CN106000319B - Remove the sorbing material of trace arsenic and its minimizing technology to trace arsenic in water body in water body - Google Patents
Remove the sorbing material of trace arsenic and its minimizing technology to trace arsenic in water body in water body Download PDFInfo
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- CN106000319B CN106000319B CN201610627285.0A CN201610627285A CN106000319B CN 106000319 B CN106000319 B CN 106000319B CN 201610627285 A CN201610627285 A CN 201610627285A CN 106000319 B CN106000319 B CN 106000319B
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- graphene oxide
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The sorbing material of trace arsenic and its minimizing technology to trace arsenic in water body in water body are removed the invention discloses a kind of, sorbing material, it is prepared as follows obtaining, graphene oxide dispersion and poly-vinyl alcohol solution are mixed, then graphene oxide membrane is obtained through vacuum filtration, graphene film most is made through hydrazine hydrate reduction afterwards, which is sorbing material.When removing trace arsenic in water body, the concentration of arsenic in staying water is allocated as 0.1 ~ 5mg/L, and it is 29 to adjust water pH value, then adds in aforementioned sorbing material and adsorb 12 hours or more, that is, realize Trace Arsenic in Water（Ⅲ）Removal；The additive amount of sorbing material is 0.1g/L ~ 0.4g/L.The sorbing material graphene film of gained of the invention is to Trace Arsenic in Water（Ⅲ）With higher removal efficiency, more than 99% is reached as high as.
Description
Technical field
The present invention relates to the removals of arsenic in water body, and in particular to a kind of sorbing material of trace arsenic and its right of removing in water body
The minimizing technology of trace arsenic, belongs to water-treatment technology field in water body.
Background technology
Arsenic（Ⅲ）One of element most strong as toxicity, is widely present in natural water and the drinking water of the mankind, to people
Class health and ecological environment constitute a serious threat, thus by people's extensive concern.The newest regulation drink of United States environmental protection agency
It must not be higher than 10ppb with arsenic concentration in water.How effectively to eradicate arsenic in water body seems extremely important.Traditional arsenic minimizing technology master
There are oxidizing process, the precipitation method, flocculence, ion-exchange, hyperfiltration, absorption method etc., wherein absorption method is due to simple, high
The advantages that imitating, is cheap is paid attention to by people.Although conventional sorbing material such as activated carbon, flyash, mineral etc. can go to remove water
Middle arsenic（Ⅲ）, but be difficult to eradicate Trace Arsenic in Water（Ⅲ）, and regenerability is poor.Therefore, searching can effectively remove trace in water
The sorbing material of amount arsenic is the target that people pursue.
Graphene is a kind of New Two Dimensional carbon nanomaterial, has larger specific surface area（2630m2/g）With abundant π
Electronics, thus can be acted on and heavy metal ion be adsorbed, and show stronger absorption property by Lewis Acids and Bases.Together
Sample, graphene also show stronger removal efficiency to the trace arsenic in water body.However, since pi-pi accumulation acts on, in aqueous solution
In graphene easily reunite, and be difficult to recycling.Therefore, separable graphene-based composite material is researched and developed in water
The removal of trace arsenic seems particularly urgent.
Invention content
For deficiencies of the prior art, the object of the present invention is to provide a kind of suctions for removing trace arsenic in water body
Enclosure material and its minimizing technology to trace arsenic in water body, the present invention can efficiently remove Trace Arsenic in Water.
The technical proposal of the invention is realized in this way：
The sorbing material of trace arsenic, is prepared as follows obtaining in a kind of removal water body, by graphene oxide dispersion
It is mixed with poly-vinyl alcohol solution, then obtains graphene oxide membrane through vacuum filtration, graphene most is made through hydrazine hydrate reduction afterwards
Film, the graphene film are sorbing material.
Specific preparation process is as follows,
1）Prepare respectively a concentration of 5mg/ml graphene oxide dispersion and a concentration of 0.2 wt% polyvinyl alcohol it is molten
Liquid；
2）Graphene oxide dispersion is mixed into ultrasound with poly-vinyl alcohol solution, obtains mixed liquor, graphene oxide dispersion
It is 1 with poly-vinyl alcohol solution volume ratio：（0-4）；
3）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
4）Graphene oxide membrane is added in appropriate amount of deionized water, then adds in appropriate hydrazine hydrate in deionized water to oxygen
Graphite alkene film is restored, and obtains graphene film；
5）Graphene film is washed with deionized water to neutrality, drying box drying.
The graphene oxide dispersion is prepared as follows obtaining, and adds graphene oxide into deionized water, surpasses
Sound disperses 1 ~ 4h；The poly-vinyl alcohol solution is prepared as follows obtaining, by polyvinyl alcohol be added to 90 ~ 98 DEG C go from
In sub- water, dissolve 3 ~ 5 hours.
The method for removing trace arsenic in water body, 0.1 ~ 5mg/L is allocated as, and adjust water by the concentration of arsenic in staying water
Body pH value is 2-9, then adds in aforementioned sorbing material and adsorbs 12 hours or more, that is, realizes Trace Arsenic in Water（Ⅲ）Removal；
The additive amount of sorbing material is 0.1g/L ~ 0.4g/L.
Preferably, the concentration of arsenic is allocated as 5ppm in staying water, and it is 6 to adjust water pH value, then adds in right
It is required that any sorbing materials of 1-3 adsorb 12 hours or more, that is, realize Trace Arsenic in Water（Ⅲ）Removal.
Compared with prior art, the present invention has the advantages that：
1）The sorbing material graphene film of gained of the invention is to Trace Arsenic in Water（Ⅲ）With higher removal efficiency, highest
Up to more than 99%.
2）Sorbing material graphene film of the present invention is prepared using vacuum filtration technology and chemical reduction method, system
Standby process is simple, quick, easy to operate, can be mass-produced.
3）Appropriate polyvinyl alcohol can prevent the mutual accumulation between graphene in graphene film, to graphene nanometer sheet
There is supporting role, interlamellar spacing, exposed more adsorption sites, so as to be conducive to arsenic in graphene film interbed are increased by support
Diffusion and absorption.
Description of the drawings
Fig. 1 is the digital photograph figure of graphene film made from embodiment 4.
Fig. 2 is the section SEM figures of graphene film made from embodiment 4.
Specific embodiment
Technical scheme of the present invention is described in detail below in conjunction with the accompanying drawings.
The sorbing material of trace arsenic, is prepared as follows obtaining, graphene oxide is disperseed in present invention removal water body
Liquid and poly-vinyl alcohol solution mixing, then obtain graphene oxide membrane through vacuum filtration, graphite most are made through hydrazine hydrate reduction afterwards
Alkene film, the graphene film are sorbing material.
Specific preparation process of the invention is as follows,
1）Graphene oxide dispersion and poly-vinyl alcohol solution are prepared respectively；Wherein graphene oxide dispersion is a concentration of
5mg/ml simultaneously is prepared as follows obtaining, and adds graphene oxide into deionized water, 1 ~ 4h of ultrasonic disperse；Polyethylene
A concentration of 0.2 wt% of alcoholic solution simultaneously is prepared as follows obtaining, and polyvinyl alcohol is added in 90 ~ 98 DEG C of deionized waters, molten
Solution 3 ~ 5 hours.
2）Graphene oxide dispersion is mixed into ultrasound with poly-vinyl alcohol solution, obtains mixed liquor；Graphene oxide dispersion
It is 1 with poly-vinyl alcohol solution volume ratio：（0-4）；It is preferred that 1：（1-3）；Optimal is 1：2；
3）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
4）Will graphene oxide membrane add in appropriate amount of deionized water in, then add in appropriate hydrazine hydrate to graphene oxide membrane into
Row reduction, obtains graphene film；The purpose for adding hydrazine hydrate is for the oxygen-containing group on redox graphene surface, amount root
It is controlled according to the purpose.
5）Graphene film is washed with deionized water to neutrality, drying box drying.
The method of trace arsenic, is first configured to 0.1 ~ 5mg/L by the concentration of arsenic in staying water in present invention removal water body,
And water pH value is adjusted as 2-9, it then adds in sorbing material prepared by the present invention and adsorbs 12 hours or more, that is, realize underwater trace
Arsenic（Ⅲ）Removal；The additive amount of sorbing material is 0.1g/L ~ 0.4g/L.
Preferably, the concentration of arsenic in staying water is first formulated as 5ppm, and it is 6 to adjust water pH value, then by every
It rises water body 0.2g and adds in sorbing material absorption 12 hours or more prepared by the present invention, that is, realize Trace Arsenic in Water（Ⅴ）Removal.
With reference to specific embodiment, the present invention is further explained.
Embodiment 1
（1）It adds graphene oxide into deionized water, ultrasonic 1h obtains 5mg/ml graphene oxide dispersions；
（2）Polyvinyl alcohol is added in 95 DEG C of deionized waters, dissolves 3 hours, obtains 0.2 wt% poly-vinyl alcohol solutions；
（3）1ml graphene oxide dispersions are mixed into ultrasound with 0ml poly-vinyl alcohol solutions, i.e., the two volume ratio is 1：
0, that is, it is not added with poly-vinyl alcohol solution；
（4）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
（5）The graphene oxide membrane of above-mentioned preparation is put into 5ml deionized waters, 1ml hydrazine hydrate reductions is then added in, obtains
To graphene film；
（6）Graphene film is washed with deionized water to neutrality, drying box drying.
Embodiment 2
（1）It adds graphene oxide into deionized water, ultrasonic 2h obtains 5mg/ml graphene oxide dispersions；
（2）Polyvinyl alcohol is added in 92 DEG C of deionized waters, dissolves 3 hours, obtains 0.2 wt% poly-vinyl alcohol solutions；
（3）1ml graphene oxide dispersions are mixed into ultrasound with 1ml poly-vinyl alcohol solutions, i.e., the two volume ratio is 1：
1；
（4）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
（5）The graphene oxide membrane of above-mentioned preparation is put into 5ml deionized waters, 1ml hydrazine hydrate reductions is then added in, obtains
To graphene film；
（6）Graphene film is washed with deionized water to neutrality, drying box drying.
Embodiment 3
（1）It adds graphene oxide into deionized water, ultrasonic 2h obtains 5mg/ml graphene oxide dispersions；
（2）Polyvinyl alcohol is added in 96 DEG C of deionized waters, dissolves 4 hours, obtains 0.2 wt% poly-vinyl alcohol solutions；
（3）1ml graphene oxide dispersions are mixed into ultrasound with 2ml poly-vinyl alcohol solutions, i.e., the two volume ratio is 1：
2；
（4）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
（5）The graphene oxide membrane of above-mentioned preparation is put into 5ml deionized waters, 3ml hydrazine hydrate reductions is then added in, obtains
To graphene film；
（6）Graphene film is washed with deionized water to neutrality, drying box drying.
Embodiment 4
（1）It adds graphene oxide into deionized water, ultrasonic 4h obtains 5mg/ml graphene oxide dispersions；
（2）Polyvinyl alcohol is added in 98 DEG C of deionized waters, dissolves 4 hours, obtains 0.2 wt% poly-vinyl alcohol solutions；
（3）1ml graphene oxide dispersions are mixed into ultrasound with 3ml poly-vinyl alcohol solutions, i.e., the two volume ratio is 1：
3；
（4）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
（5）The graphene oxide membrane of above-mentioned preparation is put into 5ml deionized waters, 5ml hydrazine hydrate reductions is then added in, obtains
To graphene film；
（6）Graphene film is washed with deionized water to neutrality, drying box drying.
Fig. 1 is the digital photograph figure of graphene film made from embodiment 4.Fig. 2 is cutting for graphene film made from embodiment 4
Face SEM schemes.
Embodiment 5
（1）It adds graphene oxide into deionized water, ultrasonic 4h obtains 5mg/ml graphene oxide dispersions；
（2）Polyvinyl alcohol is added in 98 DEG C of deionized waters, dissolves 4 hours, obtains 0.2 wt% poly-vinyl alcohol solutions；
（3）1ml graphene oxide dispersions are mixed into ultrasound with 4ml poly-vinyl alcohol solutions, i.e., the two volume ratio is 1：
4；
（4）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
（5）The graphene oxide membrane of above-mentioned preparation is put into 5ml deionized waters, 4ml hydrazine hydrate reductions is then added in, obtains
To graphene film；
（6）Graphene film is washed with deionized water to neutrality, drying box drying.
In order to verify that the graphene film sorbing material prepared by the present invention removes Trace Arsenic in Water（Ⅲ）Effect：First prepare
5 parts of identical 5ppm arsenic solutions, it is 6 then to adjust its pH respectively, then in 5 parts of arsenic（Ⅲ）Embodiment 1- is sequentially added in solution
Graphene film sorbing material prepared by 5 and adsorption treatment 12 hours or more, that is, complete Trace Arsenic in Water（Ⅲ）Absorption, experiment
The results are shown in Table 1.
1 graphene film of table is to arsenic in water（Ⅲ）Removal efficiency
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Removal efficiency | 88.2% | 95.4% | 99.6% | 93.1% | 84.9% |
If not adding in polyvinyl alcohol, graphene can be accumulated, and adsorption site can be shielded, so very low.This
The purpose that invention adds in polyvinyl alcohol is exactly the interlamellar spacing in order to improve graphene film, so as to improve adsorption capacity.It is but a large amount of to add
Enter polyvinyl alcohol, excessive polyvinyl alcohol can cover the adsorption site inside graphene film, so its adsorption capacity can drop instead
It is low.Sorbing material proposed by the present invention is support effect in fact（Play the role of improve interlamellar spacing, exposed more adsorption sites,
So as to improve adsorption capacity）And coverage effect（Excessive polyvinyl alcohol can also play the role of improving interlamellar spacing, but coat big
The adsorption site of amount）Between trade-off relationship.Based on this, graphene oxide dispersion is pressed after choosing comprehensively of the present invention（It is a concentration of
5mg/ml）With poly-vinyl alcohol solution（0.2 wt% of concentration）Volume ratio is 1：0-4 is added.
The present invention has the prominent advantages that the preparation process of graphene film is simple, quick, easy to operate；The graphene film of preparation
There is higher removal efficiency to Trace Arsenic in Water.
The above embodiment of the present invention is only example to illustrate the invention, and is not the embodiment party to the present invention
The restriction of formula.For those of ordinary skill in the art, other differences can also be made on the basis of the above description
The variation and variation of form here can not be exhaustive all embodiments.It is every to belong to technical scheme of the present invention institute
The obvious changes or variations amplified out are still in the row of protection scope of the present invention.
Claims (4)
1. a kind of sorbing material for removing trace arsenic in water body, it is characterised in that：It is prepared as follows obtaining, by graphite oxide
Alkene dispersion liquid and poly-vinyl alcohol solution mixing, then obtain graphene oxide membrane, most afterwards through hydrazine hydrate reduction system through vacuum filtration
Graphene film is obtained, which is sorbing material；
Specific preparation process is as follows,
1）The graphene oxide dispersion of a concentration of 5mg/mL and the poly-vinyl alcohol solution of a concentration of 0.2 wt% are prepared respectively；
2）Graphene oxide dispersion is mixed into ultrasound with poly-vinyl alcohol solution, obtains mixed liquor, graphene oxide dispersion is with gathering
Glycohol solution volume ratio is 1：（1-3）；
3）Mixed liquor is added in Vacuum filtration device and is filtered, obtains graphene oxide membrane；
4）Graphene oxide membrane is added in appropriate amount of deionized water, then adds in appropriate hydrazine hydrate in deionized water to aoxidizing stone
Black alkene film is restored, and obtains graphene film；
5）Graphene film is washed with deionized water to neutrality, drying box drying.
2. the sorbing material of trace arsenic in removal water body according to claim 1, it is characterised in that：The graphene oxide
Dispersion liquid is prepared as follows obtaining, and adds graphene oxide into deionized water, 1 ~ 4h of ultrasonic disperse；
The poly-vinyl alcohol solution is prepared as follows obtaining, and polyvinyl alcohol is added in 90 ~ 98 DEG C of deionized waters, dissolving
3 ~ 5 hours.
3. remove the method for trace arsenic in water body, it is characterised in that：The concentration of arsenic in staying water is allocated as 0.1 ~ 5mg/
L, and water pH value is adjusted as 2-9, any sorbing material absorption 12 hours or more of claim 1-2 is then added in, i.e.,
Realize Trace Arsenic in Water（Ⅲ）Removal；The additive amount of sorbing material is 0.1g/L ~ 0.4g/L.
4. remove the method for trace arsenic in water body, it is characterised in that：The concentration of arsenic in staying water is allocated as 5ppm, and adjust
It is 6 to save water pH value, then adds in any sorbing materials of claim 1-2 and adsorbs 12 hours or more, that is, realizes in water
Trace arsenic（Ⅲ）Removal；The additive amount of sorbing material is 0.1g/L ~ 0.4g/L.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108083377A (en) * | 2017-12-25 | 2018-05-29 | 中国科学院合肥物质科学研究院 | A kind of method for reducing heavy metal arsenic toxicity |
| CN108178127A (en) * | 2018-02-27 | 2018-06-19 | 宣城亨旺新材料有限公司 | The minimizing technology of arsenic in hydrofluoric acid |
| CN109081430A (en) * | 2018-09-17 | 2018-12-25 | 中车环境科技有限公司 | It can accelerate the preparation method of the reproducibility graphene oxide Modified Membrane of water treatment procedure |
| CN111519044A (en) * | 2020-05-19 | 2020-08-11 | 福州大学 | Method for preparing simple substance arsenic by chemical reduction of sodium arsenate |
| CN115178224B (en) * | 2022-05-06 | 2023-08-01 | 河南工程学院 | Nitrogen-doped hydrothermal carbon/graphene composite membrane and preparation method and application thereof |
| CN115893396A (en) * | 2022-10-25 | 2023-04-04 | 哈尔滨工业大学 | Preparation method of cassava residue derived graphene oxide film |
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