CN105435771B - A kind of preparation method of tinbase composite catalyst and the cathode material containing the catalyst - Google Patents
A kind of preparation method of tinbase composite catalyst and the cathode material containing the catalyst Download PDFInfo
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- CN105435771B CN105435771B CN201510958892.0A CN201510958892A CN105435771B CN 105435771 B CN105435771 B CN 105435771B CN 201510958892 A CN201510958892 A CN 201510958892A CN 105435771 B CN105435771 B CN 105435771B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
Abstract
The invention discloses a kind of tinbase composite catalyst for belonging to environmental protection and technical field of resource comprehensive utilization and the cathode material containing the catalyst preparation method.Pink salt, citrate are uniformly mixed in water and obtain metal tin-salt solution, then it is mixed with carbon nanotubes alcohol solution, after ultrasound to stabilization add reducing agent fully reduce or add highly basic carry out hydro-thermal process, finally it is washed, filter, be dried to obtain tinbase composite catalyst.By the catalyst, conductive carbon material and binding agent in volatile alcohol after mixing, suppress on steel wire, drying to obtain the cathode material of stanniferous based composite catalyst at room temperature.Catalyst and cathode material prepared by the method, can be effectively to CO2It is electrochemically transformed, the faradic efficiency of catalytic reaction can be more than 60%, and gained cathode material long catalytic life has preferable stability.
Description
Technical field
The invention belongs to environmental protection and technical field of resource comprehensive utilization, and in particular to a kind of tinbase composite catalyst and
The preparation method of cathode material containing the catalyst.
Background technology
Carbon dioxide is the one of the major reasons for causing greenhouse effects, carries out trans-utilization to carbon dioxide, on the one hand may be used
To reduce the discharge of greenhouse gases, on the other hand can slow down because a large amount of use of fossil fuel and caused by resource exhaustion, together
Shi Shixian energy stores again.The method that conversion processing is carried out to carbon dioxide is very much, mainly there is bioanalysis, radiation method, thermalization
Method, (light) electrochemical process etc., wherein electrochemically reducing carbon dioxide method have extensive advantage：1st, driven by power, power come
Source is extensive, can directly by the use of renewable electric power or power grid give up electricity be used as power source；2nd, product has higher selectivity；3、
Operating condition is gentle, can react under normal temperature and pressure；4th, solvent can be used as proton source, it is not necessary to be passed through H2Etc. additional matter
Component；5、CO2Being convertible into can further be utilized for a variety of basic chemical industry raw materials, product, high financial profit.
Its key of Carbon dioxide electrochemical reduction is catalyst, and catalyst can directly affect the activity of reaction, stabilization
Property and selectivity of product.Prior art route use be mostly metal or alloy catalyst, it is active it is low, stability is poor, easy
The shortcomings of liberation of hydrogen, poor selectivity of product, constrain the development of the extensive recycling of carbon dioxide.
The content of the invention
The present invention is directed to deficiency of the prior art, its purpose is to provide a kind of tinbase composite catalyst and containing the catalysis
The preparation method of the cathode material of agent.
To achieve these goals, the technical solution that the present invention takes is as follows：
A kind of preparation method of tinbase composite catalyst, it is characterised in that the preparation method comprises the following steps：
(1) carbon nanotubes is added into volume ratio as 1:In the ethanol of x and the mixed liquor of deionized water, ultrasonic disperse 3h with
On, obtain solution A；
The value range of the x is：0.1<x<100；
(2) it is added to after pink salt is mixed with citrate in deionized water and forms mixed solution, the lemon in mixed solution
Acid group excessively enables tin ion to be complexed completely；By mixed solution, ultrasonic disperse is stablized to it at room temperature, obtains solution B；
(3) solution A is mixed with solution B, ultrasound is uniformly dispersed to carbon nanotubes, obtains solution C；Wherein, 1g in solution C
Carbon nanotubes corresponds to 0.001-0.1mol metal tin ions；
(4) under the conditions of continual ultrasonic, excessive borohydride salts powder or borohydride salts aqueous solution are added into solution C to tin
Ion is reduced, and into solution, bubble-free produces, and obtains solution D；Or after excessive highly basic is added into solution C, it is placed on
In polytetrafluoroethylcontainer container, at 100 DEG C -180 DEG C heat 5 it is small when more than, obtain solution E；
(5) solution D or E being filtered with deionized water, cleaned, the solid of acquisition is placed in baking oven in 40 DEG C of -80 DEG C of dryings,
The black powder of gained is tinbase composite catalyst.
The tinbase composite catalyst obtained by the solution D is tin-oxide/tin/carbon nanometer pipe composite material.
The tinbase composite catalyst obtained by the solution E is stannic oxide/carbon nano tube compound material.
Carbon nanotubes described in step (1) is single wall, double-walled or multi-walled carbon nanotube；By chemical vapour deposition technique,
Graphite acr method or Template synthesis.
For carbon nano tube surface described in step (1) after pickling or oxidation processes, its surface grafting has carboxyl or hydroxyl
Hydrophilic group, dispersion degree in deionized water improve.
Pink salt described in step (2) is stannous salt or tetravalence pink salt；The citrate is sodium citrate or lemon
Sour potassium.
Borohydride salts described in step (4) are NaBH4Or KBH4；Highly basic is NaOH or KOH；BH4 -Or OH-With tin ion
Molar ratio be more than 10.
A kind of preparation method of the cathode material of stanniferous based composite catalyst, the preparation method comprise the steps of：
(1) by tinbase composite catalyst, conductive carbon material and binding agent according to 8:1:The ratio of 0.5-4 is in volatile alcohol
In mixed, stir to volatile alcohol all volatilize, formed sticky solid；
The volatile alcohol is ethanol or isopropanol；
(2) sticky solid is suppressed on the steel wire of 150-400 mesh by pressing, dried at room temperature.
Conductive carbon described in step (1) is graphite or conductive black；Binding agent is naphthol solution or polytetrafluoroethylene (PTFE)
Solution.
Single side compacting or two-sided compacting are compressed to described in step (2), passes through roll squeezer, machine for pressing noodles or tablet press machine reality
It is existing.
The opposite side material of the two-sided compacting is the sticky solid of equivalent or the conductive material of equivalent；
The conductive materials are graphite, conductive black, carbon nanotubes or graphene.
The cathode material of tinbase composite catalyst or stanniferous based composite catalyst is in CO2Application in electrochemical conversion.
The CO2The drawing efficiency of electrochemical conversion method is more than 60%.
Beneficial effects of the present invention are：The tinbase composite catalyst and cathode material prepared using the invention, can be effectively right
CO2It is electrochemically transformed, the faradic efficiency of catalytic reaction can be reacted more than 60% and can obtain greater activity, preferably stablize
Property and the small organic molecule product such as relatively single CO, formic acid, gained cathode material long catalytic life, there is preferable stablize
Property.
Embodiment
The present invention provides a kind of tinbase composite catalyst and the cathode material containing the catalyst preparation method, tie below
Closing embodiment, the present invention will be further described, but protection scope of the present invention is not limited to this.
Embodiment 1：The preparation of tinbase composite catalyst (tin-oxide/tin/carbon nanometer pipe composite material).
By 0.02mol SnCl2Being added with 0.05mol sodium citrates in 100mL deionized waters, ultrasound is completely dissolved to it,
The SnCl of 0.2M is prepared2- sodium citrate aqueous solution, ie in solution A.
0.1g carbon nanotubes is taken, is added into the mixed solution of 25mL deionized waters/25mL ethanol, ultrasound 3 is small at room temperature
When more than carbon nanotubes is uniformly dispersed, obtain solution B.
Take 10mL solution As to be mixed with 50mL solution Bs, at ambient temperature ultrasound more than 1.5h, obtain solution C.Continuing
Under ultrasound condition, 2.78g KBH are slowly added into solution C4Reduced, reduction process at least keeps 2h, until in solution
Bubble-free is emerged, and obtains solution D.
Solution D is filtered with deionized water and is cleaned, the solid of acquisition is placed in 60 DEG C of baking ovens dry, the black powder of gained
As tinbase composite catalyst, this catalyst core are metallic tin, and surface is the tin-oxide of one layer of self-assembling formation.
Embodiment 2：The system of the cathode material of stanniferous based composite catalyst (tin-oxide/tin/carbon nanometer pipe composite material)
Standby and electrochemical reduction CO2Experiment.
Take 80mg tinbases composite catalyst (tin-oxide/tin/carbon nanometer pipe composite material), 10mg C45 carbon blacks, 20mg
PTFE emulsion (60% content), adds ethanol in proper amount, and stirring to ethanol whole is volatilized in measuring cup, obtains sticky solid；Will
Sticky solid is suppressed in tinbase composite catalyst on the cathode material on 300 mesh steel wires, formed after compacting by machine for pressing noodles
Load capacity be 20mg/cm2。
CO is carried out in H-type electrolytic cell2Reduction experiment, reaction system is three electrodes, is Pt electrodes to electrode, reference
Electrode is saturation calomel (SCE), and working electrode is above-mentioned cathode material, cathode and to passing through Nafion protons between electrode chamber
Exchange membrane separates.Reaction system is 0.1M potassium bicarbonate aqueous solutions, and CO is continually fed into reaction process2Gas.
In N before reaction2The 0.1M KHCO of saturation330 minutes, the preelectrolysis experiment of -2.0V vs SCE are first carried out in solution,
To avoid in CO2Tin-oxide is reduced in electro-reduction process.After preelectrolysis, to system in -0.6V~-2.0V sections
Linear voltammetric scan is carried out, the reduction peak of tin-oxide does not occur.
CO2The voltage range of electrochemical reducting reaction is -0.8V~-1.8V vs SCE, using 0.2V as interval, the time 1
Hour.Experiment is found, within the reaction time of 1h, Faradaic current keeps stablizing, and does not occur substantially decaying.Since -1.0V
There is formic acid generation, with alive reduction (increase of overpotential) is applied, increased trend, faraday is presented in the amount for producing formic acid
Efficiency reduces afterwards as the increase of voltage first raises, faradic efficiency highest during -1.4V, and about 65%.
Embodiment 3：The preparation of tinbase composite catalyst (stannic oxide/carbon nano tube compound material).
By 0.02mol SnCl2Added with 0.05mol sodium citrates in 100mL deionized waters, ultrasound is made to being completely dissolved
It is standby to obtain the SnCl of 0.2M2- sodium citrate aqueous solution, ie in solution A.
0.1g carbon nanotubes is taken, is added into the mixed solution of 25mL deionized waters/25mL ethanol, ultrasound 3 is small at room temperature
When more than be uniformly mixed carbon nanotubes, obtain solution B.
Take 10mL solution As to be mixed with 50mL solution Bs, at ambient temperature ultrasound more than 1.5h, obtain solution C.Continuing
Under ultrasound condition, into solution C add 0.02mol KOH, be then placed in polytetrafluoroethylcontainer container, at 150 DEG C into
Row hydro-thermal reaction, reaction time 10h, obtains solution E.
Solution E is filtered with deionized water and is cleaned, the solid of acquisition is placed in 60 DEG C of baking ovens dry, obtains that tinbase is compound to urge
Agent, this catalyst are stannic oxide/carbon nano tube compound material.Understood through Electronic Speculum characterization, the dioxy of 1-3nm in the catalyst
Change the nanosphere that tin nanometer sheet is self-assembled into 30-40nm, this nano-stannic oxide ball is deposited on single-root carbon nano-tube fiber or more
In the tube bank of root carbon nanotubes composition.
Embodiment 4：The preparation of the cathode material of stanniferous based composite catalyst (stannic oxide/carbon nano tube compound material) and
Electrochemical reduction CO2Experiment.
Take 80mg tinbases composite catalyst (stannic oxide/carbon nano tube compound material) catalyst, 10mg C45 carbon blacks,
20mg PTFE emulsions (60% content), add ethanol in proper amount, and stirring is complete to ethanol volatilization in measuring cup, obtains sticky solid
Body.Sticky solid is suppressed by machine for pressing noodles and is urged in tinbase is compound on the cathode material on 300 mesh steel wires, formed after compacting
The load capacity of agent is 20mg/cm2。
CO is carried out in H-type electrolytic cell2Reduction experiment, reaction system is three electrodes, is Pt electrodes to electrode, reference
Electrode is saturation calomel (SCE), and working electrode is above-mentioned cathode material, cathode and to passing through Nafion protons between electrode chamber
Exchange membrane separates.Reaction system is 0.1M potassium bicarbonate aqueous solutions, and CO is continually fed into reaction process2Gas.
In N before reaction2The 0.1M KHCO of saturation330 minutes, the preelectrolysis experiment of -2.0V vs SCE are first carried out in solution,
To avoid in CO2Tin-oxide is reduced in electro-reduction process.After preelectrolysis, to system in -0.6V~-2.0V sections
Linear voltammetric scan is carried out, the reduction peak of stannic oxide does not occur.CO2The voltage range of electrochemical reducting reaction is -0.8V
~-1.8V vs SCE, using 0.2V as interval, when the time is 1 small.Experiment is found, within the reaction time of 1h, Faradaic current is protected
It is fixed to keep steady, and does not occur substantially decaying.From -1.0V begin with formic acid produce, with apply it is alive reduction the (increasing of overpotential
Add), increased trend is presented in the amount for producing formic acid, and faradic efficiency reduces afterwards as the increase of voltage first raises, method during -1.4V
Efficiency highest is drawn, about 40%.
Claims (10)
1. a kind of preparation method of tinbase composite catalyst, it is characterised in that the preparation method comprises the following steps：
(1) carbon nanotubes is added into volume ratio as 1：In the ethanol of x and the mixed liquor of deionized water, more than ultrasonic disperse 3h, obtains
To solution A；
The value range of the x is：0.1<x<100；
(2) it is added to after mixing divalence or tetravalence pink salt with sodium citrate or potassium citrate in deionized water and forms mixed solution,
Citrate in mixed solution excessively enables tin ion to be complexed completely；By mixed solution at room temperature ultrasonic disperse to its
Stablize, obtain solution B；
(3) solution A is mixed with solution B, ultrasound is uniformly dispersed to carbon nanotubes, obtains solution C；Wherein, 1g carbon is received in solution C
Mitron corresponds to 0.001-0.1mol tin ions；
(4) under the conditions of continual ultrasonic, excess NaBH is added into solution C4Or KBH4Powder or NaBH4Or KBH4Aqueous solution is to tin
Ion is reduced, and into solution, bubble-free produces, and obtains solution D；Or into solution C after addition excess NaOH or KOH, by it
Be placed in polytetrafluoroethylcontainer container, at 100 DEG C -180 DEG C heat 5 it is small when more than, obtain solution E；Wherein BH4 -Or OH-With tin
The molar ratio of ion is more than 10；
(5) solution D or E are filtered with deionized water, cleaned, the solid of acquisition is placed in baking oven in 40 DEG C of -80 DEG C of dryings, gained
Black powder be tinbase composite catalyst.
2. the preparation method of a kind of tinbase composite catalyst according to claim 1, it is characterised in that by the solution D
The tinbase composite catalyst of acquisition is tin-oxide/tin/carbon nanometer pipe composite material.
3. the preparation method of a kind of tinbase composite catalyst according to claim 1, it is characterised in that by the solution E
The tinbase composite catalyst of acquisition is stannic oxide/carbon nano tube compound material.
A kind of 4. preparation method of tinbase composite catalyst according to claim 1, it is characterised in that institute in step (1)
The carbon nanotubes stated is single wall, double-walled or multi-walled carbon nanotube；Closed by chemical vapour deposition technique, graphite acr method or template
Into.
A kind of 5. preparation method of tinbase composite catalyst according to claim 1, it is characterised in that institute in step (1)
After pickling or oxidation processes, its dispersion degree in deionized water improves the carbon nano tube surface stated.
A kind of 6. preparation method of the cathode material of stanniferous based composite catalyst, it is characterised in that the preparation method include with
Lower step：
(1) tinbase for preparing the preparation method of tinbase composite catalyst of claim 1-5 any one of them a kind of is compound to urge
Agent, conductive carbon material and binding agent are according to 8:1:The ratio of 0.5-4 is mixed in volatile alcohol, is stirred to volatile
Alcohol all volatilizees, and forms sticky solid；
The volatile alcohol is ethanol or isopropanol；
(2) sticky solid is suppressed on the steel wire of 150-400 mesh by pressing, dried at room temperature.
A kind of 7. preparation method of the cathode material of stanniferous based composite catalyst according to claim 6, it is characterised in that
Conductive carbon described in step (1) is graphite or conductive black；Binding agent is naphthol solution or polytetrafluoroethylsolution solution.
A kind of 8. preparation method of the cathode material of stanniferous based composite catalyst according to claim 6, it is characterised in that
Single side compacting or two-sided compacting are compressed to described in step (2), is realized by roll squeezer, machine for pressing noodles or tablet press machine.
A kind of 9. preparation method of the cathode material of stanniferous based composite catalyst according to claim 8, it is characterised in that
The opposite side material of the two-sided compacting is the sticky solid of equivalent or the conductive material of equivalent；
The conductive materials are graphite, conductive black, carbon nanotubes or graphene.
10. tinbase composite catalyst or claim 6-9 that in claim 1-5 prepared by preparation method described in any claim
The cathode material of stanniferous based composite catalyst prepared by preparation method described in middle any claim is in CO2In electrochemical conversion
Using, it is characterised in that the CO2The faradic efficiency of electrochemical conversion method is more than 60%.
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| CN108441878A (en) * | 2018-03-01 | 2018-08-24 | 浙江大学 | A kind of electrochemically reducing carbon dioxide reaction nanometer tin-based catalyst and the preparation method and application thereof |
| CN108889291B (en) * | 2018-06-13 | 2020-10-23 | 中国科学院化学研究所 | SnO2Modified fullerene composite material with micro-nano structure and preparation method and application thereof |
| CN112768650A (en) * | 2020-12-31 | 2021-05-07 | 上海今海新材料科技有限公司 | Sodium-ion battery negative electrode material and preparation method thereof |
| CN114836778A (en) * | 2022-03-16 | 2022-08-02 | 杭州师范大学 | TiO supported by PdCu alloy particles 2 Preparation method of metal nanosheet material electrocatalyst |
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