CN109592748A - A kind of iron carbon composite and preparation method - Google Patents
A kind of iron carbon composite and preparation method Download PDFInfo
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- CN109592748A CN109592748A CN201811448251.0A CN201811448251A CN109592748A CN 109592748 A CN109592748 A CN 109592748A CN 201811448251 A CN201811448251 A CN 201811448251A CN 109592748 A CN109592748 A CN 109592748A
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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
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
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- General Chemical & Material Sciences (AREA)
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a kind of iron carbon composite and preparation method, preparation method step: in nitrogen environment, ferrous sulfate aqueous solution is uniformly mixed with carbon nanotube, obtains mixture；Reducing agent ethanol solution is added drop-wise in mixture, is stirred, with ultrapure water, centrifugation；Solid is added in chitosan-acetic acid solution, and continues to stir, is uniformly mixed, separates, the particle of diameter 4-6cm is made, obtains iron carbon composite.The invention has the benefit that iron carbon composite of the invention exists with nano-form, and specific surface area is larger, and reaction effect is good.The space structure of chitosan serves not only as the substrate of nano zero valence iron and carbon nanotube, and the reusable property of reinforcing material in the present invention.Method of the invention is easy, low in cost, and product mix effect is ideal, is not easy to be passivated, material specific surface area is big, is suitable for high concentration hard-degraded organic waste water handles.
Description
Technical field
The present invention relates to nano material synthesis technical fields, more particularly to a kind of iron carbon composite and preparation method.
Background technique
Iron/carbon micro-electrolysis technique is initially by Soviet Studies and to develop originating from or so the 60 to 70's of twentieth century
Come, in beauty, day etc., country once caused to pay attention to extensively, and there are many engineering experiences.China was from twentieth century 80 years
In generation, introduces the technology, because of the spies such as its raw material sources is extensive, cheap, high treating effect, low energy consumption, technical operation is simple and practical
Point has been applied to the pretreatment stage of the waste water such as printing and dyeing, plating, pharmacy, papermaking, petrochemical industry, and being rich in processing high concentration has
In terms of the waste water of the toxic hard-degraded substance of machine, there is unique technical advantage.
At the same time, for the variety of problems generated in application, domestic and foreign scholars are also continuously improving iron-carbon micro-electrolysis
Technique develops the various good iron/carbon micro-electrolytic materials of technical performance, so that iron/carbon micro-electrolysis technique application range is not
It is disconnected to expand, promote the progress of this treatment process.
Type about iron-carbon micro-electrolysis filler in production application at present mainly has waste iron filing filler and waste iron filing
Active carbon filler, iron copper scale filler, iron copper modified zeolite filler, ferrous manganese ore active carbon filler, iron filings flyash filler etc..These
For material greatly mostly from the byproduct generated in nature or production and living, the iron in raw material is in industrial processes mostly
Iron sheet, industrial waste iron filing, steel slag etc..Relative material itself, superiority especially cheap and easy to get, but application process send out
Existing, using iron filings and carbon dust, this isolated material of active carbon is easy to appear mixing unevenness, easily during micro-electrolysis reaction
It is hardened, passivation the problems such as.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of iron carbon composite.
A second object of the present invention is to provide a kind of preparation methods of iron carbon composite.
A kind of preparation method of iron carbon composite, comprising the following steps: in nitrogen environment, in proportion by 90-150mL
Concentration is that the ferrous sulfate aqueous solution of 0.03-0.05M is uniformly mixed with 0.5-1.5g carbon nanotube, obtains mixture；In mass ratio
For the ratio of 1:2-3, the reducing agent ethanol solution of 0.03-0.06M is added drop-wise in mixture, is stirred 20-30 minutes, use is ultrapure
Water rinses 2-4 times, centrifugation；Solid is added in the chitosan-acetic acid solution that 150-200ml mass concentration is 90%-95%,
And continue to stir, it is uniformly mixed, separates, the particle of diameter 4-6cm is made, obtains iron carbon composite.
The carbon nanotube internal diameter is 5-10nm.
The reducing agent is sodium borohydride or potassium borohydride.
The chitosan is that viscosity is 500~800mPas, deacetylation 90%.
A kind of iron carbon composite of above method preparation
The invention has the benefit that
(1) iron carbon composite of the invention exists with nano-form, and specific surface area is larger, and reaction effect is good.
(2) space structure of chitosan serves not only as the substrate of nano zero valence iron and carbon nanotube, Er Qiezeng in the present invention
The reusable property of strong material.
(3) method of the invention is easy, low in cost, and product mix effect is ideal, is not easy to be passivated, material specific surface area
Greatly, it is suitable for high concentration hard-degraded organic waste water to handle.
Detailed description of the invention
Fig. 1 is iron carbon composite pattern of the invention.
Specific embodiment
Carbon nanotube (wins space high-tech new material technology Co., Ltd in Beijing), and the source of carbon nanotube does not limit this one kind
Product, the property of other enterprise's productions carbon nanotube similar with the rich product of space high-tech new material technology Co., Ltd in Beijing,
It can be used for the present invention.
The present invention is described in further detail combined with specific embodiments below.
Embodiment 1
A kind of preparation method of iron carbon composite, comprising the following steps: in nitrogen environment, be by 120mL concentration
The ferrous sulfate aqueous solution of 0.04M is uniformly mixed with 1g carbon nanotube, obtains mixture；It is in mass ratio the ratio of 1:2, it will
The ethanol solution of sodium borohydride of 0.05M is added drop-wise in mixture, is stirred 25 minutes, with ultrapure water 3 times, centrifugation；By solid
It is added in the chitosan-acetic acid solution that 180ml mass concentration is 93%, and continues to stir, be uniformly mixed, separate, (rolling is made
Circle) diameter 4-6cm particle, obtain iron carbon composite (Fig. 1).The carbon nanotube internal diameter is 5-10nm.The chitosan is
Viscosity is 700mPas, deacetylation 90%.
Embodiment 2
A kind of preparation method of iron carbon composite, comprising the following steps: in nitrogen environment, in proportion by 90mL concentration
It is uniformly mixed for the ferrous sulfate aqueous solution of 0.05M with 0.5g carbon nanotube, obtains mixture；It is in mass ratio the ratio of 1:2.5,
The ethanol solution of sodium borohydride of 0.06M is added drop-wise in mixture, is stirred 20 minutes, with ultrapure water 2 times, centrifugation；It will consolidate
Body is added in the chitosan-acetic acid solution that 150ml mass concentration is 95%, and continues to stir, and is uniformly mixed, and is separated, and is made straight
The particle of diameter 4-6cm obtains iron carbon composite.The carbon nanotube internal diameter is 5-10nm.The chitosan is that viscosity is
500mPas, deacetylation 90%.
Embodiment 3
A kind of preparation method of iron carbon composite, comprising the following steps: in proportion that 150mL is dense in nitrogen environment
Degree is that the ferrous sulfate aqueous solution of 0.03M is uniformly mixed with 1.5g carbon nanotube, obtains mixture；It is in mass ratio the ratio of 1:3,
The potassium borohydride ethanol solution of 0.03M is added drop-wise in mixture, is stirred 30 minutes, with ultrapure water 4 times, centrifugation；It will consolidate
Body is added in the chitosan-acetic acid solution that 200ml mass concentration is 90%, and continues to stir, and is uniformly mixed, and is separated, and is made straight
The particle of diameter 4-6cm obtains iron carbon composite.The carbon nanotube internal diameter is 5-10nm.The chitosan is that viscosity is
800mPas, deacetylation 90%.
Embodiment 4
A kind of water treatment effect of iron carbon composite:
Certain destructor plant percolate waste water (abbreviation waste water A), waste water TOC value are 4875mg/L.
A kind of iron carbon composite (each 6g) prepared by embodiment 1, embodiment 2 and embodiment 3 is separately added into three burnings
It in cup, is separately added into beaker above-mentioned waste water A (300mL), adjusts pH value to 3, aeration head is added, opens aeration, reacts 1h
Afterwards, quiescent setting 0.5h takes supernatant to measure its TOC value, and the results are shown in Table 1.
The result of 1 embodiment 1 of table, embodiment 2 and embodiment 3 to wastewater treatment
| Project | TOC(mg/L) | TOC degradation rate |
| Embodiment 1 | 1189 | 75.6% |
| Embodiment 2 | 1170 | 76% |
| Embodiment 3 | 1175 | 75.9% |
Embodiment 5
A kind of iron carbon composite and conventional iron carbon material handle waste water effect:
Conventional iron carbon material: equal for 2:1 mixing in mass ratio by iron powder (partial size 0.8-1mm), active powdered carbon (120 mesh)
It is even.
Iron carbon composite and each 6g of conventional iron carbon material prepared by embodiment 1 are added separately in two beakers, to
It is separately added into beaker above-mentioned waste water A (300mL), adjusts pH to 3, aeration head is added, open aeration, after reacting 0.5h, from
Heart separation takes supernatant, measures its COD value, under similarity condition, respectively after react lh, 1.5h, 2h, 2.5h, 3h, is centrifugated
Supernatant is taken, respective TOC value is measured, the results are shown in Table 2.
Table 2: the experimental result of 1 iron carbon composite of embodiment and conventional iron carbon material processing waste water
It is reacted in 1.5h it can be seen from the processing result of above-mentioned iron carbon composite and conventional iron carbon material to waste water A,
Iron carbon composite reaction speed is significantly greater than conventional iron carbon material, and after reacting 2h, iron carbon composite TOC degradation rate is up to 75%
More than, conventional iron carbon material TOC degradation rate only 56%.This is mainly due to iron carbon composite specific surface area with higher,
Reactivity is higher, effectively prevent the generation of passivation, hardened phenomenon during the reaction, reaction efficiency is high, and the iron carbon
Contain the nano zero valence iron in composite material, the nano zero valence iron can effectively prevent electrode polarization, substantially increase electrolysis
Efficiency accelerates TOC degradation, shortens the reaction time.
The foregoing is merely presently preferred embodiments of the present invention, is merely illustrative for the purpose of the present invention, and not restrictive
's.Those skilled in the art understand that in the spirit and scope defined by the claims in the present invention many changes can be carried out to it,
It modifies or even equivalent, but falls in protection scope of the present invention.
Claims (5)
1. a kind of preparation method of iron carbon composite, which comprises the following steps: in nitrogen environment, in proportion
The ferrous sulfate aqueous solution that 90-150mL concentration is 0.03-0.05M is uniformly mixed with 0.5-1.5g carbon nanotube, must be mixed
Object；In mass ratio it is the ratio of 1:2-3, the reducing agent ethanol solution of 0.03-0.06M is added drop-wise in mixture, stirs 20-30
Minute, with ultrapure water 2-4 times, centrifugation；Solid is added to the chitosan vinegar that 150-200ml mass concentration is 90-95%
In acid solution, and continue to stir, be uniformly mixed, separates, the particle of diameter 4-6cm is made, obtains iron carbon composite.
2. according to the method described in claim 1, it is characterized in that the carbon nanotube internal diameter is 5-10nm.
3. according to the method described in claim 1, it is characterized in that the reducing agent is sodium borohydride or potassium borohydride.
4. deacetylated according to the method described in claim 1, it is characterized in that it is 500~800mPas that the chitosan, which is viscosity,
Degree 90%.
5. a kind of iron carbon composite prepared by the method for one of claim 1-4.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113003803A (en) * | 2021-03-10 | 2021-06-22 | 南京乐透思环保科技有限公司 | Iron-carbon filler containing nano treatment unit and preparation method thereof |
| CN113634589A (en) * | 2021-06-07 | 2021-11-12 | 广东石油化工学院 | Combined remediation method for composite contaminated soil by using iron-carbon-based material |
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| CN103191742A (en) * | 2013-04-11 | 2013-07-10 | 济南市供排水监测中心 | Carbon material loaded nano zero valence metal catalyst and preparation method and application thereof |
| CN104525136A (en) * | 2014-10-27 | 2015-04-22 | 湖北工程学院 | Composite material, and preparation method and application thereof |
| CN105983394A (en) * | 2015-03-05 | 2016-10-05 | 江南石墨烯研究院 | Method for preparing efficient and magnetically separable dye adsorbent |
| CN106001599A (en) * | 2016-05-27 | 2016-10-12 | 浙江工业大学 | Preparation method of multi-walled carbon nanotube/nanoscale bimetal zero-valent iron composite material |
| CN108722356A (en) * | 2018-06-11 | 2018-11-02 | 东北农业大学 | A kind of nano zero valence iron loads the preparation method of hydrophilic porous biological carbon composite |
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2018
- 2018-11-30 CN CN201811448251.0A patent/CN109592748A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191742A (en) * | 2013-04-11 | 2013-07-10 | 济南市供排水监测中心 | Carbon material loaded nano zero valence metal catalyst and preparation method and application thereof |
| CN104525136A (en) * | 2014-10-27 | 2015-04-22 | 湖北工程学院 | Composite material, and preparation method and application thereof |
| CN105983394A (en) * | 2015-03-05 | 2016-10-05 | 江南石墨烯研究院 | Method for preparing efficient and magnetically separable dye adsorbent |
| CN106001599A (en) * | 2016-05-27 | 2016-10-12 | 浙江工业大学 | Preparation method of multi-walled carbon nanotube/nanoscale bimetal zero-valent iron composite material |
| CN108722356A (en) * | 2018-06-11 | 2018-11-02 | 东北农业大学 | A kind of nano zero valence iron loads the preparation method of hydrophilic porous biological carbon composite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113003803A (en) * | 2021-03-10 | 2021-06-22 | 南京乐透思环保科技有限公司 | Iron-carbon filler containing nano treatment unit and preparation method thereof |
| CN113634589A (en) * | 2021-06-07 | 2021-11-12 | 广东石油化工学院 | Combined remediation method for composite contaminated soil by using iron-carbon-based material |
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Application publication date: 20190409 |