CN109694120A - Chitin based biomass charcoal double-face electrode piece and preparation method thereof for Electro Sorb - Google Patents
Chitin based biomass charcoal double-face electrode piece and preparation method thereof for Electro Sorb Download PDFInfo
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- CN109694120A CN109694120A CN201910054662.XA CN201910054662A CN109694120A CN 109694120 A CN109694120 A CN 109694120A CN 201910054662 A CN201910054662 A CN 201910054662A CN 109694120 A CN109694120 A CN 109694120A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
Abstract
The chitin based biomass charcoal double-face electrode piece and preparation method thereof that the present invention relates to a kind of for Electro Sorb.Its technical solution is: dry by chitin powder cleaning, screening in nitrogen atmosphere and 400~500 DEG C of 1~2h of heat preservation, obtains pre- charing powder.Pre- charing powder and potassium hydroxide powder are mixed and are placed in vacuum tube furnace, in 800 DEG C~900 DEG C 2~3h of heat preservation, obtains biomass carbon powder I.Biomass carbon powder I is added in the HCl solution of 10wt%, is stirred, cleaning obtains biomass carbon powder II.Conductive agent, biomass carbon powder II and Kynoar are mixed, are dissolved in dimethyl acetamide, is mixed；Obtained mixed serum is coated uniformly on the two sides of collector titanium sheet, dries, and the chitin based biomass charcoal double-face electrode piece for Electro Sorb is made in freeze-drying.Production cost of the present invention is low, and made product electrode internal resistance is small, capacitance is high and absorption property is good, the processing suitable for different quality.
Description
Technical field
The invention belongs to chitin based biomass charcoal double-face electrode chip technology fields.More particularly to a kind of for Electro Sorb
Chitin based biomass charcoal double-face electrode piece and preparation method thereof.
Background technique
Electro Sorb technology has that safe and efficient, device simple, convenient for safeguarding, operation energy consumption is low, the removal of environmental-friendly, salinity
The advantages that rate height and ant-scaling and be widely used in high-salt wastewater processing (Huang Wei capacitive deionization method electrode material desalination be special
Property and processing vanadium extraction high-salt wastewater study the Wuhan [D]: Wuhan University of Technology, 2014).However, some about Electro Sorb desalination
Experimental study is low and the problems such as electrode utilization rate is not high in the prevalence of adsorption efficiency, such issues that restrict to a certain extent
The industrial applications of Electro Sorb desalination (Wang L, Zhou Y, Wang J, et al.Approaching capacitive
deionization(CDI)on desalination of water and wastewater-new progress and its
potential[J].Advanced Materials Research,2015,1088(3):557-561；Zhang Shichun, Liu Haining,
Wang Shidong etc. electric adsorption electrode Progress In Preparation [J] Treatment of Industrial Water, 2017,37 (5): 5-9).
Currently, widely used Carbon Materials have good electric conductivity, biggish specific surface area, excellent chemical stability
And morphology controllable, it is considered to be a kind of ideal electrode material, including active carbon, carbon aerogels, carbon nanotube, graphene and charcoal
Fiber etc., however the most production cost valuableness of these carbon materials and complex process, are difficult large-scale industrial production.Common is carbon-based
Material surface has hydrophobicity, causes salting liquid ion and the contact resistance in carbon material surface duct to increase, largely drops
Low its capacitive property (influence [J] of the such as Duan little Yue, Chang Limin, Liu Wei preparation process to activated carbon electrodes electro adsorption capacity
Environmental science and technology, 2010,33 (5): 63-66；Li Na, Han Yiming, the surface for being permitted to build the ordered mesoporous carbon material such as hero are modified
And Electrochemical Properties [J] functional material, 2015,46 (S1): 25-29).
In the preparation process of electrode slice, common method has a pressed disc method and mould shape method, but these methods there is also
Electrode material the problem of being unevenly distributed on a current collector (Gao feng, Shao guanghua, Qu jiangying, Lv
siyuan,Li yuqian,Wu mingbo.Tailoring of porous and nitrogen-rich carbons
derived from hydrochar for high-performance supercapacitor
electrodes.Electrochimica Acta,2015,155,201-208).Grinding for electrode slice is prepared using cladding process at present
Study carefully actually rare, Meng Yulan (preparation of Meng Yulan porous charcoal and flowing electrode and its research [D] Dalian University of Science & Engineering of desalting performance
University, 2015) use the electrode of the cladding process preparation problem larger there is also electrode material cost valuableness and electrode internal resistance.
Summary of the invention
The present invention is directed to overcome the deficiencies of existing technologies, and it is an object of the present invention to provide a kind of production cost it is low for Electro Sorb
The preparation method of chitin based biomass charcoal double-face electrode piece, the chitin based biomass for Electro Sorb prepared with this method
Charcoal double-face electrode plate electrode internal resistance is small, capacitance is high and absorption property is good.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that:
Step 1: chitin powder is cleaned 3~5 times with deionized water, filter, dry 2~3h at 60 DEG C~80 DEG C,
Screening obtains the chitin powder that partial size is less than 0.0385mm；The chitin powder by partial size less than 0.0385mm is placed in again
In quartz boat, under the conditions of nitrogen atmosphere, 400~500 DEG C is warming up to the rate of 5~10 DEG C/min, 1~2h is kept the temperature, obtains
Pre- charing powder.
Step 2: pressing the pre- charing powder: the mass ratio of potassium hydroxide powder is 3~5: 1, by the pre- charing powder
It is mixed with potassium hydroxide powder, obtains mixed-powder；The mixed-powder is placed in vacuum tube furnace, with 5~10 DEG C/min
Rate be warming up to 800 DEG C~900 DEG C, keep the temperature 2~3h, obtain biomass carbon powder I.
Step 3: being 0.08~0.12Kg/L by solid-to-liquid ratio, it is 10% that mass fraction, which is added, in the biomass carbon powder I
HCl solution in, stir 10~15min, stand 1~2h；It is cleaned 2~4 times with deionized water again, dries, obtain biomass carbon
Powder II.
Step 4: pressing conductive agent: the biomass carbon powder II: the mass ratio 1 of Kynoar: (15~20): (2~
4), the conductive agent, the biomass carbon powder II and the Kynoar are mixed, obtain mixture；Solid-to-liquid ratio is pressed again
For 0.15~0.2Kg/L, the mixture is dissolved in dimethyl acetamide, 10~15min of ultrasonic mixing, magnetic agitation 1~
2h obtains mixed serum.
Step 5: the mixed serum to be coated uniformly on to the one side of collector titanium sheet, dry；Again by the mixed serum
It is evenly applied to the another side of collector titanium sheet, is dried；Then it is freeze-dried 6~8h, the chitin base for Electro Sorb is made
Biomass carbon double-face electrode piece.
Purity >=95% of the chitin powder, the partial size < 0.05mm of chitin powder.
Purity >=99% of the potassium hydroxide powder；The partial size < 0.1mm of potassium hydroxide powder.
Purity >=99.5% of the Kynoar powder, the partial size < 0.1mm of Kynoar powder.
The conductive agent is one of graphite, carbon fiber, carbon nanotube, graphene and acetylene black.
The average coating thickness of the coating is 0.25~0.3mm.
Due to the adoption of the above technical scheme, the present invention has the positive effect that compared with the existing technology:
(1) present invention is first carbonized in advance using chitin powder as raw material, then by KOH modification and keeps reaction system
Temperature, so that its is carried out complete carbonization reaction, obtained biomass carbon powder II is under binder and conductive agent collective effect
Coated in collector titanium sheet, so that the chitin based biomass charcoal double-face electrode piece for Electro Sorb be made, production technology is simple
It is single and at low cost.
(2) for the chitin that the present invention uses for natural material, rich reserves are nontoxic.Biomass carbon powder II is unique
Three-dimensional self supporting structure can effectively overcome powder carbon-based material in preparing electrode process since the addition of binder etc. causes
Electrode internal resistance increase, Carbon Materials duct blocking, capacitive property decline the defects of, i.e., the first prepared by the present invention for Electro Sorb
The electrode internal resistance of shell element based biomass charcoal double-face electrode piece is smaller, Carbon Materials duct is unobstructed and capacitive property is higher.
(3) present invention during the preparation process, in addition to prepared by biomass carbon powder I, remaining is carried out at normal temperature, energy consumption compared with
It is low low with production cost.The Electro Sorb efficiency of the prepared chitin based biomass charcoal double-face electrode piece for Electro Sorb is than single
Face electrode is significantly increased.
(4) the chitin based biomass charcoal double-face electrode piece prepared by the present invention for Electro Sorb is inhaled for metal in waste water
Sea water desalination is echoed with good adsorption effect, and the chitin based biomass charcoal double-face electrode piece for Electro Sorb prepared is suitable
It is applied widely in water process of different nature.
Therefore, production cost of the invention is low, the prepared chitin based biomass charcoal double-face electrode for Electro Sorb
Plate electrode internal resistance is small, capacitance is high and absorption property is good, the processing suitable for different quality.
Detailed description of the invention
Fig. 1 is a kind of SEM figure of biomass carbon II prepared by the present invention；
Fig. 2 is the using effect of the three kinds prepared by the present invention chitin based biomass charcoal double-face electrode pieces for Electro Sorb
Figure.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection scope
System.
It is first that technical parameter Unify legislation involved in present embodiment is as follows to avoid repeating, in embodiment not
It repeats again:
Purity >=95% of the chitin powder, the partial size < 0.05mm of chitin powder.
Purity >=99% of the potassium hydroxide powder；The partial size < 0.1mm of potassium hydroxide powder.
Purity >=99.5% of the Kynoar powder, the partial size < 0.1mm of Kynoar powder.
The average coating thickness of the coating is 0.25~0.3mm.
Implementation case 1
A kind of chitin based biomass charcoal double-face electrode piece and preparation method thereof for Electro Sorb.It is made described in the present embodiment
The step of Preparation Method, is:
Step 1: chitin powder is cleaned 3~5 times with deionized water, filter, dry 2~3h at 60 DEG C~80 DEG C,
Screening obtains the chitin powder that partial size is less than 0.0385mm；The chitin powder by partial size less than 0.0385mm is placed in again
In quartz boat, under the conditions of nitrogen atmosphere, 400~440 DEG C is warming up to the rate of 5~10 DEG C/min, 1~2h is kept the temperature, obtains
Pre- charing powder.
Step 2: pressing the pre- charing powder: the mass ratio of potassium hydroxide powder is 3~4: 1, by the pre- charing powder
It is mixed with potassium hydroxide powder, obtains mixed-powder；The mixed-powder is placed in vacuum tube furnace, with 5~10 DEG C/min
Rate be warming up to 800 DEG C~850 DEG C, keep the temperature 2~3h, obtain biomass carbon powder I.
Step 3: being 0.08~0.12Kg/L by solid-to-liquid ratio, it is 10% that mass fraction, which is added, in the biomass carbon powder I
HCl solution in, stir 10~15min, stand 1~2h；It is cleaned 2~4 times with deionized water again, dries, obtain biomass carbon
Powder II.
Step 4: pressing conductive agent: the biomass carbon powder II: the mass ratio 1 of Kynoar: (15~18): (2~
3), the conductive agent, the biomass carbon powder II and the Kynoar are mixed, obtain mixture；Solid-to-liquid ratio is pressed again
For 0.15~0.2Kg/L, the mixture is dissolved in dimethyl acetamide, 10~15min of ultrasonic mixing, magnetic agitation 1~
2h obtains mixed serum.
Step 5: the mixed serum to be coated uniformly on to the one side of collector titanium sheet, dry；Again by the mixed serum
It is evenly applied to the another side of collector titanium sheet, is dried；Then it is freeze-dried 6~8h, the chitin base for Electro Sorb is made
Biomass carbon double-face electrode piece.
The conductive agent is graphite.
Implementation case 2
A kind of chitin based biomass charcoal double-face electrode piece and preparation method thereof for Electro Sorb.It is made described in the present embodiment
The step of Preparation Method, is:
Step 1: chitin powder is cleaned 3~5 times with deionized water, filter, dry 2~3h at 60 DEG C~80 DEG C,
Screening obtains the chitin powder that partial size is less than 0.0385mm；The chitin powder by partial size less than 0.0385mm is placed in again
In quartz boat, under the conditions of nitrogen atmosphere, 430~470 DEG C is warming up to the rate of 5~10 DEG C/min, 1~2h is kept the temperature, obtains
Pre- charing powder.
Step 2: pressing the pre- charing powder: the mass ratio of potassium hydroxide powder is 3.5~4.5: 1, by the pre- charing
Powder and potassium hydroxide powder mixing, obtain mixed-powder；The mixed-powder is placed in vacuum tube furnace, with 5~10 DEG C/
The rate of min is warming up to 825 DEG C~875 DEG C, keeps the temperature 2~3h, obtains biomass carbon powder I.
Step 3: being 0.08~0.12Kg/L by solid-to-liquid ratio, it is 10% that mass fraction, which is added, in the biomass carbon powder I
HCl solution in, stir 10~15min, stand 1~2h；It is cleaned 2~4 times with deionized water again, dries, obtain biomass carbon
Powder II.
Step 4: pressing conductive agent: the biomass carbon powder II: the mass ratio 1 of Kynoar: (16~19): (2.5
~3.5), the conductive agent, the biomass carbon powder II and the Kynoar are mixed, obtain mixture；Again by solid
Liquor ratio is 0.15~0.2Kg/L, the mixture is dissolved in dimethyl acetamide, 10~15min of ultrasonic mixing, magnetic agitation
1~2h obtains mixed serum.
Step 5: the mixed serum to be coated uniformly on to the one side of collector titanium sheet, dry；Again by the mixed serum
It is evenly applied to the another side of collector titanium sheet, is dried；Then it is freeze-dried 6~8h, the chitin base for Electro Sorb is made
Biomass carbon double-face electrode piece.
The conductive agent is carbon fiber.
Implementation case 3
A kind of chitin based biomass charcoal double-face electrode piece and preparation method thereof for Electro Sorb.It is made described in the present embodiment
The step of Preparation Method, is:
Step 1: chitin powder is cleaned 3~5 times with deionized water, filter, dry 2~3h at 60 DEG C~80 DEG C,
Screening obtains the chitin powder that partial size is less than 0.0385mm；The chitin powder by partial size less than 0.0385mm is placed in again
In quartz boat, under the conditions of nitrogen atmosphere, 460~500 DEG C is warming up to the rate of 5~10 DEG C/min, 1~2h is kept the temperature, obtains
Pre- charing powder.
Step 2: pressing the pre- charing powder: the mass ratio of potassium hydroxide powder is 4~5: 1, by the pre- charing powder
It is mixed with potassium hydroxide powder, obtains mixed-powder；The mixed-powder is placed in vacuum tube furnace, with 5~10 DEG C/min
Rate be warming up to 850 DEG C~900 DEG C, keep the temperature 2~3h, obtain biomass carbon powder I.
Step 3: being 0.08~0.12Kg/L by solid-to-liquid ratio, it is 10% that mass fraction, which is added, in the biomass carbon powder I
HCl solution in, stir 10~15min, stand 1~2h；It is cleaned 2~4 times with deionized water again, dries, obtain biomass carbon
Powder II.
Step 4: pressing conductive agent: the biomass carbon powder II: the mass ratio 1 of Kynoar: (17~20): (3~
4), the conductive agent, the biomass carbon powder II and the Kynoar are mixed, obtain mixture；Solid-to-liquid ratio is pressed again
For 0.15~0.2Kg/L, the mixture is dissolved in dimethyl acetamide, 10~15min of ultrasonic mixing, magnetic agitation 1~
2h obtains mixed serum.
Step 5: the mixed serum to be coated uniformly on to the one side of collector titanium sheet, dry；Again by the mixed serum
It is evenly applied to the another side of collector titanium sheet, is dried；Then it is freeze-dried 6~8h, the chitin base for Electro Sorb is made
Biomass carbon double-face electrode piece.
The conductive agent is one of carbon nanotube, graphene and acetylene black.
Present embodiment has the positive effect that compared with the existing technology:
(1) present embodiment is first carbonized in advance using chitin powder as raw material, then by KOH modification and is kept
The temperature of reaction system makes it carry out complete carbonization reaction, and as shown in FIG. 1, FIG. 1 is implementations for obtained biomass carbon powder II
A kind of SEM figure of biomass carbon II prepared by example 2；It will be seen from figure 1 that II structure bulk multi-hole of biomass carbon obtained, has
Biggish specific surface area, pore channel is unobstructed, is conducive to interionic transmission in Electro Sorb.It is common in binder and conductive agent
Effect is lower to be coated in collector titanium sheet, so that the chitin based biomass charcoal double-face electrode piece for Electro Sorb be made, is produced
Simple process and at low cost.
(2) chitin that present embodiment uses is natural material, and rich reserves are nontoxic.Biomass charcoal powder
The unique three-dimensional self supporting structure in end II can effectively overcome powder carbon-based material in preparing electrode process due to binder etc.
The defects of electrode internal resistance increase caused by adding, the blocking of Carbon Materials duct, capacitive property decline, i.e., prepared by present embodiment
The chitin based biomass charcoal double-face electrode piece for Electro Sorb electrode internal resistance is smaller, Carbon Materials duct is unobstructed and capacitive character
It can be higher.
(3) present embodiment during the preparation process, in addition to prepared by biomass carbon powder I, remaining at normal temperature into
Row, energy consumption are lower low with production cost.The electricity of the prepared chitin based biomass charcoal double-face electrode piece for Electro Sorb is inhaled
Attached efficiency is significantly increased than single-side electrode.
(4) the chitin based biomass charcoal double-face electrode piece for Electro Sorb of present embodiment preparation is used for waste water
Middle metal adsorption and sea water desalination are as shown in Fig. 2, Fig. 2 is a kind of chitin for Electro Sorb that Examples 1 to 3 is prepared respectively
The using renderings of based biomass charcoal double-face electrode piece；As can be seen from Figure 2: prepared three kinds are used for the chitin of Electro Sorb
Based biomass charcoal electrode slice adsorption effect in Electro Sorb desalination processes is good, and capacitance is high, and the first for Electro Sorb prepared
Shell element based biomass charcoal double-face electrode piece is applied widely suitable for water process of different nature.
Therefore, the production cost of present embodiment is low, the prepared chitin based biomass charcoal for Electro Sorb
Double-face electrode plate electrode internal resistance is small, capacitance is high and absorption property is good, the processing suitable for different quality.
Claims (7)
1. a kind of preparation method of the chitin based biomass charcoal double-face electrode piece for Electro Sorb, it is characterised in that the preparation
The step of method, is:
Step 1: chitin powder is cleaned 3~5 times with deionized water, filter, dry 2~3h, sieve at 60 DEG C~80 DEG C
Point, obtain the chitin powder that partial size is less than 0.0385mm；The chitin powder by partial size less than 0.0385mm is placed in stone again
Ying Zhouzhong is warming up to 400~500 DEG C with the rate of 5~10 DEG C/min, keeps the temperature 1~2h, obtain pre- under the conditions of nitrogen atmosphere
Carbonize powder；
Step 2: pressing the pre- charing powder: the mass ratio of potassium hydroxide powder is 3~5: 1, by the pre- charing powder and hydrogen
The mixing of potassium oxide powder, obtains mixed-powder；The mixed-powder is placed in vacuum tube furnace, with the speed of 5~10 DEG C/min
Rate is warming up to 800 DEG C~900 DEG C, keeps the temperature 2~3h, obtains biomass carbon powder I；
Step 3: being 0.08~0.12Kg/L by solid-to-liquid ratio, it is 10% that mass fraction, which is added, in the biomass carbon powder I
In HCl solution, 10~15min is stirred, stands 1~2h；It is cleaned 2~4 times with deionized water again, dries, obtain biomass charcoal powder
End II；
Step 4: conductive agent: the biomass carbon powder II: the mass ratio 1 of Kynoar: (15~20): (2~4) is pressed, it will
The conductive agent, the biomass carbon powder II and Kynoar mixing, obtain mixture；It is again 0.15 by solid-to-liquid ratio
The mixture is dissolved in dimethyl acetamide by~0.2Kg/L, 10~15min of ultrasonic mixing, and 1~2h of magnetic agitation is obtained
Mixed serum；
Step 5: the mixed serum to be coated uniformly on to the one side of collector titanium sheet, dry；It is again that the mixed serum is uniform
Another side coated on collector titanium sheet, drying；Then it is freeze-dried 6~8h, the chitin base biology for Electro Sorb is made
Matter charcoal double-face electrode piece.
2. the preparation method of the chitin based biomass charcoal double-face electrode piece according to claim 1 for Electro Sorb,
It is characterized in that purity >=95% of the chitin powder, the partial size < 0.05mm of chitin powder.
3. the preparation method of the chitin based biomass charcoal double-face electrode piece according to claim 1 for Electro Sorb,
It is characterized in that purity >=99% of the potassium hydroxide powder；The partial size < 0.1mm of potassium hydroxide powder.
4. the preparation method of the chitin based biomass charcoal double-face electrode piece according to claim 1 for Electro Sorb,
It is characterized in that purity >=99.5% of the Kynoar powder, the partial size < 0.1mm of Kynoar powder.
5. the preparation method of the chitin based biomass charcoal double-face electrode piece according to claim 1 for Electro Sorb,
It is characterized in that the conductive agent is one of graphite, carbon fiber, carbon nanotube, graphene and acetylene black.
6. the preparation method of the chitin based biomass charcoal double-face electrode piece according to claim 1 for Electro Sorb,
The average coating thickness for being characterized in that the coating is 0.25~0.3mm.
7. a kind of chitin based biomass charcoal double-face electrode piece for Electro Sorb, it is characterised in that the first for Electro Sorb
Shell element based biomass charcoal double-face electrode piece be any one of according to claim 1~6 described in the chitin for Electro Sorb
The chitin based biomass charcoal double-face electrode piece of Electro Sorb is used for prepared by the preparation method of based biomass charcoal double-face electrode piece.
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| CN110372067A (en) * | 2019-06-05 | 2019-10-25 | 清华大学 | A kind of flowing electrode and its application |
| CN111573792A (en) * | 2019-08-08 | 2020-08-25 | 湖南大学 | Preparation method of capacitive deionization electrode active material, capacitive deionization electrode and application of capacitive deionization electrode |
| CN111575014A (en) * | 2020-06-08 | 2020-08-25 | 中国环境科学研究院 | Soil conditioner based on composite biochar |
| CN115571954A (en) * | 2022-11-18 | 2023-01-06 | 中国科学院合肥物质科学研究院 | Capacitive deionization adsorption electrode and preparation method thereof |
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| 张婉春: "生物质碳基复合电极的制备及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 * |
| 曾毓群，李宝华，周鹏伟，康飞宇，陈立泉: "流延涂布法制备活性炭电极膜片的超级电容器", 《新型炭材料》 * |
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| CN111573792A (en) * | 2019-08-08 | 2020-08-25 | 湖南大学 | Preparation method of capacitive deionization electrode active material, capacitive deionization electrode and application of capacitive deionization electrode |
| CN111575014A (en) * | 2020-06-08 | 2020-08-25 | 中国环境科学研究院 | Soil conditioner based on composite biochar |
| CN115571954A (en) * | 2022-11-18 | 2023-01-06 | 中国科学院合肥物质科学研究院 | Capacitive deionization adsorption electrode and preparation method thereof |
| CN115571954B (en) * | 2022-11-18 | 2023-03-07 | 中国科学院合肥物质科学研究院 | Capacitive deionization adsorption electrode and preparation method thereof |
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