CN105601074B - A kind of electroplating sludge cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide - Google Patents
A kind of electroplating sludge cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide Download PDFInfo
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Abstract
The high-efficiency resource recycling new method of processing is cooperateed with carbon dioxide the invention discloses a kind of electroplating sludge, it is to prepare the cathod catalyst that charcoal is used as bioelectrochemical system by raw material of electroplating sludge, it realizes the high-efficiency resource recycling to electroplating sludge, while cooperates with processing carbon dioxide and obtain a kind of new method of the organic product of high added value.The present invention uses the electroplating sludge rich in heavy metal to prepare charcoal as bioelectrochemical system cathod catalyst for raw material, it is simple for process of low cost, reaction condition is mild, and the charcoal performance prepared is stablized, it is stronger to the catalysis reducing power of carbon dioxide, available for catalysis carbon dioxide reduction high efficient resourcing is cooperateed with realize electroplating sludge and carbon dioxide.
Description
Technical field：
The high-efficiency resource recycling new method of processing is cooperateed with carbon dioxide the present invention relates to a kind of electroplating sludge.
Background technology：
Electroplating sludge is a kind of dangerous solid waste, is mainly derived from electroplating industry wastewater treatment process.With China
Economic development, electroplating industry are quickly grown, and the discharge of the annual electroplating wastewater in China is increased rapidly, lead to the electroplating sludge generated
It gradually rises, and has caused a series of resource and environmental problem.And chemical composition is extremely complex in electroplating sludge, mainly
Contain the heavy metal compounds such as iron, nickel, copper, zinc, chromium and solubility salt.Wherein, 0.5~1% is usually contained in electroplating sludge
Nickel, 1~2% copper ,~3% chromium, 1~2% zinc etc., metal content be far above metal high-grade ore, have it is higher
Recycle value.Both at home and abroad to there are mainly three types of the processing modes of electroplating sludge：Harmlessness disposing, thermochemical treatment, resource
Change and utilize.Since innoxious and thermochemical treatment electroplating sludge will all generate environment different degrees of influence, and can not make money
Source is utilized effectively.Therefore, with the reinforcing of circular economy idea, grinding in electric plating sludge resource use aspects in recent years
Study carefully and significantly increase, this will also become next research hotspot.
Carbon dioxide is one of main greenhouse gases, has the ability for absorbing infrared ray, and form one in an atmosphere
Kind invisible cloche so that the heat of solar radiation to the earth can not outer layers space divergence and generate " greenhouse effects ".Greatly
The discharge of amount GHG carbon dioxide causes global climate significantly to warm, and leads to sea-level rise, the polarization of water resource
More serious, grain yield is impacted, and economic development and the existence of the mankind reduce carbon dioxide therefore by serious threat
Discharge and reduce atmospheric carbon dioxide levels and become an important subject of human survival and development.Dioxy at present
Changing carbon reduction recovery method has：Radiate reduction, electronation, thermochemical reduction, photoreduction and electrochemical reduction etc..Although
Many reduction conversion processes are feasible in theory, but by CO under alap energy consumption2Be reduced into high added value has
Machine object is one of Research Challenges, and bioelectrochemical system reduction method is expected to become solution in numerous reducing and conversion methods
The effective means of this difficulties.
It is badly in need of safe and efficient recycling for electroplating sludge, carbon dioxide is badly in need of effectively reduction while it is high additional to obtain
The problems such as being worth organic matter, it would be highly desirable to solve.
Invention content：
The high-efficiency resource recycling for cooperateing with processing with carbon dioxide the object of the present invention is to provide a kind of electroplating sludge is newly square
Method is to prepare the cathod catalyst that charcoal is used as bioelectrochemical system by raw material of electroplating sludge, is realized dirty to plating
The high-efficiency resource recycling of mud, while cooperate with processing carbon dioxide and obtain a kind of new method of the organic product of high added value.
The present invention is achieved by the following technical programs：
A kind of electroplating sludge cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide, includes the following steps：
(1) using electroplating sludge as raw material, drying, 700~900 DEG C of 2~4h of pyrolysis pyrolysis under atmosphere of inert gases,
It stirs for 24 hours, washes in 2mol/L HCl solutions, drying, as sludge organism charcoal；
(2) the sludge organism charcoal will be made in step (1) to mix with certain proportion with ethyl alcohol, nafion solution, ultrasound
Into pasty mixture, and by pasty mixture with 0.5~1mg/cm2Load capacity be supported on carbon cloth, the paste will have been loaded
Cathod catalyst of the carbon cloth of shape mixture as bioelectrochemical system leads into the cathode chamber of the bioelectrochemical system
Enter carbon dioxide, realization electroplating sludge cooperates with processing with carbon dioxide.
For electroplating sludge after high temperature pyrolysis, major metal component is converted to CuFeNi, FeNi, Fe1.6Ni2.4,
Fe8.7NiS10And Cu2The metallic compounds such as O, and such compound can greatly reduce the reduction potential of carbon dioxide, to dioxy
The reduction conversion for changing carbon has very strong catalytic action.Carbon dioxide is passed through into the cathode chamber of bioelectrochemical system, and is fitted
When the height for adjusting additional power source, the organic compound of a variety of high added values can obtain by detection, organic product in the present invention
Mainly there are formic acid, acetic acid and methane etc..
Preferably, step (1) electroplating sludge by pyrolysis stirs for 24 hours in 2mol/L HCl solutions, in being washed to
Property, 105 DEG C of dryings are milled to 100~150 mesh.
Preferably, the sludge organism charcoal 20mg, the ethyl alcohol 1ml and 1 μ l of the nafion solution are mixed in step (2)
It closes.Nafion solution, that is, perfluor polystyrolsulfon acid solution is a kind of material with many properties, electrode modification,
The fields such as electrochemical analysis, electrochemical catalysis, chemical sensor, nano material preparation have extensive use.
Preferably, step (2) bioelectrochemical system applied voltage >=0.3V.Applied voltage is set as in the present invention
>=0.3V, as applied voltage increases, organic product yield also gradually increases.
Further, formic acid, acetic acid and methane is made in the bioelectrochemical system.
Preferably, step (1) the electroplating sludge raw material includes Fe, Ni and Cu.
Further, described metal Fe, Ni and Cu become CuFeNi, FeNi, Fe by the pyrolysis1.6Ni2.4,
Fe8.7NiS10And Cu2O metallic compounds.
The beneficial effects of the invention are as follows：
(1) its major metal component of electroplating sludge after high temperature pyrolysis is converted to CuFeNi, FeNi, Fe1.6Ni2.4,
Fe8.7NiS10And Cu2The metallic compounds such as O, and such compound can greatly reduce the reduction potential of carbon dioxide, to dioxy
The reduction conversion for changing carbon has very strong catalytic action；
(2) electroplating sludge rich in heavy metal is used to prepare charcoal as bioelectrochemical system cathode catalysis for raw material
Agent, simple for process of low cost, reaction condition is mild, and the charcoal performance prepared is stablized, the catalysis to carbon dioxide
Reducing power is stronger, and high efficient resourcing is cooperateed with realize electroplating sludge and carbon dioxide available for catalysis carbon dioxide reduction.
Description of the drawings：
Fig. 1 is bioelectrochemical system installation drawing；
Fig. 2 is the SEM figures of 1 electroplating sludge charcoal of the embodiment of the present invention；
Fig. 3 is the XRD diagram of 1 electroplating sludge charcoal of the embodiment of the present invention；
Fig. 4 is the XPS figures of 1 electroplating sludge charcoal of the embodiment of the present invention；
Fig. 5 is yield of acetic acid figure in the embodiment of the present invention 1, embodiment 3, comparative example 1, comparative example 2；
Fig. 6 is formate yield figure in the embodiment of the present invention 1, embodiment 3, comparative example 1, comparative example 2.
Specific embodiment：
It is the further explanation to the present invention rather than limitation of the present invention below.
The equipment and reagent used except special instruction, the present invention is the art routine commercial products.
Embodiment 1
To be rich in the electroplating sludge of Fe, Ni, Cu heavy metal as raw material, 105 DEG C of baking 2h, lower 900 DEG C in nitrogen gas atmosphere
4h is pyrolyzed, is stirred for 24 hours in 2mol/L HCl solutions after cooling, is washed to neutrality, 105 DEG C of dryings are milled to 100~150 mesh,
As sludge organism charcoal.
Electroplating sludge (20mg) before not being pyrolyzed obtained sludge organism charcoal (20mg) or respectively with ethyl alcohol 1ml and nafion
1 μ l of solution are mixed, ultrasonic into pasty mixture, and by pasty mixture with 0.5~1mg/cm2Carrying capacity be supported on carbon cloth,
Cathod catalyst of the carbon cloth as bioelectrochemical system as shown in Figure 1 of pasty mixture will be loaded, to bioelectrochemical
Carbon dioxide is passed through in the cathode chamber of system, realization electroplating sludge cooperates with processing with carbon dioxide.
Physico-Chemical Characterization discovery, SEM figure such as Fig. 2, XRD diagram such as Fig. 3, XPS are carried out to the sludge organism charcoal prepared
Figure is as shown in Figure 4.It is obtained by Fig. 2, the sludge organism charcoal of gained is more regular laminated structure, is obtained by Fig. 3 and Fig. 4, electricity
It plates and contains the various heavies such as Fe, Ni, Cu in sludge in raw material after prepared by pyrolysis, be transformed into CuFeNi, FeNi,
Fe1.6Ni2.4, Fe8.7NiS10And Cu2The metallic compounds such as O.
The results show that carbon dioxide is passed through into the bioelectrochemical system cathode chamber of cathode load sludge organism charcoal,
Adjusting applied voltage is 0.3V, monitors the discovery of its cathode product, there is a small amount of formic acid, acetic acid and methane production, yield of acetic acid such as Fig. 5
It is as shown in Figure 6 with formate yield.And carbon dioxide is passed through into the bioelectrochemical system cathode chamber of cathode load electroplating sludge,
When it is 0.6V to adjust voltage, the generation of organic matter is not detected.
Embodiment 2
It is same as Example 1, the difference lies in：
In the lower 700 DEG C of pyrolysis 2h of nitrogen gas atmosphere.
Since 4 hour pyrolysis times make pyrolytic reaction more thorough in embodiment 1, pyrolysis prepares CuFeNi,
FeNi, Fe1.6Ni2.4, Fe8.7NiS10And Cu2The effect of the metallic compounds such as O is more better than being pyrolyzed 2 hours in embodiment 2.
Embodiment 3
It is same as Example 1, the difference lies in：
Adjusting applied voltage is 0.6V, monitors the discovery of its cathode product, there is a small amount of formic acid, acetic acid and methane production, acetic acid
Yield such as Fig. 5 and formate yield are as shown in fig. 6, formic acid, acetic acid and methane concentration ratio applied voltage significantly increase when being 0.3V.
Comparative example 1
It is same as Example 1, the difference lies in：
In the case of non-applied voltage, the product situation of cathode chamber is monitored.As a result, it has been found that it on this condition, does not detect
To organic compound, as shown in Figure 5 and Figure 6.
Comparative example 2
It is same as Example 3, the difference lies in：
Cathode electrode is carbon cloth, unsupported sludge organism charcoal, monitors the discovery of its cathode product, has no formic acid, acetic acid and first
Alkane produces, and illustrates that sludge organism charcoal has catalytic action to the reduction of carbon dioxide conversion really, as shown in Figure 5 and Figure 6.
It can be obtained by Fig. 5 and Fig. 6：Organic compound is not detected in non-applied voltage, and adjusting applied voltage is 0.3V,
The discovery of its cathode product is monitored, there is a small amount of formic acid, acetic acid and a methane production, adjustings applied voltage is 0.6V, formic acid, acetic acid and first
Alkane concentration ratio applied voltage significantly increases when being 0.3V.
Comparative example 3
It is same as Example 3, the difference lies in：
Charcoal is prepared as cathod catalyst by raw material of municipal sludge.
Comparative example 4
It is same as Example 3, the difference lies in：
Charcoal is prepared as cathod catalyst by raw material of printing and dyeing sludge.
Comparative example 3, comparative example 4 are compared with Example 3 compared in external voltage under conditions of 0.6V, to detect the production of its cathode
Object is found, is urged when using the electroplating sludge not being pyrolyzed, the municipal sludge charcoal being pyrolyzed and printing and dyeing sludge charcoal as cathode
The generation of formic acid, acetic acid and methane organic compound is showed no during agent, in bioelectrochemical system, and detects and finds that municipal administration is dirty
The metallic elements such as Cu, Ni are had no in two kinds of sludge of mud and printing and dyeing sludge, and the electroplating sludge that is not pyrolyzed, the municipal administration after pyrolysis are dirty
CuFeNi, FeNi, Fe are had no in mud charcoal and printing and dyeing sludge charcoal1.6Ni2.4, Fe8.7NiS10And Cu2The metal compounds such as O
Object, illustrate to have restored carbon dioxide conversion catalytic action is metallic compound.
Its major metal component of electroplating sludge after high temperature pyrolysis is converted to CuFeNi, FeNi, Fe1.6Ni2.4,
Fe8.7NiS10And Cu2The metallic compounds such as O, and such compound can greatly reduce the reduction potential of carbon dioxide, to dioxy
The reduction conversion for changing carbon has very strong catalytic action.
Above-listed detailed description is illustrating for possible embodiments of the present invention, which is not to limit this hair
Bright the scope of the claims, all equivalence enforcements or change without departing from carried out by the present invention are intended to be limited solely by the scope of patent protection of this case
In.
Claims (6)
1. a kind of electroplating sludge cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide, which is characterized in that including such as
Lower step：
(1) using electroplating sludge as raw material, drying, 700~900 DEG C of 2~4h of pyrolysis under atmosphere of inert gases, then in 2mol/L
It stirs for 24 hours, washes in HCl solution, drying, as sludge organism charcoal；
(2) the sludge organism charcoal will be made in step (1) to mix with ethyl alcohol, nafion solution, it is ultrasonic into pasty mixture, and
By pasty mixture with 0.5~1mg/cm2Load capacity be supported on carbon cloth, will load the pasty mixture carbon cloth make
For the cathod catalyst of bioelectrochemical system, carbon dioxide is passed through into the cathode chamber of the bioelectrochemical system, is realized
Electroplating sludge cooperates with processing with carbon dioxide；
Step (2) bioelectrochemical system applied voltage >=0.3V.
2. electroplating sludge according to claim 1 cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide,
It is characterized in that, step (1) stirs the electroplating sludge of pyrolysis for 24 hours in 2mol/L HCl solutions, is washed to neutrality, and 105 DEG C dry
It is dry, it is milled to 100~150 mesh.
3. electroplating sludge according to claim 1 cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide,
It is characterized in that, mixes the sludge organism charcoal 20mg, the ethyl alcohol 1ml and 1 μ l of the nafion solution in step (2).
4. electroplating sludge according to claim 1 cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide,
It is characterized in that, formic acid, acetic acid and methane is made in the bioelectrochemical system.
5. electroplating sludge according to claim 1 cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide,
It is characterized in that, step (1) the electroplating sludge raw material includes Fe, Ni and Cu.
6. electroplating sludge according to claim 5 cooperates with the high-efficiency resource recycling new method of processing with carbon dioxide,
It is characterized in that, described metal Fe, Ni and Cu become CuFeNi, FeNi, Fe by the pyrolysis1.6Ni2.4, Fe8.7NiS10And Cu2O
Metallic compound.
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| IT201700110538A1 (en) * | 2017-10-03 | 2019-04-03 | Univ Degli Studi Milano | MICROBIAL ELECTROCHEMICAL SYSTEMS BASED ON BIOMASS AND BIOGENIC MATERIALS |
| CN108704933B (en) * | 2018-04-26 | 2020-09-11 | 中国石油大学(北京) | Device and method for in-situ remediation of hexavalent chromium contaminated soil |
| CN110639488A (en) * | 2019-08-30 | 2020-01-03 | 中国科学院广州能源研究所 | Application of biomass-based carbon material in electrochemical reduction of carbon dioxide |
| CN110639489B (en) * | 2019-08-30 | 2022-08-12 | 中国科学院广州能源研究所 | Application of municipal sludge biochar in electrochemical synthesis of ammonia |
| CN111593371B (en) * | 2020-06-10 | 2021-05-11 | 中国科学院广州能源研究所 | Municipal sludge multistage carbon material and application thereof in carbon dioxide electrochemical reduction |
| CN111900415A (en) * | 2020-07-10 | 2020-11-06 | 上海大学 | Method for preparing metal-nitrogen co-doped oxygen reduction catalyst by using electroplating sludge |
| CN114586609B (en) * | 2022-03-28 | 2023-04-28 | 香港科技大学 | Planting method for improving yield and active ingredient content of medicinal plants |
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