CN107585771A - A kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template - Google Patents
A kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template Download PDFInfo
- Publication number
- CN107585771A CN107585771A CN201710434875.6A CN201710434875A CN107585771A CN 107585771 A CN107585771 A CN 107585771A CN 201710434875 A CN201710434875 A CN 201710434875A CN 107585771 A CN107585771 A CN 107585771A
- Authority
- CN
- China
- Prior art keywords
- pnipam
- silicon dioxide
- template
- hollow microsphere
- prepared
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Manufacturing Of Micro-Capsules (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention is a kind of method that silicon dioxide hollow microsphere is prepared by template of PNIPAM, and it is about 32 DEG C that PNIPAM, which has minimum consolute temperature (LCST),.When less than 32 DEG C, PNIPAM is soluble in water.And when temperature is higher than 32 DEG C, PNIPAM is not soluble in water, and reunion balling-up separates out from the aqueous solution.According to PNIPAM this characteristic, the PNIPAM aqueous solution is warming up on LCST, adds TEOS, due to carrying amide group on PNIPAM side chains, TEOS can be promoted in its surface hydrolysis condensation in-situ preparation SiO2, formed using PNIPAM as core, SiO2For the core shell structure complex microsphere of shell.When temperature is reduced to below LCST, PNIPAM is dissolved in water, and is washed away from system, so as to which silicon dioxide hollow microsphere be made.
Description
Technical field
The present invention relates to the preparation field of porous nano microballoon, is specially that one kind prepares silica by template of PNIPAM
The method of hollow microsphere.
Background technology
Hollow microsphere material due to its good fluidity, specific surface area is big, density is low the features such as, so being widely used in light
The fields such as electric material, filler, catalyst carrier.Because its internal space can be applied, thus become microreactor,
Slow-released carrier, medicine controlled releasing candidate materials and obtain people to its extensive concern.And inorganic oxide hollow microsphere is because of it
The advantages that physical and chemical properties are abundant, stability is good, preparation method is simple, especially causes research interest of the people to it.
Prepare the method for Inorganic Hollow Microspheres substantially have it is following several.Microemulsion polymerization method, template, spray reaction
Deng.Template therein is the method being most frequently used to.Metal material (silver, gold etc.), metal oxide (such as aluminum oxide,
SnO2Deng), semi-conducting material and hydroxyapatite and SiO2It is the main material for synthesizing Inorganic Hollow Microspheres.And working as needs to make
It is the micella that is mainly formed with organized surfactant assemblies, block copolymer, inorganic during standby inorganic oxide hollow microsphere
(such as silver, gold) colloidal nanoparticles and polyalcohol emulsion particle are as mould material.Template prepares hollow silica
Microballoon is causing people to its extensive research interest in recent years because being most often employed.
During template prepares silicon dioxide hollow microsphere, the first step is often through to TEOS fast hydrolyzings and contracting
Gather or core shell structure particle is formed in template by LBL self-assembly method (LBL)；Again in second step with high-temperature calcination or
The chemical corrosion method of soda acid is again or organic solvent dissolution method removes the template as core, finally gives in required silica
Empty microballoon.But the procedure of this multistep synthesis is complicated, and cost is higher, and can cause the waste of the energy and the pollution of environment.
Also, other compounds or functional group that this method may be damaged in silicon dioxide granule and material as shell.
The content of the invention
It is an object of the invention to provide a kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template, with solution
The problem of being proposed in certainly above-mentioned background technology.
To achieve the above object, the present invention provides following technical scheme：One kind prepares silica by template of PNIPAM
The method of hollow microsphere, sequentially added in 10ml polymerization pipes trithiocarbonic acid fat carboxylic acid derivates DMP (0.01g, 5 × 10- 5Mol) NIPAM (0.6g, 525 × 10-5Mol), AIBN (1.6mg, 1 × 10-5) and THF 5ml mol.Vacuumize, fill N2, remove
O in polymerization pipe2, it is repeated 3 times.Polymerization pipe is sealed under vacuum, and lower reaction 5h is then stirred in 60 DEG C of oil baths.Polymerization pipe
Cooled down, opened with frozen water after taking-up, diluted with 5ml THF, filtering is then precipitated in a large amount of ether, obtains PNIPAM, 30 DEG C
It is dried in vacuo 24h.
Preferably, a kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template, take a certain amount of purified
The PNIPAM crossed is added in single port bottle, is heated to 50 DEG C, is continued for some time, and adds 1ml TEOS, under the conditions of 50 DEG C, hydrolysis
More than 24h.
Compared with prior art, the beneficial effects of the invention are as follows：One-step synthesis method, procedure is simple, effectively avoids
The waste of the energy and the pollution of environment.Meanwhile other changes that will not also damage in silicon dioxide granule and material as shell
Compound or functional group.
Embodiment
It is clearly and completely described below in conjunction with the technical scheme in the embodiment of the present invention, it is clear that described reality
It is only part of the embodiment of the present invention to apply example, rather than whole embodiments.It is general based on the embodiment in the present invention, this area
The every other embodiment that logical technical staff is obtained under the premise of creative work is not made, belong to what the present invention protected
Scope.
, it is necessary to explanation in description of the invention, the orientation of instruction such as term " vertical ", " on ", " under ", " level " or
Person's position relationship is for only for ease of the description present invention and simplifies description, rather than instruction either implies signified device or member
Part must have specific orientation, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.This
Outside, " first ", " second ", " the 3rd ", " the 4th " are only used for describing purpose, and it is not intended that indicating or implying relatively important
Property.
In description of the invention, it is also necessary to explanation, unless otherwise clear and definite regulation and limitation, term " setting ", " peace
Dress ", " connected ", " connection ", should be interpreted broadly, for example, it may be connecting or being fixedly connected or removable
Connection, or integrally connected are unloaded, can be mechanical connection or electrical connection, can be directly connected to or in
Between medium be connected, can be the connection of two element internals.For the ordinary skill in the art, can be according to specific
Situation understands the concrete meaning of above-mentioned term in the present invention.
The present invention provides a kind of technical scheme：A kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template,
Sequentially added in 10ml polymerization pipes trithiocarbonic acid fat carboxylic acid derivates DMP (0.01g, 5 × 10-5Mol) NIPAM (0.6g,
525×10-5Mol), AIBN (1.6mg, 1 × 10-5) and THF5ml mol.Vacuumize, fill N2, remove the O in polymerization pipe2, repeat 3
It is secondary.Polymerization pipe is sealed under vacuum, and lower reaction 5h is then stirred in 60 DEG C of oil baths.Polymerization pipe is cooled down after taking out with frozen water,
Open, diluted with 5ml THF, filtering is then precipitated in a large amount of ether, obtain PNIPAM, 30 DEG C of vacuum drying 24h.
Preferably, a kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template, take a certain amount of purified
The PNIPAM crossed is added in single port bottle, is heated to 50 DEG C, is continued for some time, and adds 1ml TEOS, under the conditions of 50 DEG C, hydrolysis
More than 24h.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (2)
- A kind of 1. method that silicon dioxide hollow microsphere is prepared using PNIPAM as template, it is characterised in that：In 10ml polymerization pipes Sequentially add trithiocarbonic acid fat carboxylic acid derivates DMP (0.01g, 5 × 10-5Mol) NIPAM (0.6g, 525 × 10-5Mol), AIBN (1.6mg, 1 × 10-5) and THF 5ml mol.Vacuumize, fill N2, remove the O in polymerization pipe2, it is repeated 3 times.Polymerization pipe exists Sealed under vacuum condition, lower reaction 5h is then stirred in 60 DEG C of oil baths.Polymerization pipe is cooled down after taking out with frozen water, is opened, is used 5ml THF is diluted, and filtering is then precipitated in a large amount of ether, obtains PNIPAM, 30 DEG C of vacuum drying 24h.
- 2. a kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template according to claim 1, its feature It is：Take the PNIPAM of a certain amount of purified mistake to add in single port bottle, be heated to 50 DEG C, continue for some time, add 1ml TEOS, under the conditions of 50 DEG C, hydrolyze more than 24h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710434875.6A CN107585771A (en) | 2017-06-10 | 2017-06-10 | A kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710434875.6A CN107585771A (en) | 2017-06-10 | 2017-06-10 | A kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107585771A true CN107585771A (en) | 2018-01-16 |
Family
ID=61046086
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710434875.6A Pending CN107585771A (en) | 2017-06-10 | 2017-06-10 | A kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107585771A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559950A (en) * | 2009-05-11 | 2009-10-21 | 浙江大学 | Hollow silica nanosphere and preparing method thereof |
| CN103359743A (en) * | 2013-07-12 | 2013-10-23 | 浙江大学 | Preparation method for monodisperse hollow silicon dioxide nanosphere with controllable size and shell thickness |
| CN103359746A (en) * | 2013-07-12 | 2013-10-23 | 浙江大学 | Double-layer hollow silica nanosphere and preparation method thereof |
-
2017
- 2017-06-10 CN CN201710434875.6A patent/CN107585771A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559950A (en) * | 2009-05-11 | 2009-10-21 | 浙江大学 | Hollow silica nanosphere and preparing method thereof |
| CN103359743A (en) * | 2013-07-12 | 2013-10-23 | 浙江大学 | Preparation method for monodisperse hollow silicon dioxide nanosphere with controllable size and shell thickness |
| CN103359746A (en) * | 2013-07-12 | 2013-10-23 | 浙江大学 | Double-layer hollow silica nanosphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 罗春华等: "温度和光双重敏感的含偶氮苯端基的聚N_异丙基丙烯酰胺研究", 《高分子学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101503195B (en) | Method for preparing hydrophobic SiO2 aerogel | |
| CN104087077B (en) | Phase-change heat storage insulation coating based on phase-change heat storage as well as preparation method and application of coating | |
| CN105536655A (en) | Rapid preparation method for aerogel material | |
| CN104789124A (en) | A preparing method of a stable superamphiphobic surface | |
| CN101948574A (en) | Hydrophobic chitosan film containing hydrophobic nano silicon dioxide particles and preparation method thereof | |
| CN107140606A (en) | A kind of preparation method of oxide hollow microsphere | |
| WO2021097663A1 (en) | Nano-encapsulated binary composite phase change material | |
| CN107201220B (en) | A method of improving the viscosity of liquid carbon dioxide | |
| CN103506157A (en) | Solid catalyst for synthesizing methyl ethyl carbonate and preparation method thereof | |
| CN1974404A (en) | Prepn process of nanometer titania ring | |
| CN107585771A (en) | A kind of method that silicon dioxide hollow microsphere is prepared using PNIPAM as template | |
| CN104892851A (en) | Preparation method of hollow polymer microspheres | |
| CN103183922B (en) | For the carrier of phase-change accumulation energy and phase-changing energy storage material and their preparation method | |
| CN101749926A (en) | Method for fast preparing freeze-dried gel nanometer materials | |
| CN110292920A (en) | The preparation method of the doping cerium dioxide porous bead of zirconium | |
| CN103949248B (en) | A kind of composite catalyst of coated by titanium dioxide gold nanometer cage structure and its preparation method and application | |
| CN104211071B (en) | A kind of CdSSiO 2the synthetic method of nano composite material | |
| CN108707237A (en) | A kind of universal method preparing hollow metal organic frame | |
| CN105489777B (en) | A kind of calcium titanium photovoltaic material of microcapsule structure and preparation method thereof | |
| CN104162452B (en) | A kind of method with recyclable Template preparation yolk-eggshell structure hybridization nano particle | |
| CN103991901B (en) | A kind of method utilizing mixed solvent to improve trifluoro oxygen titanium acid ammonium productive rate | |
| CN104525049B (en) | Reaction vessel and method for preparing composite material by filling polyethylene dioxythiophene | |
| CN108314022A (en) | A kind of method that the direct stripping of ionic liquid prepares graphene | |
| CN109110796A (en) | A kind of water dispersible oxide copper nanometer tube and its colloidal solution and preparation method | |
| CN103212446B (en) | Preparation method of titanium dioxide-modified sol in polymer system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180116 |
|
| WD01 | Invention patent application deemed withdrawn after publication |