CN107812511A - A kind of nano adsorption material and preparation method thereof - Google Patents
A kind of nano adsorption material and preparation method thereof Download PDFInfo
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- CN107812511A CN107812511A CN201711365377.7A CN201711365377A CN107812511A CN 107812511 A CN107812511 A CN 107812511A CN 201711365377 A CN201711365377 A CN 201711365377A CN 107812511 A CN107812511 A CN 107812511A
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- 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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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The present invention discloses a kind of nano adsorption material and preparation method thereof.Nano material of the present invention is zinc oxide/titanium oxide/graphene/magnesium aluminum double hydroxide composite, and wherein each element mol ratio is Zn：Ti：C：Mg：Al=(0.18~0.25)：(0.12~0.17)：(0.17~0.74)：(0.37~0.82)：(0.17~0.44).The present invention is high using graphene oxide composite material heat endurance, and specific surface area and total pore volume are big, and heavy metal has higher adsorbance；The shortcomings that present invention overcomes carrier pore structure single, graphene is made full use of to obtain the macroporous structure of graphene oxide after aoxidizing；The present invention prepares large hole nano sorbing material using zinc oxide, titanium oxide, graphene, magnesium aluminum double hydroxide as raw material.The large hole nano sorbing material heat endurance is higher, and specific surface area and total pore volume are big.The characteristics of preparation method of nano adsorption material provided by the invention has that technique is simple simultaneously, mild condition, and pollution is low, and energy consumption is low, prospects for commercial application is wide.
Description
Technical field
The present invention relates to field of nanometer material technology, specifically a kind of nano adsorption material and preparation method thereof.
Background technology
Nano material is the new science and technology for emerging and developing rapidly in recent years.It is in fine ceramics, medical science, the energy, ring
Applied in the fields such as border.Because nano material has larger chemism and surface energy, it is easy to combined with external atom,
Stable structure is formed, therefore is often used in making adsorbent.
Conventional nano sorbing material is using natural minerals diatomite as matrix, using the loose structure of diatomite in itself, by it
Surface zeolitization, the diatomite Zeolite composite materials with hierarchical porous structure are made.The material has certain absorption to VOCs
Ability, it is 46mg/g such as to benzene adsorbance, but the material manufacturing cycle is longer, hydrothermal reaction process high energy consumption, gas-solid in addition
Phase, which turns brilliant process, need to use the poisonous organic reagents such as ethylenediamine, have latency environment harmfulness.Also prior art utilizes industry
The characteristics of porous, the specific surface area of waste flyash are big, surface energy is high carries out recycling, prepares with multi-stage porous knot
The coal ash zeolite composite of structure.Although preparation technology is relatively easy, still need to carry out hydro-thermal reaction, high energy consumption.On in addition,
It is powder to state two kinds of materials, easily by flow perturbation in VOCs adsorption processes；And powder body material is not easily recycled processing.
Compared with dusty material, block moulding material is not easy by airflow influence, and counter-bending and fold resistance is strong, especially ceramic
Material, heat endurance is good, being capable of straight forming application.Ceramics are typically industrially made into loose structure carrier, can be greatly increased
The contact area of adsorbent and adsorbate, improve adsorption efficiency；Mass transfer can effectively extend to three dimensions, material simultaneously
It can be improved.
The content of the invention
The purpose of the present invention is to overcome to prepare in the prior art and using adsorbent pores structure list existing for VOCs adsorbents
One, course of reaction high energy consumption, easily by flow perturbation the shortcomings of, there is provided a kind of nano adsorption material and preparation method thereof.This method
Main advantage be, it is compound using zinc oxide, titanium oxide, magnesium aluminum double hydroxide using the macroporous structure of graphene oxide
Material obtains nano adsorption material.The material heavy metal has efficient absorption power.The preparation method has that technique is simple, condition
Gently, energy consumption is low, and latency environment endangers more low advantage.
To achieve the above object, a kind of nano adsorption material of the present invention, the nano material are zinc oxide/oxidation
Titanium/graphene/magnesium aluminum double hydroxide composite, wherein each element mol ratio are Zn：Ti：C：Mg：Al=(0.18~
0.25)：(0.12~0.17)：(0.17~0.74)：(0.37~0.82)：(0.17~0.44).
The each element mol ratio is Zn：Ti：C：Mg：Al=0.25：0.12：0.70：0.60：0.30.Described ZnO
Grain particle diameter is 5-10nm, TiO, TiO2Grain diameter is 5-15nm, and magnesium aluminum double hydroxide particle diameter is 0.5 μm -1.5 μm.
A kind of preparation method of nano adsorption material of the present invention, comprises the following steps：
A) solwution method synthesizing zinc oxide/titanium oxide/graphene complex：In N2By ZnO and TiO, TiO under gas shielded2It is added to
In graphene oxide solution, pH is adjusted to 9-11, then adds hydrazine hydrate solution reduction；
B) hydro-thermal method synthesizing zinc oxide/titanium oxide/graphene/magnesium aluminum double hydroxide composite：By obtained zinc oxide/oxygen
Change titanium/graphene complex suspension to mix with the aqueous solution of Magnesium dichloride hexahydrate, Aluminium chloride hexahydrate and hexa,
It is put into water heating kettle and carries out hydro-thermal reaction.
The concentration of the graphene oxide solution is 0.4-1.7mg/mL.
The mass percent concentration of the hydrazine hydrate solution is 20-40%, and addition is 15-25mL/1g graphene oxides.
The reaction temperature for adding hydrazine hydrate solution reduction is 80-100 DEG C.
The concentration of aqueous solution of the Magnesium dichloride hexahydrate is 0.05-0.33mmol/mL.
The temperature for being put into progress hydro-thermal reaction in water heating kettle is 80-120 DEG C, reaction time 10-14h.
A kind of nano adsorption material of the present invention and preparation method thereof, its advantage is：Instant invention overcomes powder
Body Zeolite composite materials are easily by flow perturbation, and the shortcomings of stability difference, the graphene oxide composite material heat endurance is high, specific surface area
Big with total pore volume, heavy metal has higher adsorbance；The shortcomings that present invention overcomes carrier pore structure single, makes full use of
The macroporous structure of graphene oxide is obtained after graphene oxidation；The present invention is with zinc oxide, titanium oxide, graphene, the double hydrogen-oxygens of magnalium
Compound is raw material, prepares large hole nano sorbing material.The large hole nano sorbing material heat endurance is higher, specific surface area and total
Pore volume is big.The preparation method of nano adsorption material provided by the invention has that technique is simple simultaneously, mild condition, and pollution is low,
The characteristics of energy consumption is low, prospects for commercial application are wide.
Embodiment
Embodiment 1
A kind of nano adsorption material of the present invention, the nano material are the double hydrogen-oxygens of zinc oxide/titanium oxide/graphene/magnalium
Compound composite, wherein each element mol ratio are Zn：Ti：C：Mg：Al=0.25：0.12：0.70：0.60：0.30；It is described
ZnO particle particle diameter is 5nm, TiO, TiO2Grain diameter is 5nm, and magnesium aluminum double hydroxide particle diameter is 0.5 μm.
A kind of preparation method of nano adsorption material of the present invention, comprises the following steps：
A) solwution method synthesizing zinc oxide/titanium oxide/graphene complex：In N2By ZnO and TiO, TiO under gas shielded2It is added to
In graphene oxide solution, pH is adjusted to 9, then adds hydrazine hydrate solution reduction；
B) hydro-thermal method synthesizing zinc oxide/titanium oxide/graphene/magnesium aluminum double hydroxide composite：By obtained zinc oxide/oxygen
Change titanium/graphene complex suspension to mix with the aqueous solution of Magnesium dichloride hexahydrate, Aluminium chloride hexahydrate and hexa,
It is put into water heating kettle and carries out hydro-thermal reaction；The concentration of graphene oxide solution is 0.4mg/mL；The quality percentage of hydrazine hydrate solution
Specific concentration is 20%, and addition is 15-25mL/1g graphene oxides；The reaction temperature for adding hydrazine hydrate solution reduction is 80 DEG C；
The concentration of aqueous solution of Magnesium dichloride hexahydrate is 0.05mmol/mL.
Embodiment 2
A kind of nano adsorption material of the present invention, the nano material are the double hydrogen-oxygens of zinc oxide/titanium oxide/graphene/magnalium
Compound composite, wherein each element mol ratio are Zn：Ti：C：Mg：Al=0.18：0.12：0.17：0.37：0.17；ZnO
Grain particle diameter is 10nm, TiO, TiO2Grain diameter is 15nm, and magnesium aluminum double hydroxide particle diameter is 1.5 μm.
A kind of preparation method of nano adsorption material of the present invention, comprises the following steps：
A) solwution method synthesizing zinc oxide/titanium oxide/graphene complex：In N2By ZnO and TiO, TiO under gas shielded2It is added to
In graphene oxide solution, pH is adjusted to 11, then adds hydrazine hydrate solution reduction；
B) hydro-thermal method synthesizing zinc oxide/titanium oxide/graphene/magnesium aluminum double hydroxide composite：By obtained zinc oxide/oxygen
Change titanium/graphene complex suspension to mix with the aqueous solution of Magnesium dichloride hexahydrate, Aluminium chloride hexahydrate and hexa,
It is put into water heating kettle and carries out hydro-thermal reaction；The concentration of graphene oxide solution is 1.7mg/mL；The quality percentage of hydrazine hydrate solution
Specific concentration is 40%, and addition is 25mL/1g graphene oxides；The reaction temperature for adding hydrazine hydrate solution reduction is 100 DEG C；Six
The concentration of aqueous solution of hydrated magnesium chloride is 0.33mmol/mL.
Embodiment 3
A kind of nano adsorption material of the present invention, the nano material are the double hydrogen-oxygens of zinc oxide/titanium oxide/graphene/magnalium
Compound composite, wherein each element mol ratio are Zn：Ti：C：Mg：Al=0.20：0.15：0.65：0.75：0.40；It is described
ZnO particle particle diameter is 8nm, TiO, TiO2Grain diameter is 12nm, and magnesium aluminum double hydroxide particle diameter is 1.2 μm.
A kind of preparation method of nano adsorption material of the present invention, comprises the following steps：
A) solwution method synthesizing zinc oxide/titanium oxide/graphene complex：In N2By ZnO and TiO, TiO under gas shielded2It is added to
In graphene oxide solution, pH is adjusted to 10, then adds hydrazine hydrate solution reduction；
B) hydro-thermal method synthesizing zinc oxide/titanium oxide/graphene/magnesium aluminum double hydroxide composite：By obtained zinc oxide/oxygen
Change titanium/graphene complex suspension to mix with the aqueous solution of Magnesium dichloride hexahydrate, Aluminium chloride hexahydrate and hexa,
It is put into water heating kettle and carries out hydro-thermal reaction；The concentration of graphene oxide solution is 0.4-1.7mg/mL；The quality of hydrazine hydrate solution
Percent concentration is 30%, and addition is 20mL/1g graphene oxides；The reaction temperature for adding hydrazine hydrate solution reduction is 90
℃；The concentration of aqueous solution of Magnesium dichloride hexahydrate is 0.30mmol/mL.
Claims (9)
- A kind of 1. nano adsorption material, it is characterised in that：The nano material is the double hydrogen of zinc oxide/titanium oxide/graphene/magnalium Oxide composite, wherein each element mol ratio are Zn：Ti：C：Mg：Al=(0.18~0.25)：(0.12~0.17)： (0.17~0.74)：(0.37~0.82)：(0.17~0.44).
- A kind of 2. nano adsorption material as claimed in claim 1, it is characterised in that：The each element mol ratio is Zn：Ti：C： Mg：Al=0.25：0.12：0.70：0.60：0.30.
- A kind of 3. nano adsorption material as claimed in claim 2, it is characterised in that：The ZnO particle particle diameter is 5-10nm, TiO, TiO2Grain diameter is 5-15nm, and magnesium aluminum double hydroxide particle diameter is 0.5 μm -1.5 μm.
- A kind of 4. preparation method of nano adsorption material as claimed in claim 3, it is characterised in that：Comprise the following steps：A) it is molten Liquid method synthesizing zinc oxide/titanium oxide/graphene complex：In N2By ZnO and TiO, TiO under gas shielded2It is added to graphene oxide In solution, pH is adjusted to 9-11, then adds hydrazine hydrate solution reduction；B) hydro-thermal method synthesizing zinc oxide/titanium oxide/graphene/ Magnesium aluminum double hydroxide composite：By obtained zinc oxide/titanium oxide/graphene complex suspension and six chloride hydrates The aqueous solution mixing of magnesium, Aluminium chloride hexahydrate and hexa, is put into water heating kettle and carries out hydro-thermal reaction.
- A kind of 5. preparation method of nano adsorption material as claimed in claim 4, it is characterised in that：The graphene oxide solution Concentration be 0.4-1.7mg/mL.
- A kind of 6. preparation method of nano adsorption material as claimed in claim 4, it is characterised in that：The matter of the hydrazine hydrate solution Amount percent concentration is 20-40%, and addition is 15-25mL/1g graphene oxides.
- A kind of 7. preparation method of nano adsorption material as claimed in claim 4, it is characterised in that：The addition hydrazine hydrate solution The reaction temperature of reduction is 80-100 DEG C.
- A kind of 8. preparation method of nano adsorption material as claimed in claim 4, it is characterised in that：The Magnesium dichloride hexahydrate Concentration of aqueous solution is 0.05-0.33mmol/mL.
- A kind of 9. preparation method of nano adsorption material as claimed in claim 4, it is characterised in that：It is described to be put into water heating kettle The temperature of water-filling thermal response is 80-120 DEG C, reaction time 10-14h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108671904A (en) * | 2018-05-13 | 2018-10-19 | 宁波革创新材料科技有限公司 | A kind of compound material for water treatment of porous material loading |
| CN108855000A (en) * | 2018-06-25 | 2018-11-23 | 合肥艾飞新材料有限公司 | A kind of preparation method of nano adsorption material |
| CN109277074A (en) * | 2018-09-29 | 2019-01-29 | 苏州金宏气体股份有限公司 | A kind of preparation method of metal ion adsorption material |
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| CN103127907A (en) * | 2011-12-05 | 2013-06-05 | 中国科学技术大学 | Nanometer adsorption material and preparation method thereof |
| CN106799207A (en) * | 2017-02-24 | 2017-06-06 | 马鞍山纽泽科技服务有限公司 | A kind of adsorbent for heavy metal and its preparation technology |
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2017
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| CN103127907A (en) * | 2011-12-05 | 2013-06-05 | 中国科学技术大学 | Nanometer adsorption material and preparation method thereof |
| CN102941042A (en) * | 2012-10-25 | 2013-02-27 | 北京理工大学 | Graphene/metal oxide hybrid aerogel, preparation method and applications thereof |
| CN106799207A (en) * | 2017-02-24 | 2017-06-06 | 马鞍山纽泽科技服务有限公司 | A kind of adsorbent for heavy metal and its preparation technology |
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| LÜ MEIJIAO等: ""Applications of graphene-based materials in environmental protection and detection"", 《CHINESE SCIENCE BULLETIN》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108671904A (en) * | 2018-05-13 | 2018-10-19 | 宁波革创新材料科技有限公司 | A kind of compound material for water treatment of porous material loading |
| CN108671904B (en) * | 2018-05-13 | 2021-10-26 | 宁波革创新材料科技有限公司 | Composite water treatment material loaded by porous material |
| CN108855000A (en) * | 2018-06-25 | 2018-11-23 | 合肥艾飞新材料有限公司 | A kind of preparation method of nano adsorption material |
| CN109277074A (en) * | 2018-09-29 | 2019-01-29 | 苏州金宏气体股份有限公司 | A kind of preparation method of metal ion adsorption material |
| CN109277074B (en) * | 2018-09-29 | 2021-10-15 | 苏州金宏气体股份有限公司 | Preparation method of metal ion adsorption material |
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