CN110054191A - A kind of preparation method of porous silicon dioxide nano piece - Google Patents
A kind of preparation method of porous silicon dioxide nano piece Download PDFInfo
- Publication number
- CN110054191A CN110054191A CN201910327331.9A CN201910327331A CN110054191A CN 110054191 A CN110054191 A CN 110054191A CN 201910327331 A CN201910327331 A CN 201910327331A CN 110054191 A CN110054191 A CN 110054191A
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- silicon dioxide
- porous silicon
- solid
- dioxide nano
- nano piece
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of porous silicon dioxide nano piece, include the following steps: that the super absorbent polymer resin for taking appropriate certain form makes its abundant water swelling at the solid-state hydrogel of corresponding form；It is proportionally added into solid-state hydrogel, ethyl orthosilicate, the ammonium hydroxide that volumetric concentration is 10~30%, mixed solvent in the reactor, after ultrasonic, stirring, reaction forms the solid-state hydrogel solution of nano silica load；Supernatant will be outwelled after the solid-state hydrogel solution centrifugation of nano silica load, after being washed three times with dehydrated alcohol, after dry 5~48 hours to super absorbent polymer resin dehydration, by resulting porous silicon dioxide nano piece crude product at 400~800 DEG C, in N23~6 hours are calcined under atmosphere to get two-dimensional porous silica nanosheet.The present invention prepares raw material and is easy to get, and cost is relatively low, and simple process, reaction condition is mild, non-environmental-pollution, and can according to need the regulation for carrying out pore size.
Description
Technical field
The present invention relates to field of inorganic nano-material preparation, and in particular to a kind of preparation side of porous silicon dioxide nano piece
Method.
Background technique
In recent years, Development of Nano-technology is advanced fast, and nano material is in absorption, catalysis, environmental protection, load medicine, life
The fields such as science obtain extensive concern.Nanoscale porous material is to develop a kind of more rapid material in current material subject
Material has the characteristics that nano pore is more, structure is spacious, surface area is big, in light, electricity, magnetic, catalysis, biological medicine, sensing and nanometer
Engineering etc. has huge potential using value.The big, absorption with surface area and pore volume of porous silicon dioxide nano piece
Ability is strong, and the orderly characteristics such as adjustable, high mechanical strength, corrosion-resistant and good biocompatibility of cellular structure can answer extensively
For fields such as catalyst carrier, pharmaceutical carrier, biomedical imaging and chemistry, have a extensive future.That reports at present is various porous
There are different problems in the synthetic method of silica nanometer piece, such as deposit silica using graphene template, exist
It is expensive, the shortcomings that low output；Kaolinite is such as removed using heat-acid activation method, the shortcomings that there are complex process, limits two
The industrial applications of silica nanometer sheet.
Summary of the invention
To solve the above problems, preparing raw material the present invention provides a kind of preparation method of porous silicon dioxide nano piece
It is easy to get, cost is relatively low, and simple process, reaction condition is mild, non-environmental-pollution, and can according to need the tune for carrying out pore size
Control.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of preparation method of porous silicon dioxide nano piece, includes the following steps:
S1, the super absorbent polymer resin of appropriate certain form is taken to make its abundant water swelling at the solid-state of corresponding form
Hydrogel；
S2,1 parts by weight solid-state hydrogel, 15~25 parts by weight ethyl orthosilicates, 5~100 weight are added in the reactor
Ammonium hydroxide that part volumetric concentration is 10~30%, 2000~8000 parts by weight mixed solvents after 30~60min of ultrasound, stir
100min~for 24 hours, reaction forms the solid-state hydrogel solution of nano silica load；
S3, supernatant will be outwelled after the solid-state hydrogel solution centrifugation of nano silica load, is washed with dehydrated alcohol
After three times, dry 5~48 hours to the dehydration of super absorbent polymer resin to get porous silicon dioxide nano piece crude product；
S4, by porous silicon dioxide nano piece crude product at 400~800 DEG C, in N23~6 hours are calcined under atmosphere to get two
Tie up porous silicon dioxide nano piece.
Further, the super absorbent polymer resin is polyacrylate.
Further, the mixed solvent is the ratio mixing gained that water and ethyl alcohol are 2: 5 by volume.
Further, using freeze-drying or spray drying in the step S3.
The invention has the following advantages:
The present invention prepares raw material and is easy to get, and cost is relatively low, and simple process, reaction condition is mild, non-environmental-pollution, and can root
According to the regulation for needing to carry out pore size.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
A kind of preparation method of porous silicon dioxide nano piece, includes the following steps:
S1, the superabsorbent polyacrylate macromolecule resin of appropriate certain form is taken to make its abundant water swelling at phase
Answer the solid-state hydrogel of form；
S2,1 parts by weight solid-state hydrogel, 15 parts by weight ethyl orthosilicates, 5 parts by weight volumetric concentrations are added in the reactor
Ammonium hydroxide, 2000 parts by weight mixed solvents for 10% after ultrasonic 30min, stir 100min, it is negative that reaction forms nano silica
The solid-state hydrogel solution of load；Wherein, the mixed solvent is the ratio mixing gained that water and ethyl alcohol are 2: 5 by volume；
S3, supernatant will be outwelled after the solid-state hydrogel solution centrifugation of nano silica load, is washed with dehydrated alcohol
After three times, 5~48 hours are freeze-dried to the dehydration of super absorbent polymer resin to get porous silicon dioxide nano piece crude product；
S4, by porous silicon dioxide nano piece crude product at 600 DEG C, in N2Calcined under atmosphere 3~6 hours it is more to get two dimension
Hole silica nanometer piece.
Embodiment 2
A kind of preparation method of porous silicon dioxide nano piece, including the following steps:
S1, the superabsorbent polyacrylate macromolecule resin of appropriate certain form is taken to make its abundant water swelling at phase
Answer the solid-state hydrogel of form；
S2,1 parts by weight solid-state hydrogel, 25 parts by weight ethyl orthosilicates, 100 parts by weight volumes are added in the reactor
Ammonium hydroxide that concentration is 30%, 8000 parts by weight mixed solvents, after ultrasonic 60min, for 24 hours, reaction forms nano silica for stirring
The solid-state hydrogel solution of load；Wherein, the mixed solvent is the ratio mixing gained that water and ethyl alcohol are 2: 5 by volume；
S3, supernatant will be outwelled after the solid-state hydrogel solution centrifugation of nano silica load, is washed with dehydrated alcohol
After three times, 5~48 hours are spray-dried to the dehydration of super absorbent polymer resin to get porous silicon dioxide nano piece crude product；
S4, by porous silicon dioxide nano piece crude product at 800 DEG C, in N2Calcined under atmosphere 3~6 hours it is more to get two dimension
Hole silica nanometer piece.
Embodiment 3
A kind of preparation method of porous silicon dioxide nano piece, including the following steps:
S1, the superabsorbent polyacrylate macromolecule resin of appropriate certain form is taken to make its abundant water swelling at phase
Answer the solid-state hydrogel of form；
S2,1 parts by weight solid-state hydrogel, 20 parts by weight ethyl orthosilicates, 52.5 parts by weight volumes are added in the reactor
Ammonium hydroxide that concentration is 20%, 5000 parts by weight mixed solvents, after ultrasonic 45min, stir 12h, reaction forms nano silica
The solid-state hydrogel solution of load；Wherein, the mixed solvent is the ratio mixing gained that water and ethyl alcohol are 2: 5 by volume；
S3, supernatant will be outwelled after the solid-state hydrogel solution centrifugation of nano silica load, is washed with dehydrated alcohol
After three times, 5~48 hours are freeze-dried to the dehydration of super absorbent polymer resin to get porous silicon dioxide nano piece crude product；
S4, by porous silicon dioxide nano piece crude product at 800 DEG C, in N2Calcined under atmosphere 3~6 hours it is more to get two dimension
Hole silica nanometer piece.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (4)
1. a kind of preparation method of porous silicon dioxide nano piece, characterized by the following steps:
S1, the super absorbent polymer resin of appropriate certain form is taken to make its abundant water swelling at the solid-state water-setting of corresponding form
Glue；
S2,1 parts by weight solid-state hydrogel, 15~25 parts by weight ethyl orthosilicates, 5~100 parts by weight bodies are added in the reactor
Ammonium hydroxide that product concentration is 10~30%, 2000~8000 parts by weight mixed solvents, after 30~60min of ultrasound, stir 100min~
For 24 hours, reaction forms the solid-state hydrogel solution of nano silica load；
S3, supernatant will be outwelled after the solid-state hydrogel solution centrifugation of nano silica load, is washed three times with dehydrated alcohol
Afterwards, 5~48 hours are dried to the dehydration of super absorbent polymer resin to get porous silicon dioxide nano piece crude product；
S4, by porous silicon dioxide nano piece crude product at 400~800 DEG C, in N2Calcined under atmosphere 3~6 hours it is more to get two dimension
Hole silica nanometer piece.
2. a kind of preparation method of porous silicon dioxide nano piece as described in claim 1, it is characterised in that: the high water absorption
Property macromolecule resin be polyacrylate.
3. a kind of preparation method of porous silicon dioxide nano piece as described in claim 1, it is characterised in that: the mixing is molten
Agent is the ratio mixing gained that water and ethyl alcohol are 2: 5 by volume.
4. a kind of preparation method of porous silicon dioxide nano piece as described in claim 1, it is characterised in that: the step S3
It is middle to use freeze-drying or spray drying.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111992192A (en) * | 2020-09-02 | 2020-11-27 | 河北环境工程学院 | Preparation method of natural organic polymer water treatment agent |
| CN112863901A (en) * | 2021-03-03 | 2021-05-28 | 郑州航空工业管理学院 | Preparation method of supercapacitor slurry |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931718A (en) * | 2006-10-09 | 2007-03-21 | 中国科学技术大学 | Prepn process of hollow silica ball |
| CN102275939A (en) * | 2011-07-28 | 2011-12-14 | 浙江大学 | Preparation method of two-dimensional porous silica nanosheet |
-
2019
- 2019-04-20 CN CN201910327331.9A patent/CN110054191A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931718A (en) * | 2006-10-09 | 2007-03-21 | 中国科学技术大学 | Prepn process of hollow silica ball |
| CN102275939A (en) * | 2011-07-28 | 2011-12-14 | 浙江大学 | Preparation method of two-dimensional porous silica nanosheet |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111992192A (en) * | 2020-09-02 | 2020-11-27 | 河北环境工程学院 | Preparation method of natural organic polymer water treatment agent |
| CN112863901A (en) * | 2021-03-03 | 2021-05-28 | 郑州航空工业管理学院 | Preparation method of supercapacitor slurry |
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Application publication date: 20190726 |
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