CN108823595A - A kind of method of solar energy STEP process high-temperature electrolysis lignin - Google Patents
A kind of method of solar energy STEP process high-temperature electrolysis lignin Download PDFInfo
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Abstract
The present invention relates to a kind of solar energy STEP process high-temperature electrolysis lignin systems, the electrolyte of the system is melting NaOH-KOH, and constant-current electrolysis or constant-potential electrolysis can be used between 280~340 DEG C in electrolytic cell temperature, when using constant-current electrolysis, current density is controlled in 25~200mA/cm2Between；When using constant-potential electrolysis, voltage is controlled between 1V；After electrolysis, solid, liquid, gas tri-state product is obtained, solid product is mainly charcoal, and gaseous products are mainly hydrogen, methane and a small amount of hydro carbons, and liquid product is mainly small organic molecule.It is 340 DEG C in temperature, current density 200mA/cm2Under conditions of, lignin conversion rate is up to 83.87%, generates a large amount of hydrogen and a small amount of methane, and coking rate is low, utilizes for Liginon Resourceization and new energy development provides new approach.
Description
Technical field
The invention belongs to new energy developments and biomass recycling use field；More particularly to a kind of solar energy STEP process
The method of high-temperature electrolysis lignin.
Background technique
The reduction of fossil energy and getting worse for environmental pollution force people to seek to clean reproducible substitution in recent years
The energy.Wherein, as a kind of important renewable resource, since its yield is huge, the huge application potential of biomass is
Start to highlight.It is estimated that National 1 year can produce 1.3*109Ton dry biomass.Chinese annual stalk theoretical resources amount
Reach 450,000,000 tons of dry biomass.Biomass energy " 13 " planning and include the vast agriculture of China in many developing countries
Village area, biomass are still used as fuel directly to burn, this can cause huge pollution to environment.If can be with economically feasible side
Formula effectively recycles biomass, will efficiently solve global energy shortage problem.
Wherein lignin is the resource that native cellulose is only second on the earth as one of three kinds of component parts of biomass
Two natural polymers abundant have very big development potentiality.Because its stable tridimensional network becomes recycling
Difficult point.The whole world generates every year to be utilized in about 1.5-1.8 hundred million tons of industrial lignins only less than 2%, and the overwhelming majority is made
For cheap fuel burn-up or any discharge, the wasting of resources is not only caused, serious environmental pollution is also brought.Then, how will
Lignin is efficiently converted into high valuable chemicals and receives the extensive concern of people.Unfortunately, existing technology or
For research algae, the research of the biomass (not generating chemistry of lignin's product) based on cellulose such as stalk or locating
The a large amount of energy is consumed when managing lignin.
Solar energy has the advantages that resourceful, covering is extensive, facilitates trans-utilization, non-polluting renewable, it is considered to be 21
Century may replace one of optimal selection of traditional fossil energy.Early in the photochemical scholar Giacomo of Italy in 1912
Ciamician just proposes that the photochemical development of solar energy will make the mankind welcome real Green Chemistry industry.Solar use
Matter of utmost importance is efficient conversion solar energy.Washington, DC college professor Licht etc. proposes STEP theory first.It is by too
Positive energy photo-thermal, photoelectric coupling generate the molecule containing energy, to improve the efficiency of solar energy utilization using efficient chemical process is realized.?
In research later, including STEP ironmaking, STEP hydrogen manufacturing, STEP wastewater treatment, STEP synthesize ammonia, and STEP organic synthesis STEP receives
Rice fiber, STEP carbon capture etc., the technique using more and more extensive.
Therefore, the processing that the environmentally friendly and economically feasible method of one kind is used to large-scale waste wood element is formulated
It is still a very big challenge.
Summary of the invention
The present invention provides a kind of energy conservation, simple, inexpensive, the efficient Liginon Resourceizations of system to utilize method, the sun
Energy STEP high-temperature electrolysis lignin system, the system is using solar energy as single energy sources, in low decomposition voltage and relatively
Under cryogenic conditions, the high added values fuel such as hydrogen, methane are generated, realize the resource utilization of lignin.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of solar energy STEP process high-temperature electrolysis lignin
Method provide hot environment using the optical and thermal effect of solar energy for system, optical-electronic effect provides electric energy, to melt NaOH-
KOH carries out constant-current electrolysis or constant-potential electrolysis to lignin in the electrolytic cell with cathode and anode as electrolyte.
Further, it is electrolysed using solar energy STEP process high-temperature electrolysis lignin system, which includes the sun
Energy photothermal conversion unit, solar photoelectric conversion unit and STEP lignin conversion unit three parts, solar energy thermal transition list
Member heats lignin conversion unit, and solar photoelectric conversion unit provides electric energy, STEP wood to lignin conversion unit
Mediated conversion unit is made of cathode, anode, electrolytic cell and electrolyte, and electrolyte is melting NaOH-KOH, and electrolytic cell temperature exists
Between 280~340 DEG C, constant-current electrolysis or constant-potential electrolysis can be used, when using constant-current electrolysis, current density control exists
25~200mA/cm2Between, it is 2cm with electrode area2When for, electric current is between 0.05~0.4A at this time；Using constant voltage
When electrolysis, voltage is controlled between 1V；After electrolysis, solid, liquid, gas tri-state product is obtained, solid product is mainly charcoal, gaseous state
Product is mainly hydrogen, methane and a small amount of hydro carbons, and liquid product is mainly small organic molecule.Based on above-mentioned high-temperature electrolysis
The method of the high-temperature electrolysis lignin of lignin system, includes the following steps：
(1) electrolysis cells being made of cathode, anode, electrolytic cell and electrolyte are constructed；
(2) parabolic type solar condenser is equipped with two-dimensional tracking micromirror control system, to keep sun focus.With
At a temperature of the tuning of track control system, reactor is located at the focal spot of sun inspissator, heats solid electrolyte in electrolytic cell
To form molten state electrolyte；
(3) control lignin conversion cell temperature is constant at 280~340 DEG C；
(4) the silicon-based photovoltaic module equipped with lithium storage battery is for converting the solar into electric energy.Control constant current density
In 25~200mA/cm2, certain time is reacted, solid, liquid, gas tri-state product is generated.
The reaction mechanism of the solar energy STEP high-temperature electrolysis lignin is：
Lignin thermal chemical reaction：
Lignin→[Lignin]*(Activated State)+CxHy+Thermo-products
Lignin electrochemical reaction is：
At anode：
[Lignin]*+OH--e-→Oxidized products+CxHy+H2O
At cathode：
H2O+e-→H2+OH-
Net reaction：
Lignin→Oxidized products+CxHy+H2
Further, when electrolyte is solid-state, electrolyte is provided by the solar energy optical-thermal conversion unit and reaches completely molten
Melt thermal energy required for state.
Further, the solar photoelectric conversion unit is using solar concentrator to the temperature of thermo-electrically chemical reactor
Degree is matched, and regulates and controls heating temperature by adjusting condenser angle.
Further, the electrode material of the lignin conversion unit is nickel electrode.
Further, the lignin conversion unit uses high-purity corundum body crucible, high purity nickel or other high temperature corrosion-resistings
Type reactor.
Advantageous effects of the invention are as follows：
1, cell reaction process heats electrolyte by solar energy optical-thermal conversion unit, so that it becomes molten state forms electricity
Solve environment；Electric energy is provided using solar photoelectric conversion unit simultaneously, regulates and controls required decomposition voltage or electric current, passes through electrolysis wood
Quality obtains available fuel and high added value organic matter, realizes the conversion and storage of solar energy to chemical energy, thus real
Show the resource utilization of lignin.
2, the lignin dissolved in molten caustic soda sodium hydroxide-potassium hydroxide electrolyte of the present invention is by converting for solid-state
The high added values fuel such as charcoal, liquid small organic molecule and gaseous hydrogen methane, to realize the high added value of lignin
Conversion and resource utilization.
3, the system handles lignin, electrolysis temperature by control current density and electrolysis temperature or voltage and electrolysis temperature
Degree is 280~340 DEG C, and using constant-current electrolysis or constant-potential electrolysis, when using constant-current electrolysis, current density is controlled 25
~200mA/cm2Between, when using constant-potential electrolysis, voltage control is after 1V or so, electrolysis three hours, lignin total conversion
Reach 83.87%.
4, compared with prior art, which has the characteristics that following prominent：First, reaction is whole to utilize solar energy, nothing
Other resources, clean and environmental protection need to be utilized；Second, the reaction time substantially reduces, and 340 DEG C of temperature, current density 200mA/cm2, instead
Lignin always selects rate to reach 83.87% after answering three hours；Third, reaction temperature substantially reduce, compared to thermal cracking, the system
Lignin can effectively be converted in the environment of 340 DEG C；4th, reaction environment is relatively easy, and condition is relatively mild,
Using molten caustic soda sodium hydroxide-potassium hydroxide as electrolyte, relatively mild environment not only can achieve, but also support as electrolyte
Electrolysis；5th, cheap nickel sheet electrode can be selected in electrode material, significantly reduces production cost；6th, which can be significantly
Reduction lignin aqueous solution color.
Detailed description of the invention
Fig. 1 is that absorbing through solar energy STEP process treated lignin aqueous solution of being measured by ultraviolet specrophotometer becomes
Rate, content of lignin is 1g/l in water sample；
Fig. 2 a is solar energy STEP process treated the solid product conversion ratio at 0.4A, different temperatures, Fig. 2 b be
340 DEG C, solar energy STEP process treated solid product conversion ratio under different electric currents；
Fig. 3 is the yield of the hydrogen of solar energy STEP process and independent pyrolytic process, methane；
Fig. 4 a is the yield of solar energy STEP process treated hydrogen, methane under 340 DEG C, different electric currents, and Fig. 4 b- exists
0.4A, the yield of solar energy STEP process treated hydrogen, methane under different temperatures；
Fig. 5 is the methane production and curent change situation under the conditions of constant voltage 1V in the processing of solar energy STEP process；
Fig. 6 is solar energy STEP process liquid product and the only gas chromatographic analysis of the liquid product product of pyrolytic process；
Fig. 7 be lignin as former state, after STEP process reaction product and only after pyrolytic process reaction product in 5g/L aqueous solution
In particle diameter distribution；
Fig. 8 be lignin as former state (right side), after STEP process (in) and only after pyrolytic process (left side) aqueous solution photo, in water
The concentration of lignin sample is 1g/L.
Fig. 9 is present system schematic diagram,
In Fig. 9：1 solar energy optical-thermal conversion unit；2 solar photoelectric conversion units；3 lignin conversion units；
Figure 10 is lignin conversion cell schematics of the present invention,
In Figure 10：1 anode；2 cathodes；3 solar photoelectric conversion units；4 air guide outlets；5 carrier gas inlet pipes；6 electrolysis
Pond；7 electrolyte；8 metal devices.
Specific embodiment
Embodiment 1：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Distinguishing temperature constant is 260 DEG C, 280 DEG C, 300 DEG C, 320 DEG C and 340 DEG C, electric current point
Inconstant is 0.05A, 0.1A, 0.2A, 0.3A and 0.4A, and after reacting three hours, reaction residual is soluble in water, and use is ultraviolet
Spectrophotometric determination content of lignin, lignin conversion rate are as shown in Figure 1.
Parabolic type solar condenser is equipped with two-dimensional tracking micromirror control system in the present embodiment, to keep the sun burnt
Point.At a temperature of tracking control system tunes, reactor is located at the focal spot of sun inspissator, heats solid in corundum crucible
State electrolyte is to form molten state electrolyte；Silicon-based photovoltaic module equipped with lithium storage battery is for converting the solar into electric energy.
As shown in Figure 1, measured by ultraviolet specrophotometer, through solar energy STEP process treated lignin characteristic peak with
The raising of electric current and temperature and gradually decrease.Illustrate that STEP process is highly effective to the degradation of lignin.In 0.4A,
Under conditions of 340 DEG C, lignin conversion rate is up to 83.87%.
Embodiment 2：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Distinguishing temperature constant is 260 DEG C, 280 DEG C, 300 DEG C, 320 DEG C and 340 DEG C, electric current point
Not it is constant be 0.05A, 0.1A, 0.2A, 0.3A and 0.4A, it is after reacting three hours, reaction residual is soluble in water, consolidate
After liquid separation, dry filter residue is washed to get charcoal, yield is as shown in Figure 2.
As shown in Figure 2, as the temperature rises, charcoal yield is significantly raised, from 3.94% to 7.72% (260 DEG C,
0.4A) (340 DEG C, 0.4A).Well below being commonly pyrolyzed obtained coking rate.Illustrate under solar energy STEP process, melts
NaOH-KOH serves not only as electrolyte, and lignin can be made heated more balanced, dispersion more thoroughly, be conducive to convert
The progress of reaction.And in different current responses, with the raising of electric current, coking rate is not changed significantly, but fluctuate compared with
Greatly.
Embodiment 3：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Keeping temperature constant is 340 DEG C, and constant electric current difference is 0A and 0.4A, reacts three hours,
Gaseous products are acquired in reaction, by gas chromatographic analysis hydrogen and methane content, as shown in Figure 3.
From the figure 3, it may be seen that the gas yield of STEP lignin conversion process will be far longer than the gas yield of only pyrolytic reaction.
The volume of methane is reduced over time during STEP lignin reaction, but the increase of hydrogen.And only pyrolytic reaction
Predominant gas product is methane, and with the growth in reaction time, the amount of methane gradually increases.Speculate that methane may be from lignin
Methoxyl group in molecule is heated fall off produced by, and in STEP reaction, lignin is influenced by the coupling of thermoelectric field, reaction
The oxidation of initial stage methoxyl group, which falls off, to be become apparent.In subsequent reaction process, STEP lignin reaction is in anode, most possibly
It is lignin molecule directly in middle part chain rupture, is broken down into organic oxycarbide.With further oxidation, these organic matters can quilt
Be oxidized to much smaller molecule, rather than only pyrolytic reaction when, from the edge chain rupture of lignin molecule, it is organic to form methane etc.
Object.So there is the amount that methane content (19.814mL) caused by only pyrolytic reaction is higher than the reaction of STEP lignin conversion
(7.53mL)。
Embodiment 4：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Distinguishing temperature constant is 260 DEG C, 280 DEG C, 300 DEG C, 320 DEG C and 340 DEG C, electric current point
Inconstant is 0.05A, 0.1A, 0.2A, 0.3A and 0.4A, reacts three hours, acquires gaseous products in reaction, pass through gas phase color
Spectrum analysis hydrogen and methane content, as shown in Figure 4.
As shown in Figure 4, the generation of hydrogen is promoted by the increase of temperature and electric current.Methane production is increased with the raising of temperature,
, just with the effect of electric current on the contrary, electric current is higher, methane production is lower for this.The result shows that gas conversion has selectivity, with temperature
Variation with electric current and change, i.e., can by adjusting temperature (sun thermochemical process) and Faradaic current (sun electrochemical process)
To realize the highly selective of gaseous product.
Embodiment 5：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Keeping temperature constant is 340 DEG C, and constant voltage is 1V, reacts three hours, acquires in reaction
Gaseous products monitor real-time current with multimeter, as a result as shown in Figure 5 by gas chromatographic analysis methane content
As shown in Figure 5, most start that a biggish current density is presented due to fresh electrode surface, then rapidly under
Drop, this shows that oxidation reaction has occurred really in lignin at high temperature.Then pushed away according to the production quantity of methane in electrolytic process
It surveys, the average oxidation state of lignin is possible to time to time change in experiment, illustrates the transformation mechanism of lignin at any time
Change and changes.
Embodiment 6：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Keeping temperature constant is 340 DEG C, and constant electric current difference is 0A and 0.4A, reacts three hours,
Reaction residual is dissolved in water, pH value is adjusted to 3 or so with hydrochloric acid, filtering extracts filtrate with ether, extracted with gas chromatographic analysis
Liquid product is taken, as a result as shown in Figure 6
It will be appreciated from fig. 6 that the complicated multiplicity of the organic matter extracted after reaction.The reaction product and STEP lignin conversion being only pyrolyzed
It compares, only pyrolytic reaction generates more higher organic matter.And the more low boiling points of STEP lignin conversion generation are organic
Object (c, d).This directly confirms the deduction to liquid product above.It has to be mentioned that this is also only to be driven for first 19 minutes
The organic matter driven out of.Illustrate that STEP lignin conversion is that small molecule water soluble organism plays promotion work to lignin conversion
With.
Embodiment 7：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Keeping temperature constant is 340 DEG C, and constant electric current difference is 0A and 0.4A, reacts three hours,
Reaction residual is dissolved in water, is configured to 100mL solution, measures particle size respectively with laser particle analyzer, as shown in Figure 7.
As shown in Figure 7, there are three peak is assembled in thermal decomposition product, the size at one of peak is bigger than primary sample, this meaning
Size distribution of the product in pyrolytic process be it is extensive, irregular depolymehzation process not only occurs for lignin, but also sends out
Raw irregular depolymehzation process.But compared with independent pyrolysis, condensate size is obviously reduced, but still has an aggregation peak.Knot
Fruit shows that stepping lignin conversion can effectively reduce the partial size that lignin is assembled in aqueous solution.
Embodiment 8：The present embodiment provides hot environment using the optical and thermal effect of solar energy for system, and optical-electronic effect provides
Electric energy is being that cathode and anode are electrolysed lignin with nickel sheet electrode to melt NaOH-KOH as electrolyte.The sun
The method of energy STEP process high-temperature electrolysis lignin carries out in the steps below：
17g KOH, 13g NaOH and 0.5g lignin are uniformly mixed respectively, are put into corundum crucible；It respectively will be effective
Area 2cm2Nickel sheet as electrode；Keeping temperature constant is 340 DEG C, and constant electric current difference is 0A and 0.4A, reacts three hours,
Reaction residual is dissolved in water, is configured to 500mL solution, solution colour is as shown in Figure 8.
As shown in Figure 8, the lignin liquor after being only pyrolyzed obviously deepens, and after STEP lignin conversion process, wood
The coloration of quality solution is substantially reduced.Reason may be that the chromophoric groups such as C=O, C=C increase in lignin after high-temperature heat treatment
More ,-OH ,-CH ,-OCH wait auxochrome groups also to be changed, so as to cause induced coloration.But coupled solar-electricity it
Afterwards, most chromophoric group and Zhu Se group are oxidized, and aromatic rings is destroyed to be removed with quinone structure, so solution coloration
It is substantially reduced.
Claims (10)
1. a kind of method of solar energy STEP process high-temperature electrolysis lignin, it is characterised in that the electrolytic method utilizes solar energy
Optical and thermal effect provide hot environment for system, optical-electronic effect provides electric energy, to melt NaOH-KOH as electrolyte, in band
Have in the electrolytic cell of cathode and anode and constant-current electrolysis or constant-potential electrolysis are carried out to lignin.
2. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 1, it is characterised in that electrolysis
Pond temperature is between 280~340 DEG C.
3. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 2, it is characterised in that use
When constant-current electrolysis, current density is controlled in 25~200mA/cm2Between.
4. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 2, it is characterised in that use
When constant-potential electrolysis, voltage is controlled between 1V.
5. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 1, it is characterised in that KOH with
The quality of NaOH is 17：13.
6. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 1, it is characterised in that described
Electrolytic cell is high temperature corrosion-resisting type reactor.
7. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 6, it is characterised in that use
High-purity corundum body crucible, high purity nickel are as electrolytic cell.
8. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 1, it is characterised in that cathode
It is nickel electrode with anode.
9. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 1, it is characterised in that be equipped with
The silicon-based photovoltaic module of lithium storage battery is for converting the solar into electric energy.
10. a kind of method of solar energy STEP process high-temperature electrolysis lignin according to claim 1, it is characterised in that utilize
Solar concentrator is for converting the solar into thermal energy.
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