CN107792860A - The preparation method of silicon dioxide colloid microballoon - Google Patents
The preparation method of silicon dioxide colloid microballoon Download PDFInfo
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- CN107792860A CN107792860A CN201711228922.8A CN201711228922A CN107792860A CN 107792860 A CN107792860 A CN 107792860A CN 201711228922 A CN201711228922 A CN 201711228922A CN 107792860 A CN107792860 A CN 107792860A
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- CN
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- Prior art keywords
- silicon dioxide
- dioxide colloid
- preparation
- microballoon
- colloid microballoon
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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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
A kind of preparation method of silicon dioxide colloid microballoon, belongs to textile material field, it is characterised in that：Absolute ethyl alcohol is added in three neck round bottom flask and two kinds of solvents are well mixed by deionized water, high-speed stirred；Quickly stirred after adding ammoniacal liquor, add tetraethyl orthosilicate and alcohol mixeding liquid, after quick stirring；Reaction is straight to cause reaction to terminate；It is centrifuged at a high speed, is taken out after sample topples over supernatant through centrifuge, microballoon is diluted to scattered, then centrifugal treating again with water or ethanol, disperseed；The material not reacted completely is removed, the drying of silicon dioxide colloid microsphere solid will be obtained.The silicon dioxide microsphere surface of synthesis is smooth, and sphericity is good, size uniformity, and infrared spectrum analysis understands that the microballoon of synthesis has the characteristic feature peak of silica, and a small amount of oh group is contained on its silicon dioxide microsphere surface.
Description
Technical field
The invention belongs to textile material field, more particularly to a kind of preparation method of silicon dioxide colloid microballoon.
Background technology
At present, textile coloration is based on pigmentary color, and the generation of schemochrome need not add dyestuff or pigment, is a kind of new
The ecological bionical pigmentation pathway of grain husk, is increasingly paid close attention to by dyeing and finishing practitioner.If photonic crystal structure color is applied to weaving
It on product, can not only assign fabric bright-coloured color and luster, and lifelike effect of adding lustre to can be formed, this is also that tradition is spun
The strong supplement of fabric coloring system.At present, the method that researcher has been presented for a variety of self assembly construction colloidal crystals, mainly
There are following a few classes:（1）The sedimentation of certain force off field；（2）Vertical deposition method.
Settling methods：The monodisperse latex of extra fine quality fraction is evenly dispersed in solvent, colloid micro ball
With the evaporation of solvent, slow deposition forms periodic regular arrangement architecture on substrate under gravity.Advantage is
Preparation technology and equipment are simple, short without particular/special requirement, assembling cycle to experimental provision.Its shortcoming is that thickness is difficult to control, sample
Defect is more, is not easy to form single uniform crystal structure, it is difficult to prepare the ordered structure of large area etc..
Vertical deposition method：Substrate is disposed vertically in the assembles concentration of monodisperse latex, when the solvent evaporates, liquid
Slowly land from substrate, colloid micro ball, which by capillary force and electrostatic repulsion etc. acts on substrate both sides, to carry out accumulation and form the cycle
Property arrangement ordered structure.Advantage is that preparation technology is simple, easily adjusts photonic crystal thickness etc..Shortcoming is influenceed by substrate
Greatly, and to temperature, humidity and the external environment condition such as shockproof require higher.
The content of the invention
A kind of the present invention is intended to provide preparation method of silicon dioxide colloid microballoon.
The preparation method of silicon dioxide colloid microballoon of the present invention, comprises the following steps：
（1）Absolute ethyl alcohol and deionized water are added in three neck round bottom flask, high-speed stirred 5-10min mixes two kinds of solvents equal
It is even；（2）After addition ammoniacal liquor after quick stirring 5-10min, volume ratio is added as 1:4 tetraethyl orthosilicate and alcohol mixeding liquid,
After quick stirring 2min；（3）20h is reacted under the conditions of 25 DEG C of temperature, rotating speed 300r/min directly causes reaction to terminate；（4）Through centrifugation
Machine is centrifuged at a high speed, and after 15min, takes out after sample topples over supernatant, microballoon diluted again with water or ethanol it is scattered, then from
Heart processing, disperses；（5）Continuous operation more than 3 times, the material not reacted completely is removed, silicon dioxide colloid microballoon will be obtained and consolidated
Body is dried.
The preparation method of silicon dioxide colloid microballoon of the present invention, mixer used in the whipping process are heat collecting type
Constant temperature blender with magnetic force.
The preparation method of silicon dioxide colloid microballoon of the present invention, step（4）The rotating speed of the centrifuge is
6000r/min。
The preparation method of silicon dioxide colloid microballoon of the present invention, step（5）The drying temperature is 80 DEG C.
The preparation method of silicon dioxide colloid microballoon of the present invention, the electrical conductivity of the deionized water is 16.8M Ω
cm-1。
The preparation method of silicon dioxide colloid microballoon of the present invention, step（5）The silicon dioxide colloid microballoon
Particle diameter is 150-300nm.
The preparation method of silicon dioxide colloid microballoon of the present invention, by strictly control reaction in tetraethyl orthosilicate,
The concentration of ammoniacal liquor and water, synthesizes silicon dioxide colloid microballoon of the particle size range in 180-380nm, and single dispersing indices P DI is less than
0.08.Increase within the specific limits with the concentration of tetraethyl orthosilicate, ammoniacal liquor and water, the silicon dioxide colloid microspherulite diameter of synthesis
Increase therewith；The silicon dioxide microsphere surface of synthesis is smooth, and sphericity is good, size uniformity, and infrared spectrum analysis understands to synthesize
Microballoon there is the characteristic feature peak of silica, a small amount of oh group is contained on its silicon dioxide microsphere surface.
Embodiment
The preparation method of silicon dioxide colloid microballoon of the present invention, comprises the following steps：（1）In three neck round bottom flask
Add absolute ethyl alcohol and two kinds of solvents are well mixed by deionized water, high-speed stirred 5-10min；（2）Quickly stirred after adding ammoniacal liquor
After mixing 5-10min, volume ratio is added as 1:4 tetraethyl orthosilicate and alcohol mixeding liquid, after quickly stirring 2min；（3）In temperature
25 DEG C are spent, reaction 20h directly causes reaction to terminate under the conditions of rotating speed 300r/min；（4）It is centrifuged at a high speed through centrifuge, after 15min,
Take out after sample topples over supernatant, microballoon is diluted to scattered, then centrifugal treating again with water or ethanol, disperseed；（5）Continuous operation
More than 3 times, the material not reacted completely is removed, the drying of silicon dioxide colloid microsphere solid will be obtained.
The preparation method of silicon dioxide colloid microballoon of the present invention, mixer used in the whipping process are heat collecting type
Constant temperature blender with magnetic force.Step（4）The rotating speed of the centrifuge is 6000r/min.Step（5）The drying temperature is 80 DEG C.
The electrical conductivity of the deionized water is 16.8M Ω cm-1.Step（5）The particle diameter of the silicon dioxide colloid microballoon is 150-
300nm.Ammoniacal liquor plays catalytic action in the reaction, can accelerate the hydrolysis rate of tetraethyl orthosilicate, when other reaction conditions are constant
When, by the concentration for changing catalyst ammonia water（0.278-0.65mol/L）, Study of Catalyst ammonia concn is to silicon dioxide colloid
The influence of microspherulite diameter and its monodispersity.As ammonia concn from 0.278mol/L increases to 0.65mol/L, the dioxy of synthesis
SiClx colloid micro ball particle diameter increases to 365nm by 206nm.The increase of ammonia concn in reaction system, has greatly accelerated positive silicic acid
The hydrolysis rate of ethyl ester, the intermediate Si (OH) generated in system4Number increases therewith.Meanwhile the increase of ammonia concn is notable
Promote Si (OH)4The aggregation growth speed of product, ultimately result in the increase of silicon dioxide colloid microballoon average quality, silica
The particle diameter of colloid micro ball mutually strains greatly.The monodispersity of silicon dioxide colloid microballoon is characterized using PDI values, PDI values are smaller, represent
The silicon dioxide colloid Microsphere Size of synthesis is more homogeneous, and difference is smaller between colloid micro ball, and PDI values are bigger, and colloid micro ball size is got over
Heterogeneity, difference is bigger between colloid micro ball.The dioxide/silica gel that water concentration synthesizes in 0.278mol/L-0.44mol/L scopes
For body microballoon single dispersing index all 0.08 or so, that is, the silicon dioxide colloid microballoon synthesized is monodispersed, is appropriate for follow-up
Self-assembled structures add lustre to research.The silicon dioxide colloid microspherulite diameter narrow distribution of synthesis, microspherulite diameter span is little, illustrates micro-
Ball Size Distribution further proves that the silicon dioxide colloid microballoon of synthesis has preferable monodispersity than more uniform.But when
When the silicon dioxide colloid microspherulite diameter of synthesis is excessive, rapid subsidence and accumulation easily occur in an assembling process for colloid micro ball,
And PDI values can also increase, it is unfavorable for the orderly self assembly of follow-up colloid micro ball.
When water concentration increases to 7.56mol/L from 4.06mol/L, the silicon dioxide colloid microspherulite diameter of synthesis from
199nm progressively increases to 331nm.This explanation increases with the increase of water concentration in reaction system, teos hydrolysis speed,
The intermediate product Si (OH) generated in reaction4Quantity increase, while the rate of polymerization in system also increases, the silica of generation
Colloid micro ball particle diameter also increases therewith, and while silicon dioxide colloid microspherulite diameter increase, its surface OH- quantity is also with increasing
Add, thus add the elecrtonegativity of silicon dioxide colloid microsphere surface, reunion probability is collided between microballoon and is declined, greatly strengthen breast
The stability of liquid system.But a large amount of ions can also substantially reduce the elecrtonegativity of microsphere surface caused by teos hydrolysis,
The stability of emulsion system and the dispersiveness of microballoon can be influenceed by very big.
As tetraethyl orthosilicate concentration from 0.048mol/L increases to 0.352mol/L, the particle diameter of silicon dioxide colloid microballoon
Increase to 380nm from 200nm.Because with the increase of silicon source concentration in system, resulting intermediate product silicic acid is hydrolyzed
Si(OH)4Concentration increases, and its polycondensation speed also accordingly increases, and the particle diameter of prepared silicon dioxide colloid microballoon also increases therewith
Greatly.In theory, in the reaction with the increase of silicon dioxide colloid microspherulite diameter ,-OH the contents of silica surface also can be with
Increase, and then add the stability of system, reduce the sedimentation of colloid micro ball, but in real reaction, tetraethyl orthosilicate
Hydrolysis can produce a large amount of ions, these ion concentrations increase with the increase of tetraethyl orthosilicate concentration, greatly reduce dioxy
The elecrtonegativity on SiClx colloid micro ball surface, reduces system stability, and then adds silicon dioxide colloid microballoon and assemble
Possibility.In addition, under the conditions of low concentration tetraethyl orthosilicate, the average distance between synthesis colloid micro ball can be increased, avoided
Interparticle reunion, be advantageous to the stabilization of system.
After reaction starts 10min, the silicon dioxide colloid microspherulite diameter synthesized in reaction system increases sharply, silica
Colloid micro ball particle diameter is rapidly increased to 200nm or so by 85nm in a short time, but the monodispersity of microballoon is very poor, reacts 3h
Afterwards, silicon dioxide colloid microspherulite diameter growth trend eases up, and microspherulite diameter is gradually stablized, and single dispersing index is 0.08 or so.Reacting
At initial stage, ammonia concn is higher in system, and teos hydrolysis speed is big, the Si (OH) of formation4Product number increase, Si (OH)4Production
Thing condensation speed increase, so as to form a large amount of silicon dioxide colloid microballoons in initial reaction stage.But the dioxy that initial reaction stage is formed
SiClx colloid micro ball particle diameter is small and specific surface area is big, and the stability of microballoon is very poor, it is easy to the Si (OH) newly formed around absorption4
Product forms the less big particle diameter microballoon of specific surface area, so as to which microspherulite diameter is continuously increased.Therefore, the silica of initial reaction stage
Colloid micro ball size is uneven.
Claims (6)
1. a kind of preparation method of silicon dioxide colloid microballoon, it is characterised in that comprise the following steps：（1）In three neck round bottom flask
Two kinds of solvents are well mixed by middle addition absolute ethyl alcohol and deionized water, high-speed stirred 5-10min；（2）Add after ammoniacal liquor quickly
After stirring 5-10min, volume ratio is added as 1:4 tetraethyl orthosilicate and alcohol mixeding liquid, after quickly stirring 2min；（3）
25 DEG C of temperature, reaction 20h directly causes reaction to terminate under the conditions of rotating speed 300r/min；（4）It is centrifuged at a high speed through centrifuge, 15min
Afterwards, take out after sample topples over supernatant, microballoon is diluted to scattered, then centrifugal treating again with water or ethanol, disperseed；（5）Continuously
Operation more than 3 times, the material not reacted completely is removed, the drying of silicon dioxide colloid microsphere solid will be obtained.
2. the preparation method of silicon dioxide colloid microballoon according to claim 1, it is characterised in that：The whipping process institute
It is heat collecting type constant temperature blender with magnetic force with mixer.
3. the preparation method of silicon dioxide colloid microballoon according to claim 2, it is characterised in that：Step（4）It is described from
The rotating speed of scheming is 6000r/min.
4. the preparation method of silicon dioxide colloid microballoon according to claim 3, it is characterised in that：Step（5）The baking
Dry temperature is 80 DEG C.
5. the preparation method of silicon dioxide colloid microballoon according to claim 4, it is characterised in that：The deionized water
Electrical conductivity is 16.8M Ω cm-1。
6. the preparation method of silicon dioxide colloid microballoon according to claim 5, it is characterised in that：Step（5）Described two
The particle diameter of silicon oxide colloid microballoon is 150-300nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711228922.8A CN107792860A (en) | 2017-11-29 | 2017-11-29 | The preparation method of silicon dioxide colloid microballoon |
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| CN201711228922.8A CN107792860A (en) | 2017-11-29 | 2017-11-29 | The preparation method of silicon dioxide colloid microballoon |
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| CN107792860A true CN107792860A (en) | 2018-03-13 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111430670A (en) * | 2020-04-13 | 2020-07-17 | 阮弟根 | Positive electrode plate, processing method thereof, application of positive electrode plate in preparation of lithium battery, and lithium battery |
| CN113307277A (en) * | 2021-05-20 | 2021-08-27 | 上海工程技术大学 | Silica nanoparticle with controllable particle size, and preparation method and application thereof |
| CN115818652A (en) * | 2022-11-23 | 2023-03-21 | 中国科学院深圳先进技术研究院 | Silicon dioxide filler for chip-level underfill adhesive and preparation method and application thereof |
-
2017
- 2017-11-29 CN CN201711228922.8A patent/CN107792860A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111430670A (en) * | 2020-04-13 | 2020-07-17 | 阮弟根 | Positive electrode plate, processing method thereof, application of positive electrode plate in preparation of lithium battery, and lithium battery |
| CN113307277A (en) * | 2021-05-20 | 2021-08-27 | 上海工程技术大学 | Silica nanoparticle with controllable particle size, and preparation method and application thereof |
| CN115818652A (en) * | 2022-11-23 | 2023-03-21 | 中国科学院深圳先进技术研究院 | Silicon dioxide filler for chip-level underfill adhesive and preparation method and application thereof |
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