CN109692667A - A kind of biomass arsenic removal material and preparation method thereof - Google Patents
A kind of biomass arsenic removal material and preparation method thereof Download PDFInfo
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- CN109692667A CN109692667A CN201910109559.0A CN201910109559A CN109692667A CN 109692667 A CN109692667 A CN 109692667A CN 201910109559 A CN201910109559 A CN 201910109559A CN 109692667 A CN109692667 A CN 109692667A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- Environmental & Geological Engineering (AREA)
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- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of biomass arsenic removal materials and preparation method thereof; using biomass fiber as substrate; arsenic removal active component Zero-valent Iron is middle layer, silica is protective layer, and Zero-valent Iron is in array distribution on biomass fiber surface, and coated with silica is in zeroth order iron surface.The diameter of biomass fiber is 5~30 μm in material of the present invention, and the partial size of nano zero valence iron is 10~100nm, silicon dioxide layer with a thickness of 20~200nm；Wherein the mass ratio of the biomass fiber and nano zero valence iron is 10~1:1, and the mass ratio of silicon dioxide layer and nano zero valence iron is 0.5~1:1.The present invention can improve the removal rate of arsenic in water body, reduce cost, reduce the pollution to environment, be a kind of rising biomass new material, have potential economic benefit, social benefit and environmental benefit, can be applied to the arsenic in removal water body.
Description
Technical field
The present invention relates to a kind of biomass arsenic removal materials and preparation method thereof, belong to biological material preparation technical field.
Background technique
Arsenic is a kind of toxic environmental contaminants, passes through the exploitation and smelting of the metal containing arsenic, burning of coal, the pesticide containing arsenic
The modes such as application, the manufacture of glass, pigment, paper are to Environment release.Arsenic is usually to exist in the form of trivalent arsenic and pentavalent arsenic,
Trivalent arsenic is often more stronger than other arsenic compound toxicity, once it is discharged into ambient enviroment, not only contaminant water, air and soil,
And can be enriched with by food chain, huge threat is constituted to human health.Currently, arsenic and inorganic arsenic chemicals have been put into state
In the carcinogenic substance list of border Agency for Research on Cancer (ARC) publication, therefore it must be removed it before wastewater treatment.Common removal
The method of arsenic has physical method, chemical method and three kinds of bioanalysis.Physical method is that will have stronger adsorption function by physical absorption
Coagulant be added in sewage, convert precipitating for arsenic, then be separated from the water out by the means such as filtering, but this method is led to
A large amount of coagulant is often needed, adsorption efficiency is lower.In contrast, bioanalysis is a kind of preferable technology of repairing effect, centipede
Grass has been applied to the arsenic-adsorbing from soil at present, but adsorption cycle is generally 1 year or so, and the time is longer.Chemical method is to administer
One of best approach of arsenic pollution, it utilize adsorbent and pollutant redox reaction, with its period it is short, it is high-efficient, warp
The advantages of Ji, reaches adsorption effect.The active charcoal of conventional adsorbent, zeolite, rice husk, grape stem, chitosan, carbon nanotube, dioxy
Change titanium nanotube etc..
Nano zero valence iron becomes due to the features such as strong, production cost is low that interact between its small in size, magnetic strong, particle
Most widely used nano particle, at the same it is also easy to reunite, significantly reduce its some surface active property.And biomass fiber, it is generation
The most abundant natural polymer in boundary has unique property and structure.Cellulose is as the most heavy of biomass fiber
One of component wanted, since its is at low cost, nontoxic, is widely used in the base of nanometer materials containing great amount of hydroxy group
Body using cotton as substrate, makes nano zero valence iron on its surface in array distribution, and because of nano zero valence iron exposure on this basis
It is easy to aoxidize in air, and porous silica has the characteristics that light-weight, stable chemical performance, it during the preparation process can be with
Easily it is coated in nano zero-valence iron surface.
The prior art has physical method and bioanalysis to what the removal of arsenic in water body used, but physical method removal efficiency is low,
The bioanalysis period is long, and in contrast, chemical method has the advantages that high-efficient, the period is short, economical, and the present invention is based on chemical method preparations
The problem of biomass arsenic removal material, effective solution physical method and bioanalysis encounter.
Summary of the invention
The purpose of the present invention is to provide a kind of biomass arsenic removal materials and preparation method thereof, to improve going for arsenic in water body
Except rate, reduce the pollution of cost, reduction to environment.
In order to solve the above technical problems, the specific technical solution that the present invention uses is as follows:
A kind of biomass arsenic removal material, it is characterised in that: in as substrate, with arsenic removal active component Zero-valent Iron being using biomass fiber
Interbed, using silica as protective layer, nano zero valence iron is in array distribution on biomass fiber surface, and coated with silica receiving
Rice zeroth order iron surface, to effectively remove the arsenic in water body.
The diameter of the biomass fiber is 5~30 μm, and the partial size of nano zero valence iron is 10~100nm, silica
Layer with a thickness of 20~200nm；The mass ratio of the biomass fiber and nano zero valence iron is 10~1:1, silicon dioxide layer
Mass ratio with nano zero valence iron is 0.5~1:1.
A kind of preparation method of biomass arsenic removal material, it is characterised in that the following steps are included:
Step 1, by NaNO3Solution and FeCl3The solute molar ratio of solution is 5~15:1 meter, and mixed solution and biomass is fine
After dimension makes it be uniformly dispersed by ultrasonic treatment, move in reaction kettle, after reacting 10~15h at 80~120 DEG C, cooling, mistake
Filter, then washed respectively 3~6 times with deionized water and absolute alcohol, loaded the biomass fiber solid of FeOOH；
Step 2, by absolute alcohol and H2The volume ratio of O is that 5~10:1 is made into alcoholic solution, will load FeOOH
After biomass fiber solid is added in the alcoholic solution, ammonium hydroxide and tetraethyl orthosilicate, the ammonium hydroxide and positive silicon are added
The volume ratio of sour tetra-ethyl ester is 10~1:1；Magnetic agitation is to uniformly rear filtering under room temperature, with deionized water and absolute alcohol point
Xi Di not be 3~6 times, obtain the fibre solid of coated silica；
Step 3 places the fibre solid of the coated silica under reducibility gas atmosphere at 300~700 DEG C
6~12h in tube furnace obtains final product, i.e. biomass arsenic removal material after cooling.
Biomass fiber in the step 1 refers to appointing in cotton fiber, ramee, tossa or cocoanut fiber
It is a kind of.
Sonication treatment time in the step 1 is 30~60min.
It is described Step 1: use deionized water and absolute alcohol in step 2 wash respectively after, need again at 30~60 DEG C
Interior drying.
The magnetic agitation time in the step 2 is 2~6h, and mixing speed is 500~1000r/min.
The Loading sequence of ammonium hydroxide and tetraethyl orthosilicate in the step 2 is first ammonium hydroxide, rear tetraethyl orthosilicate.
Reducibility gas in the step 3 is hydrogen or hydrogen-argon-mixed.
Tube furnace in the step 3 is that heating rate is 5~15 DEG C/min, and constant temperature time is 2~5h.
The present invention has beneficial effect.Preparation process of the present invention is controllable, compared with prior art, has the effect that (1)
Internal active component of the invention is nano zero valence iron, and orderly, activity and adsorptivity with higher can be removed effectively for distribution
Arsenic in water body.The preparation process of the material is controllable, can be used for the removal of arsenic in water body；(2) present invention using silica as
Covering material, have many advantages, such as it is inexpensive, safe and environmentally protective, and coat after nano zero valence iron be not easy to be oxidized；(3) this hair
The thickness of bright silicon dioxide layer of protection has porous property, makes full use of the porosity of silica, nanometer zero in nanoscale
The high surface of valence iron is supported on the surface of biomass fiber, obtained biomass arsenic removal material have removal rate it is high,
The features such as at low cost, environmentally friendly.
Specific embodiment
Combined with specific embodiments below, technical solution of the present invention is done described further below.
Embodiment 1
A) NaNO is pressed3Solution and FeCl3The solute molar ratio of solution is 8:1 meter, and mixed solution and cotton fiber are passed through ultrasound
After 35min makes it be uniformly dispersed, move in reaction kettle, cooling after reacting 11h at 100 DEG C, filtering, with deionized water and
Absolute alcohol washs 3 times respectively, dries sample at 50 DEG C, has been loaded the fibre solid of FeOOH.
B) absolute alcohol and H are pressed2It is molten to be added to alcohol by the volume ratio 7:1 of O for the fibre solid for having loaded FeOOH
After in liquid, the volume ratio that ammonium hydroxide and tetraethyl orthosilicate is added is 6:1, magnetic agitation 4h, mixing speed 600r/ under room temperature
Min, filtering, after washing 3 times respectively with deionized water and absolute alcohol, dries sample at 50 DEG C, obtains coated silica
Fibre solid.
C) under an atmosphere of hydrogen, the fibre solid of coated silica is placed at 400 DEG C 7h in tube furnace, heated up
Rate is 8 DEG C/h, constant temperature time 2h, obtains biomass arsenic removal material after cooling.
Embodiment 2
A) NaNO is pressed3Solution and FeCl3The solute molar ratio of solution is 9:1 meter, and mixed solution and ramee are passed through ultrasound
It after 40min makes it be uniformly dispersed, moves in reaction kettle, cooling after reacting 15h at 80 DEG C, filtering, with deionized water and nothing
Water-alcohol washs 4 times respectively, dries sample at 55 DEG C, has been loaded the fibre solid of FeOOH.
B) absolute alcohol and H are pressed2It is molten to be added to alcohol by the volume ratio 5:1 of O for the fibre solid for having loaded FeOOH
After in liquid, the volume ratio that ammonium hydroxide and tetraethyl orthosilicate is added is 7:1, magnetic agitation 5h, mixing speed 700r/ under room temperature
Min, filtering, after washing 4 times respectively with deionized water and absolute alcohol, dries sample at 55 DEG C, obtains coated silica
Fibre solid.
C) under hydrogen-argon-mixed atmosphere, the fibre solid of coated silica is placed in tube furnace at 600 DEG C
8h, heating rate are 5 DEG C/h, constant temperature time 3h, obtain biomass arsenic removal material after cooling.
Embodiment 3
A) NaNO is pressed3Solution and FeCl3The solute molar ratio of solution is 5:1 meter, and mixed solution and tossa are passed through ultrasound
After 60min makes it be uniformly dispersed, move in reaction kettle, cooling after reacting 10h at 110 DEG C, filtering, with deionized water and
Absolute alcohol washs 5 times respectively, dries sample at 30 DEG C, has been loaded the fibre solid of FeOOH.
B) absolute alcohol and H are pressed2It is molten to be added to alcohol by the volume ratio 9:1 of O for the fibre solid for having loaded FeOOH
After in liquid, the volume ratio that ammonium hydroxide and tetraethyl orthosilicate is added is 10:1, magnetic agitation 6h, mixing speed 500r/ under room temperature
Min, filtering, after washing 5 times respectively with deionized water and absolute alcohol, dries sample at 30 DEG C, obtains coated silica
Fibre solid.
C) under an atmosphere of hydrogen, the fibre solid of coated silica is placed at 700 DEG C 6h in tube furnace, heated up
Rate is 12 DEG C/h, constant temperature time 4h, obtains biomass arsenic removal material after cooling.
Embodiment 4
A) NaNO is pressed3Solution and FeCl3The solute molar ratio of solution is 10:1 meter, and mixed solution and cotton fiber are passed through ultrasound
It after 45min makes it be uniformly dispersed, moves in reaction kettle, cooling after reacting 12h at 95 DEG C, filtering, with deionized water and nothing
Water-alcohol washs 4 times respectively, dries sample at 45 DEG C, has been loaded the fibre solid of FeOOH.
B) absolute alcohol and H are pressed2It is molten to be added to alcohol by the volume ratio 8:1 of O for the fibre solid for having loaded FeOOH
After in liquid, the volume ratio that ammonium hydroxide and tetraethyl orthosilicate is added is 5:1, magnetic agitation 3h, mixing speed 800r/ under room temperature
Min, filtering, after washing 4 times respectively with deionized water and absolute alcohol, dries sample at 45 DEG C, obtains coated silica
Fibre solid.
C) under hydrogen-argon-mixed atmosphere, the fibre solid of coated silica is placed in tube furnace at 500 DEG C
9h, heating rate are 10 DEG C/h, constant temperature time 3h, obtain biomass arsenic removal material after cooling.
Embodiment 5
A) NaNO is pressed3Solution and FeCl3The solute molar ratio of solution is 15:1 meter, and mixed solution and cocoanut fiber are passed through ultrasound
After 50min makes it be uniformly dispersed, move in reaction kettle, cooling after reacting 10h at 120 DEG C, filtering, with deionized water and
Absolute alcohol washs 6 times respectively, dries sample at 60 DEG C, has been loaded the fibre solid of FeOOH.
B) absolute alcohol and H are pressed2The fibre solid for having loaded FeOOH is added to alcohol by the volume ratio 10:1 of O
After in solution, the volume ratio that ammonium hydroxide and tetraethyl orthosilicate is added is 1:1, magnetic agitation 4h, mixing speed 900r/ under room temperature
Min, filtering, after washing 6 times respectively with deionized water and absolute alcohol, dries sample at 60 DEG C, obtains coated silica
Fibre solid.
C) under an atmosphere of hydrogen, the fibre solid of coated silica is placed at 300 DEG C 12h in tube furnace, risen
Warm rate is 14 DEG C/h, constant temperature time 5h, obtains biomass arsenic removal material after cooling.
Embodiment 6
A) NaNO is pressed3Solution and FeCl3The solute molar ratio of solution is 12:1 meter, and mixed solution and ramee are passed through ultrasound
It after 30min makes it be uniformly dispersed, moves in reaction kettle, cooling after reacting 14h at 85 DEG C, filtering, with deionized water and nothing
Water-alcohol washs 3 times respectively, dries sample at 40 DEG C, has been loaded the fibre solid of FeOOH.
B) absolute alcohol and H are pressed2It is molten to be added to alcohol by the volume ratio 6:1 of O for the fibre solid for having loaded FeOOH
After in liquid, the volume ratio that ammonium hydroxide and tetraethyl orthosilicate is added is 3:1, magnetic agitation 6h, mixing speed 1000r/ under room temperature
Min, filtering, after washing 3 times respectively with deionized water and absolute alcohol, dries sample at 40 DEG C, obtains coated silica
Fibre solid.
C) under hydrogen-argon-mixed atmosphere, the fibre solid of coated silica is placed in tube furnace at 450 DEG C
11h, heating rate are 15 DEG C/h, constant temperature time 4h, obtain biomass arsenic removal material after cooling.
Embodiment 7
A) NaNO is pressed3Solution and FeCl3The solute molar ratio of solution is 7:1 meter, and mixed solution and tossa are passed through ultrasound
It after 45min makes it be uniformly dispersed, moves in reaction kettle, cooling after reacting 13h at 90 DEG C, filtering, with deionized water and nothing
Water-alcohol washs 4 times respectively, dries sample at 35 DEG C, has been loaded the fibre solid of FeOOH.
B) absolute alcohol and H are pressed2It is molten to be added to alcohol by the volume ratio 7:1 of O for the fibre solid for having loaded FeOOH
After in liquid, the volume ratio that ammonium hydroxide and tetraethyl orthosilicate is added is 4:1, magnetic agitation 2h, mixing speed 800r/ under room temperature
Min, filtering, after washing 4 times respectively with deionized water and absolute alcohol, dries sample at 35 DEG C, obtains coated silica
Fibre solid.
C) under an atmosphere of hydrogen, the fibre solid of coated silica is placed at 550 DEG C 10h in tube furnace, risen
Warm rate is 9 DEG C/h, constant temperature time 2h, obtains biomass arsenic removal material after cooling.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (10)
1. a kind of biomass arsenic removal material, it is characterised in that: be as substrate, with arsenic removal active component Zero-valent Iron using biomass fiber
Middle layer, using silica as protective layer, nano zero valence iron is in array distribution on biomass fiber surface, and coated with silica exists
Nano zero-valence iron surface, to effectively remove the arsenic in water body.
2. a kind of biomass arsenic removal material according to claim 1, it is characterised in that: the diameter of the biomass fiber
Be 5~30 μm, the partial size of nano zero valence iron is 10~100nm, silicon dioxide layer with a thickness of 20~200nm；The biology
The mass ratio of matter fiber and nano zero valence iron is 10~1:1, and the mass ratio of silicon dioxide layer and nano zero valence iron is 0.5~1:1.
3. a kind of preparation method of biomass arsenic removal material according to claim 1, it is characterised in that including following step
It is rapid:
Step 1, by NaNO3Solution and FeCl3The solute molar ratio of solution is 5~15:1 meter, and mixed solution and biomass is fine
After dimension makes it be uniformly dispersed by ultrasonic treatment, move in reaction kettle, after reacting 10~15h at 80~120 DEG C, cooling, mistake
Filter, then washed respectively 3~6 times with deionized water and absolute alcohol, loaded the biomass fiber solid of FeOOH；
Step 2, by absolute alcohol and H2The volume ratio of O is that 5~10:1 is made into alcoholic solution, will load the life of FeOOH
After material fibrils solid is added in the alcoholic solution, ammonium hydroxide and tetraethyl orthosilicate, the ammonium hydroxide and positive silicic acid are added
The volume ratio of tetra-ethyl ester is 10~1:1；Magnetic agitation is distinguished to uniformly rear filtering with deionized water and absolute alcohol under room temperature
Washing 3~6 times, obtains the fibre solid of coated silica；
Step 3 places the fibre solid of the coated silica under reducibility gas atmosphere at 300~700 DEG C
6~12h in tube furnace obtains final product, i.e. biomass arsenic removal material after cooling.
4. a kind of preparation method of biomass arsenic removal material according to claim 3, it is characterised in that: the step 1
In biomass fiber refer to any one of cotton fiber, ramee, tossa or cocoanut fiber.
5. a kind of preparation method of biomass arsenic removal material according to claim 3, it is characterised in that: the step 1
In sonication treatment time be 30~60min.
6. a kind of preparation method of biomass arsenic removal material according to claim 3, it is characterised in that: the step
One, it after the use deionized water in step 2 and absolute alcohol wash respectively, needs to dry in 30~60 DEG C again.
7. a kind of preparation method of biomass arsenic removal material according to claim 3, it is characterised in that the step 2
In the magnetic agitation time be 2~6h, mixing speed be 500~1000r/min.
8. a kind of preparation method of biomass arsenic removal material according to claim 3, it is characterised in that: the step 2
In ammonium hydroxide and the Loading sequence of tetraethyl orthosilicate be first ammonium hydroxide, rear tetraethyl orthosilicate.
9. a kind of preparation method of biomass arsenic removal material according to claim 3, it is characterised in that: the step 3
In reducibility gas be hydrogen or hydrogen-argon-mixed.
10. a kind of preparation method of biomass arsenic removal material according to claim 3, it is characterised in that: the step
Tube furnace in three is that heating rate is 5~15 DEG C/min, and constant temperature time is 2~5h.
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2019
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| US20060021946A1 (en) * | 2003-09-05 | 2006-02-02 | Carl Hensman | Method and material for water treatment |
| CN105776506A (en) * | 2016-05-13 | 2016-07-20 | 合肥工业大学 | Fe/C composite porous structure material as well as preparation method and application thereof |
| CN106881059A (en) * | 2017-02-04 | 2017-06-23 | 中国科学技术大学苏州研究院 | A kind of preparation method of iron/carbon composite |
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Application publication date: 20190430 |