CN107963633A - A kind of preparation method of silica composite nanoparticle - Google Patents
A kind of preparation method of silica composite nanoparticle Download PDFInfo
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- CN107963633A CN107963633A CN201610910335.6A CN201610910335A CN107963633A CN 107963633 A CN107963633 A CN 107963633A CN 201610910335 A CN201610910335 A CN 201610910335A CN 107963633 A CN107963633 A CN 107963633A
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- Prior art keywords
- silica composite
- composite nanoparticle
- preparation
- silicon dioxide
- small
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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
Abstract
This application discloses a kind of preparation method of silica composite nanoparticle, including step：S1, by hydrolyzing tetraethoxy orthosilane, synthesize the Nano particles of silicon dioxide of even size distribution；S2, by tetraethyl orthosilicate, ammonium hydroxide and small ethanol hybrid reaction 4~6 when；S3, add methoxy silane, when reaction 10~12 is small under a shielding gas；S4, reactant centrifugation, washing, amino modified Nano particles of silicon dioxide is obtained after dry；Nano particles of silicon dioxide, be dispersed in the mixed solution of ethanol, initiator and tetrahydrofuran by s5, adds epoxy modified polysiloxane, flow back under nitrogen protection 8~10 it is small when；S6, reactant centrifugation, washing, obtain the silica composite nanoparticle of epoxy modified polysiloxane modification after dry.Improved silica nano-particles size of the present invention is small, and preparation process is simple.
Description
Technical field
This application involves super hydrophobic material technical field, more particularly to a kind of preparation of silica composite nanoparticle
Method.
Background technology
Wetting is a kind of common interfacial phenomenon, and one of key character of the surface of solids, usually with liquid in solid
The contact angle on surface characterizes.It is super-hydrophobic to refer to that surface is more than 150 ° to the contact angle of water, the super hydrophilic contact angle referred to water
Phenomenon less than 5 °.In general, wetability is determined by the chemical composition and micro-geometry of the surface of solids, suitable surface
The surface of solids and suitable surface fine structure of fine structure and high surface free energy or low surface free energy are that generation is super close
Water and super-hydrophobic two preconditions.This kind of material obtains extensively in fields such as self-cleaning material, microfluidic device and biologies
General application.
Current super-hydrophobic and ultra-hydrophilic surface preparation process mainly has template, sol-gel process, LBL self-assembly
Method, vapour deposition process etc..These preparation processes have shortcoming, and template is limited larger by template, it is difficult to realizes large area
The preparation on surface；Sol-gel process, which generally requires the modes such as ultraviolet light, could obtain Superhydrophilic, and not be suitable for preparing
The ultra-hydrophilic surface of high molecular material, has some limitations；There are efficiency is low and complex process is asked for LBL self-assembly method
Topic；Chemical vapor infiltration shortcoming is to need high-temperature operation, and process is complex, can produce poisonous and corrosive gas.Thing
Qi-regulating phase settling apparatus is expensive, and operating technology requires height, and efficiency is low, and condition is more harsh.
Electrostatic spinning is to manufacture the spining technology of polymer fiber by applying extra electric field to polymer solution, it is fine
Diameter is tieed up between micron and nanometer.It is can continuously to prepare one of most important method of nanofiber.Electrostatic spinning system
The non-woven fabrics obtained, has the characteristics that porosity is high, specific surface area is big, fiber fine degree and homogeneity are high, these characteristics make it
There is very big application prospect in fields such as filtering material, biological medicine engineering, nanometer conductor, application of membrane.
The content of the invention
It is an object of the invention to provide a kind of preparation method of silica composite nanoparticle, to overcome the prior art
In deficiency.
To achieve the above object, the present invention provides following technical solution：
The embodiment of the present application discloses a kind of preparation method of silica composite nanoparticle, including step：
S1, by hydrolyzing tetraethoxy orthosilane, synthesize the Nano particles of silicon dioxide of even size distribution；
S2, by tetraethyl orthosilicate, ammonium hydroxide and small ethanol hybrid reaction 4~6 when；
S3, add methoxy silane, when reaction 10~12 is small under a shielding gas；
S4, reactant centrifugation, washing, amino modified Nano particles of silicon dioxide is obtained after dry；
Nano particles of silicon dioxide, be dispersed in the mixed solution of ethanol, initiator and tetrahydrofuran by s5, adds epoxy
Modified silicon oil, when reflux 8~10 is small under nitrogen protection；
S6, reactant centrifugation, washing, obtain the silica composite nanoparticle of epoxy modified polysiloxane modification after dry.
Preferably, in the preparation method of above-mentioned silica composite nanoparticle, in the step s1, silica
The diameter of nano-particle is in 100nm.
Preferably, in the preparation method of above-mentioned silica composite nanoparticle, in the step s3, the protection
Gas is nitrogen or argon gas.
Preferably, in the preparation method of above-mentioned silica composite nanoparticle, in the step s5, the initiation
Agent is AIBA.
Compared with prior art, the advantage of the invention is that：Improved silica nano-particles size of the present invention is small, prepares
Technique is simple.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that embodiment described specific material ratio, process conditions and its result are only used
In the explanation present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
(1), the preparation of epoxy modified polysiloxane
S1, by four oxosilane of prestox ring and containing hydrogen silicone oil proportionally 3:1 mixing, adds potassium hydroxide catalyst and six
Tetramethyldisiloxane end-capping reagent, when 120 DEG C of thermotonuses 5 are small；
S2, centrifugation remove catalyst；
S3, depressurize supernatant acquisition silicon oil of low hydrogen content；
Toluene, be dissolved in vinyl epoxy cyclohexane by s4, adds silicon oil of low hydrogen content, under nitrogen protection, is heated to
50 DEG C reaction 6 it is small when, be warming up to 80 DEG C reaction 1 it is small when；
S5, be removed under reduced pressure toluene, obtains epoxy modified polysiloxane.
(2), the preparation method of silica composite nanoparticle
S1, hydrolyzing tetraethoxy orthosilane, synthesize Nano particles of silicon dioxide of the size in 100nm or so that be evenly distributed；
S2, by tetraethyl orthosilicate, ammonium hydroxide and small ethanol hybrid reaction 6 when；
S3, add methoxy silane, when reaction 12 is small under nitrogen protection；
S4, reactant centrifugation, washing, amino modified Nano particles of silicon dioxide is obtained after dry；
Nano particles of silicon dioxide, be dispersed in the mixed solution of ethanol, initiator and tetrahydrofuran by s5, adds epoxy
Modified silicon oil, when reflux 10 is small under nitrogen protection；
S6, reactant centrifugation, washing, obtain the silica composite nanoparticle of epoxy modified polysiloxane modification after dry.
The present embodiment improved silica nano-particles size is small, and preparation process is simple.
(3), the preparation method of Kynoar self-cleaning film
Silica composite nanoparticle, is dispersed in the mixed of Kynoar, n,N-dimethylacetamide and acetone by s1
Close in solution, the spinning solution of 18wt% concentration, the wherein quality of silica composite nanoparticle and Kynoar is made
Than for 3:1；
S2, by electrospinning process by spinning solution electrospinning in aluminium foil surface, electrostatic spinning voltage 14KV, syringe with
The distance between aluminium foil is controlled in 15cm；
After s3, drying, the hot pressing 8s under the conditions of 150 DEG C.
In the present embodiment, the ratio that combines between the Nano particles of silicon dioxide and Kynoar of epoxy modified polysiloxane modification
It is stronger, it is not easy to which that the erosion that is immersed in water is fallen, its surface has high hydrophobic angle (162 °), low roll angle (1 °), materials'use longevity
Life length.
Embodiment 2
(1), the preparation of epoxy modified polysiloxane
S1, by four oxosilane of prestox ring and containing hydrogen silicone oil proportionally 3:1 mixing, adds potassium hydroxide catalyst and six
Tetramethyldisiloxane end-capping reagent, when 110 DEG C of thermotonuses 4 are small；
S2, centrifugation remove catalyst；
S3, depressurize supernatant acquisition silicon oil of low hydrogen content；
Toluene, be dissolved in vinyl epoxy cyclohexane by s4, adds silicon oil of low hydrogen content, under nitrogen protection, is heated to
40 DEG C reaction 6 it is small when, be warming up to 80 DEG C reaction 1.5 it is small when；
S5, be removed under reduced pressure toluene, obtains epoxy modified polysiloxane.
(2), the preparation method of silica composite nanoparticle
S1, hydrolyzing tetraethoxy orthosilane, synthesize Nano particles of silicon dioxide of the size in 100nm or so that be evenly distributed；
S2, by tetraethyl orthosilicate, ammonium hydroxide and small ethanol hybrid reaction 6 when；
S3, add methoxy silane, when reaction 12 is small under nitrogen protection；
S4, reactant centrifugation, washing, amino modified Nano particles of silicon dioxide is obtained after dry；
Nano particles of silicon dioxide, be dispersed in the mixed solution of ethanol, initiator and tetrahydrofuran by s5, adds epoxy
Modified silicon oil, when reflux 10 is small under nitrogen protection；
S6, reactant centrifugation, washing, obtain the silica composite nanoparticle of epoxy modified polysiloxane modification after dry.
The present embodiment improved silica nano-particles size is small, and preparation process is simple.
(3), the preparation method of Kynoar self-cleaning film
Silica composite nanoparticle, is dispersed in the mixed of Kynoar, n,N-dimethylacetamide and acetone by s1
Close in solution, the spinning solution of 20wt% concentration, the wherein quality of silica composite nanoparticle and Kynoar is made
Than for 2:1；
S2, by electrospinning process by spinning solution electrospinning in aluminium foil surface, electrostatic spinning voltage 13KV, syringe with
The distance between aluminium foil is controlled in 17cm；
After s3, drying, the hot pressing 8s under the conditions of 130 DEG C.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive
Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Key element.
Claims (4)
1. a kind of preparation method of silica composite nanoparticle, it is characterised in that including step：
S1, by hydrolyzing tetraethoxy orthosilane, synthesize the Nano particles of silicon dioxide of even size distribution；
S2, by tetraethyl orthosilicate, ammonium hydroxide and small ethanol hybrid reaction 4~6 when；
S3, add methoxy silane, when reaction 10~12 is small under a shielding gas；
S4, reactant centrifugation, washing, amino modified Nano particles of silicon dioxide is obtained after dry；
Nano particles of silicon dioxide, be dispersed in the mixed solution of ethanol, initiator and tetrahydrofuran by s5, adds epoxide modified
Silicone oil, when reflux 8~10 is small under nitrogen protection；
S6, reactant centrifugation, washing, obtain the silica composite nanoparticle of epoxy modified polysiloxane modification after dry.
2. the preparation method of silica composite nanoparticle according to claim 1, it is characterised in that：The step s1
In, the diameter of Nano particles of silicon dioxide is in 100nm.
3. the preparation method of silica composite nanoparticle according to claim 1, it is characterised in that：The step s3
In, the protective gas is nitrogen or argon gas.
4. the preparation method of silica composite nanoparticle according to claim 1, it is characterised in that：The step s5
In, the initiator is AIBA.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610910335.6A CN107963633A (en) | 2016-10-19 | 2016-10-19 | A kind of preparation method of silica composite nanoparticle |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110467830A (en) * | 2019-07-23 | 2019-11-19 | 北京易净星科技有限公司 | Wear-resisting hydrophobic coating and the method for preparing wear-resisting hydrophobic coating |
| CN111285895A (en) * | 2018-12-10 | 2020-06-16 | 赖荣豊 | Silicon dioxide composite particle with far infrared radiation, organic precursor thereof and application of composite particle |
| CN115974089A (en) * | 2023-02-17 | 2023-04-18 | 江苏海格新材料有限公司 | Production method of active silicon micropowder |
-
2016
- 2016-10-19 CN CN201610910335.6A patent/CN107963633A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111285895A (en) * | 2018-12-10 | 2020-06-16 | 赖荣豊 | Silicon dioxide composite particle with far infrared radiation, organic precursor thereof and application of composite particle |
| CN110467830A (en) * | 2019-07-23 | 2019-11-19 | 北京易净星科技有限公司 | Wear-resisting hydrophobic coating and the method for preparing wear-resisting hydrophobic coating |
| CN115974089A (en) * | 2023-02-17 | 2023-04-18 | 江苏海格新材料有限公司 | Production method of active silicon micropowder |
| CN115974089B (en) * | 2023-02-17 | 2023-10-20 | 江苏海格新材料有限公司 | Production method of active silicon micropowder |
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Application publication date: 20180427 |