power 700W, are kept for 15 minutes, protective gas is nitrogen, flow 40mL/
Min after the completion of activation, takes out after sample is cooled to room temperature under nitrogen atmosphere, is added in 1mol/L hydrochloric acid solution, wait react
It finishes, filters, be washed with distilled water to neutrality, be subsequently placed into drying box drying 4 hours at 103 DEG C, obtain microwave-assisted
Activate Lignin-Based Activated Carbon.
Three, medium barrier plasma modified lignin resin matrix activated carbon；
Microwave-assisted activation Lignin-Based Activated Carbon is quickly modified using medium barrier plasma processing equipment
Processing, it is living to lignin-base by high energy active particles such as electronics, ion, atom, molecule and photons in plasma
Property charcoal physical etchings effect, destroy the macropore of Lignin-Based Activated Carbon, and form a large amount of nanoscale holes, adjust active carbon
Aperture structure increases micropore ratio, meanwhile, cause chemical action using the free radical of plasma, in Lignin-Based Activated Carbon
Surface introduces targeted activity chemical functional group and significantly improves the ratio of Lignin-Based Activated Carbon such as oxygen-containing functional group, nitrogen-containing functional group
Capacitor, the modified this dual synergistic effect of medium barrier plasma, can make Lignin-Based Activated Carbon in a short time
Specific surface area is compared with improving 5~30% before corona treatment, for micropore ratio compared with increasing to 80% or more before corona treatment, oxygen is first
Element, nitrogen element content are compared with improving 2~5 times before corona treatment, with the carbon resistance rod specific capacitance of its preparation compared with corona treatment
It is preceding to improve 15~45%.
Medium barrier plasma modified lignin resin matrix activated carbon specific steps described in step 3 are as follows: will be obtained in step 2
To microwave-assisted activation Lignin-Based Activated Carbon be put into the reaction chamber of medium barrier plasma processing equipment, pass through water-bath
Heating water system reagent treatment obtains processing gas to 70~100 DEG C, and water system reagent treatment is one of water, ammonium hydroxide, is recycled
Vacuum pump will be evacuated to the pressure of 20~30kPa, water vapour or ammonia in reaction chamber and water vapor mixture body is automatically introduced into instead
It answers in chamber, then starts medium barrier plasma excitation power source, adjust processing power to 30~60W, make processing in reaction chamber
Gas discharge generates a large amount of oxygen or nitrogen plasma, is modified processing to Lignin-Based Activated Carbon surface, the processing time is 1
~5 minutes.
Four, medium barrier plasma is quickly modified microwave activation lignin-base carbon resistance rod preparation；
It is 60% that 5~10% concentration are added in the Lignin-Based Activated Carbon after medium barrier plasma modification
Ptfe emulsion and 5~10% acetylene black, be rolled on double roller tablet press machine after mixing thin with a thickness of 0.4mm
Piece is put into drying box, 4 hours dry at 103 DEG C, is compressed in nickel foam and carbon resistance rod is made.
Advantages of the present invention: (1) the modification time is short: the modification time is only 1~5 minute, compared at present most
Common heat treating process (the processing time is 2~4 hours), the processing time is greatly lowered, so that lignin-base carbon resistance rod is whole
A production cycle greatly shortens, and significantly improves production efficiency；(2) a kind of multiple synergistic effect of processing significantly improves lignin-base
The chemical property of carbon resistance rod: the high energy active particle pair such as electronics, ion, atom, molecule and photon in plasma
The bombardment of Lignin-Based Activated Carbon acts on, and makes Lignin-Based Activated Carbon macropore fall damage, while the corrasion of plasma makes
The generation of its surface is a large amount of nanometer level microporous, further improves the aperture structure of active carbon, increases micropore ratio, meanwhile, utilization
The free radical of plasma causes chemical action, and introducing on Lignin-Based Activated Carbon surface has humidification to chemical property
Targeted activity chemical functional group, such as oxygen-containing functional group and nitrogen-containing functional group, the physics and chemical synergistic for passing through plasma are made
With raising 15~45% before handling the specific capacitance of modified lignin-base carbon resistance rod relatively；(3) work is handled
Skill is simple, and controllability is strong, and pollution is few, consumes energy low: only need to adjust reaction cavity vacuum degree in treatment process, processing power and
Action time, operating process is simply controllable, without heating, consumes energy low, environmentally protective, and it is living to significantly reduce modified lignin resin base
The production cost of property charcoal, enhances one's market competitiveness.
Detailed description of the invention
Fig. 1 is the electrochemical property test map of carbon resistance rod made from embodiment 1,2,3 and comparative example 1.
Specific embodiment
Embodiment 1
(1) it purifies: industrial lignin being mixed with the NaOH solution that concentration is 3%, the ratio of lignin and NaOH are 1:
10, after being stirred 1 hour at 65 DEG C, 30min is kept the temperature, hot mixing liquid is filtered by vacuum, concentration is slowly added in filtrate
It is lasting to stir for 2% dilution heat of sulfuric acid, pH to 3 is adjusted, heat preservation agglutination 30 minutes at 70 DEG C, until observing graininess
Lignin floats, and stirring makes lignin sink, and staticly settles 12 hours, beaker clear liquid at the middle and upper levels is poured out, by the particle of precipitating
Shape lignin is centrifuged with remaining supernatant liquor, and the sediment cleaned with deionized water is in neutrality up to pH,
It then dries at 60 DEG C to constant weight, obtains lignin after purification.
(2) it activates: lignin will be purified and be added in the KOH solution that concentration is 53%, the mass ratio of lignin and KOH are 1:
3, it mechanical stirring 30 minutes, is then directly placed into microwave reactor and is activated, microwave frequency is 2450 ± 50MHz,
Processing power is 700W, is kept for 15 minutes, protective gas is nitrogen, flow 40mL/min, after the completion of activation, to sample in nitrogen
Atmosphere is taken out after being cooled to room temperature under enclosing, be added in 1mol hydrochloric acid solution, and to end of reaction, filtering is washed with distilled water to
Property, it is subsequently placed into drying box at 103 DEG C drying 4 hours, obtains microwave-assisted activation Lignin-Based Activated Carbon.
(3) medium barrier plasma is modified: Lignin-Based Activated Carbon is put into medium barrier plasma processing equipment
Reaction chamber in, water vapour and ammonia gas mixture body are obtained to 70 DEG C by heating water bath ammonium hydroxide, recycle vacuum pump that will react
The pressure of 30kPa is evacuated in chamber, water vapour and ammonia gas mixture body are automatically introduced into reaction chamber, subsequent start-up dielectric impedance etc.
Gas ions excitation power source adjusts processing power to 60W, makes gas discharge in sample room, generate a large amount of oxygen-containing and nitrogenous plasmas
Body is modified processing to Lignin-Based Activated Carbon surface, and the processing time is 5 minutes.
(4) carbon resistance rod prepare: by after medium barrier plasma modification Lignin-Based Activated Carbon be added 5~
10% concentration is the acetylene black of 60% ptfe emulsion and 5~10%, is rolled on double roller tablet press machine after mixing
With a thickness of 0.4mm thin slice, it is put into drying box, it is 4 hours dry at 103 DEG C, it is compressed in nickel foam and carbon resistance rod is made.Lignin
Specific surface area, oxygen element and the nitrogen element content of matrix activated carbon and with its preparation carbon resistance rod specific capacitance and charge and discharge 2000 times
Capacitance conservation rate afterwards is shown in Table 1.
Embodiment 2
Industrial lignin is purified according to the identical step of embodiment 1 (1), obtains purifying lignin.
Microwave-assisted activation processing is carried out to purifying lignin according to the identical step of embodiment 1 (2), obtains lignin-base
Active carbon.
Lignin-Based Activated Carbon is put into the reaction chamber of medium barrier plasma processing equipment, passes through heating water bath water
Water vapour is obtained to 100 DEG C, recycles vacuum pump that will be evacuated to the pressure of 30kPa in reaction chamber, water vapour is automatically introduced into reaction
In chamber, subsequent start-up medium barrier plasma excitation power source adjusts processing power to 60W, makes gas discharge in sample room, produce
Life is a large amount of oxygen-containing and contains nitrogen plasma, is modified processing to Lignin-Based Activated Carbon surface, the processing time is 5 minutes.
Modified Lignin-Based Activated Carbon is prepared into carbon resistance rod according to the identical step of embodiment 1 (4).
Specific surface area, oxygen element and the nitrogen element content of Lignin-Based Activated Carbon and the carbon resistance rod specific capacitance prepared with it
It is shown in Table 1 with the capacitance conservation rate after charge and discharge 2000 times.
Embodiment 3
Industrial lignin is purified according to the identical step of embodiment 1 (1), obtains purifying lignin.
Microwave-assisted activation processing is carried out to purifying lignin according to the identical step of embodiment 1 (2), obtains lignin-base
Active carbon.
Lignin-Based Activated Carbon is put into the reaction chamber of medium barrier plasma processing equipment, passes through heating water bath water
Water vapour is obtained to 100 DEG C, recycles vacuum pump that will be evacuated to the pressure of 20kPa in reaction chamber, water vapour is automatically introduced into reaction
In chamber, subsequent start-up medium barrier plasma excitation power source adjusts processing power to 30W, makes gas discharge in sample room, produce
Life is a large amount of oxygen-containing and contains nitrogen plasma, is modified processing to Lignin-Based Activated Carbon surface, the processing time is 1 minute.
Modified Lignin-Based Activated Carbon is prepared into carbon resistance rod according to the identical step of embodiment 1 (4).
Specific surface area, oxygen element and the nitrogen element content of Lignin-Based Activated Carbon and the carbon resistance rod specific capacitance prepared with it
It is shown in Table 1 with the capacitance conservation rate after charge and discharge 2000 times.
Comparative example:
Industrial lignin is purified according to the identical step of embodiment 1 (1), obtains purifying lignin.
Microwave-assisted activation processing is carried out to purifying lignin according to the identical step of embodiment 1 (2), obtains lignin-base
Active carbon.
Modified Lignin-Based Activated Carbon is prepared into carbon resistance rod according to the identical step of embodiment 1 (4).
Specific surface area, oxygen element and the nitrogen element content of Lignin-Based Activated Carbon and the carbon resistance rod specific capacitance prepared with it
It is shown in Table 1 with the capacitance conservation rate after charge and discharge 2000 times.
1 medium barrier plasma modified lignin resin matrix activated carbon of table and the carbon resistance rod properties prepared with it
Note:
1. specific surface area result is obtained by full-automatic specific surface area and pore analysis instrument (ASAP2020) test；
2. the content of surface oxygen element, nitrogen is obtained by x-ray photoelectron spectroscopy (AXIS Ultra DLD) test；
3. specific capacitance test result is obtained by the cyclic voltammetry method of electrochemical workstation (CHI660D), all tests
Sweep speed be 5mV/s, scanning voltage be -1.1V arrive -0.1V.
After 4. capacitance conservation rate refers to charge and discharge 2000 times, the conservation rate of condenser capacity.
Claims (5)
1. the modified microwave of medium barrier plasma activates lignin-base carbon resistance rod preparation method, it is characterised in that: Jie
The modified microwave activation lignin-base carbon resistance rod of matter barrier plasma is prepared according to the following steps:
Step 1: Lignin pufification: purifying industrial lignin using alkaline aqueous solution extraction, impurity is removed, to subtract
Few influence to subsequent activation process；
Step 2: microwave-assisted activation prepares Lignin-Based Activated Carbon；Using KOH solution as activator, by lignin and KOH mass
It is activated than being directly placed into microwave reactor after 1: 3 mixing, obtains Lignin-Based Activated Carbon；
Step 3: medium barrier plasma modified lignin resin matrix activated carbon；Using medium barrier plasma processing equipment pair
Microwave-assisted activation Lignin-Based Activated Carbon carries out quick modification, by electronics in plasma, ion, atom, point
Son and photon high-energy active particle act on the physical etchings of Lignin-Based Activated Carbon, destroy the big of Lignin-Based Activated Carbon
Hole, and a large amount of nanoscale holes are formed, the aperture structure of active carbon is adjusted, micropore ratio is increased, meanwhile, utilize plasma
Free radical causes chemical action, introduces targeted activity chemical functional group on Lignin-Based Activated Carbon surface, significantly improves lignin
The specific capacitance of matrix activated carbon, the modified this dual synergistic effect of medium barrier plasma, can make wooden in a short time
The specific surface area of plain matrix activated carbon is compared with improving 5~30% before corona treatment, micropore ratio before corona treatment compared with increasing to
80% or more, oxygen element, nitrogen element content compared with before corona treatment improve 2~5 times, with its preparation carbon resistance rod specific capacitance compared with
15~45% are improved before corona treatment；
Step 4: the modified microwave activation lignin-base carbon resistance rod preparation of medium barrier plasma；Through dielectric impedance plasma
It is 60% ptfe emulsion and 5~10% that 5~10% concentration are added in modifies treated Lignin-Based Activated Carbon
Acetylene black is rolled into a thickness of 0.4mm thin slice on double roller tablet press machine after mixing, is put into drying box, dry at 103 DEG C
It 4 hours, is compressed in nickel foam and carbon resistance rod is made.
2. the modified microwave of medium barrier plasma according to claim 1 activates lignin-base carbon resistance rod preparation method,
It is characterized by: Lignin pufification specific steps described in step 1 are as follows: mix the NaOH solution that lignin is 3% with concentration
It closes, the ratio of lignin and NaOH are 1: 10, after stirring 1 hour at 65 DEG C, keep the temperature 30min, carry out vacuum to hot mixing liquid
It filters, the dilution heat of sulfuric acid that concentration is 2% is slowly added in filtrate, it is lasting to stir, pH to 3 is adjusted, is kept the temperature at 70 DEG C solidifying
Collection 30 minutes, until observing that graininess lignin floats, stirring makes lignin sink, and staticly settles 12 hours, burning is poured out
Cup clear liquid at the middle and upper levels, the graininess lignin of precipitating is centrifuged with remaining supernatant liquor, is cleaned with deionized water
Obtained sediment is in neutrality up to pH, is then dried at 60 DEG C to constant weight, is obtained lignin after purification.
3. the modified microwave of medium barrier plasma according to claim 1 activates lignin-base carbon resistance rod preparation method,
It is characterized by: microwave-assisted activation described in step 2 prepares Lignin-Based Activated Carbon specific steps are as follows: in proportion will purifying
Lignin is added in the KOH solution that concentration is 53%, and mechanical stirring 30min is then directly placed into microwave reactor and lives
Change processing, microwave frequency are 2450 ± 50MHz, processing power 700W, are kept for 15 minutes, protective gas is nitrogen, and flow is
40mL/min after the completion of activation, takes out after sample is cooled to room temperature under nitrogen atmosphere, is added in 1mol/L hydrochloric acid solution,
To end of reaction, filtering is washed with distilled water to neutrality, is subsequently placed into drying box drying 4 hours at 103 DEG C, obtains micro-
Wave helper activity Lignin-Based Activated Carbon.
4. the modified microwave of medium barrier plasma according to claim 1 activates lignin-base carbon resistance rod preparation method,
It is characterized by: medium barrier plasma modified lignin resin matrix activated carbon specific steps described in step 3 are as follows: by step 2
Obtained in microwave-assisted activation Lignin-Based Activated Carbon be put into the reaction chamber of medium barrier plasma processing equipment, pass through
Heating water bath water system reagent treatment obtains processing gas to 70~100 DEG C, recycle vacuum pump will be evacuated to 20 in reaction chamber~
The pressure of 30kPa, processing gas are automatically introduced into reaction chamber, then start medium barrier plasma excitation power source, are adjusted
Processing power makes processing gas in reaction chamber discharge, generates a large amount of oxygen or nitrogen plasma, live to lignin-base to 30~60W
Property carbon surface be modified processing, the processing time is 1~5 minute.
5. the modified microwave of medium barrier plasma according to claim 4 activates lignin-base carbon resistance rod preparation method,
It is characterized by: water system reagent treatment is one of water, ammonium hydroxide, the processing gas obtained after heating water bath water system reagent treatment
For one of water vapour or ammonia and water vapor mixture body.
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