CN107325322A - Modifying agent comprising nano material - Google Patents
Modifying agent comprising nano material Download PDFInfo
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- CN107325322A CN107325322A CN201610580382.9A CN201610580382A CN107325322A CN 107325322 A CN107325322 A CN 107325322A CN 201610580382 A CN201610580382 A CN 201610580382A CN 107325322 A CN107325322 A CN 107325322A
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- nano material
- modifying agent
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- hydrophobic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
Abstract
The invention discloses a kind of modifying agent for including nano material, the problem of material modified hydrophobic performance is poor, stability is poor in the prior art is mainly solved.The present invention is by using a kind of modifying agent for including nano material, nano material is dissolved in hydrophobic silicones compound ingredients, stirring is to being completely dissolved, and the technical scheme for obtaining the modifying agent comprising nano material preferably solves above mentioned problem, available in the modification of nano material.
Description
Technical field
The present invention relates to a kind of modifying agent for including nano material.
Background technology
What the wellability of the surface of solids was generally determined by the chemical composition and micro-geometry on surface.In recent years, it is super thin
Aqueous surface is due to its wide application prospect in industrial and agricultural production and people's daily life, such as：Water-oil separating, anti-corrosion
Erosion, automatically cleaning, waterproof, antifouling, drag-reducing coating etc., gradually cause the common concern of people.So-called super hydrophobic surface is usually
The contact angle referred to water is more than 150 ° of surface, and in general, super hydrophobic surface can be by hydrophobic material surface construction
Coarse structure, or modify low-surface energy substance on a solid surface to realize.
Although having reported the composition and preparation means and method of many super-hydrophobicity modifying agent at present, it is super thin
The practical application that water surface is constituted also fails to popularization, and especially simple economy, environment-friendly preparation method have to be developed.It is existing
All refer to, with low-surface energy substance costly, such as contain ring in the preparation process of most of super hydrophobic surface modifying agent of report
Oxygen tree fat, dopamine, Organic fluoride or organosilicon material compound come reduce surface surface can, and these materials are also universal
There is the defects such as poikilothermism is poor.Moreover, many methods of coarse hydrophobic surface are built, such as electrochemistry is sunk
Product, sol gel process, photoengraving, LBL self-assembly etc., can all be related to specific equipment, exacting terms and longer week
Phase, it is difficult to preparation (CN 104449357A, 2015.03.25, full text for inexpensive extensive super hydrophobic material；CN
103623709B, 2015.07.01, in full；CN 103305122B, 2015.10.21, in full；CN 102766269A,
2012.11.07, in full；CN 103951843A, 2014.07.30, in full；CN 102619093B, 2014.05.21, entirely
Literary).By contrast, silicon-fluorine polymer thing, siloxane polymer etc. not only have relatively low surface can, while have concurrently it is environment-friendly,
Resistance to temperature change, radioresistance and excellent recycling stability, can occur scion grafting polymerization, firmly under gentle preparation condition
The solid material surface that is modified is carried on, and it is cheap, it is adaptable to and large area is coated with.It is intrinsic with reference to nano-particle auxiliary agent etc.
High-ratio surface characteristic, can be in coarse structures such as solid material surface formation micro/nano level projection, grooves so that it is originally solid-
The air substitution that liquid contact is mutually partly trapped, forms the phase-contact surface of solid-liquid-gas three, thus reduces solid-liquid contact face, drop
It is easier to tumble, ultimately forms super hydrophobic surface.
The content of the invention
The technical problems to be solved by the invention are that material modified hydrophobic performance is poor in the prior art, stability is poor
There is provided a kind of new modifying agent for including nano material for problem.This method has the advantages that high stability, high hydrophobicity.
The technical solution adopted by the present invention is as follows：A kind of modifying agent for including nano material, nano material is dissolved in thin
In waterborne organic silicon compound ingredients, stir to being completely dissolved, obtain the modifying agent for including nano material；Wherein, nanometer
Material is selected from nano particle, nano wire or the nanobelt of silica；The hydrophobic silicones compound ingredients is selected from poly- two
The n-hexane or ethyl acetate mixture of methylsiloxane and octamethylcy-clotetrasiloxane curing agent, or fluorine containing silane ethanol
Solution.
In above-mentioned technical proposal, it is preferable that the mass ratio of nano material and hydrophobic silicones compound ingredients is 0.05
~0.2.
In above-mentioned technical proposal, it is preferable that the mass ratio of dimethyl silicone polymer and octamethylcy-clotetrasiloxane curing agent
For 5~10；Dimethyl silicone polymer and the compound proportion of nano material are 1~6.
In above-mentioned technical proposal, it is preferable that silicon fluoride and the mass ratio of nano material are 0.25~1；Fluorine containing silane ethanol
The concentration of solution is 3mg/mL~8mg/mL.
In above-mentioned technical proposal, it is preferable that the mechanical agitation time>4 hours.
Nano modifier stoste bonding force involved in the present invention is higher, the coarse two grades of knots constructed in solid material surface
Structure arrangement it is more random, it is thus possible to bear certain damage and keep good ultra-hydrophobicity, at the same stoste it is cheap,
Asepsis environment-protecting, it is easy to which scale is applied in expansion.
Brief description of the drawings
Fig. 1 characterizes knot for the SEM (SEM) on the gained nano modifier stoste modified product surface of embodiment 1
Really；
Fig. 2 is modified cavernous body product and water drop contact photo in embodiment 1；
Fig. 3 is that 30 water-oil separating of gained modified sponge material of embodiment 1 recycles stability test result；
Fig. 4 is the TEM characterization results of the gained nano modifier stoste of embodiment 7；
Fig. 5 is 7 institute's modified sponge materials of embodiment and water angle of wetting photo；
Fig. 6 is the SEM photograph of the modified sponge substrate material surface of the gained of embodiment 8；
Fig. 7 is the TEM characterization results of the gained nano modifier stoste of embodiment 9；
Fig. 8 is the gained modified sponge substrate material surface microscopic appearance SEM photograph of embodiment 10；
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Embodiment
【Embodiment 1】
(1) 2 grams of hydrophobicity aerosil nano particles, 7 grams of dimethyl silicone polymers, 1.2 grams of prestox rings are weighed
Tetrasiloxane is dissolved in 200 milliliters of n-hexanes, is positioned over single-necked flask and is extremely dissolved within 6 hours with puddler mechanical agitation, is obtained
To modifying agent stoste.
(2) polyurethane sponge base material is impregnated in above-mentioned modifying agent stoste 12 hours, 120 is placed in after removing drying
Hardened 6 hours in DEG C baking oven, obtain super-hydrophobic modified sponge body material.
Fig. 1 be the gained sponge material surface of embodiment 1 before modified after SEM characterize, pass through observe display
Modified sample surfaces have wrapped up a large amount of nano particles, and the nano particle cluster being packed together forms micron-nanometer level
Structure and rough fold, greatly improve the surface roughness of base material；Fig. 2 is modified sponge in embodiment 1
Body product and water drop contact photo, show its surface and the infiltration angle of water>150 °, with excellent superhydrophobic characteristic；Fig. 3 is real
Apply the products obtained therefrom of example 1 and carry out 30 water-oil separating loop test results, it was demonstrated that the stability of the stoste modified substrate material is excellent
It is good.
【Embodiment 2】
(1) 1 gram of hydrophobicity aerosil nano particle, 12 grams of dimethyl silicone polymers, 1.2 grams of prestox rings are weighed
Tetrasiloxane is dissolved in 500 milliliters of ethyl acetate, is positioned over single-necked flask and is extremely dissolved within 4 hours with puddler mechanical agitation,
Obtain the modifying agent for including nano material.
(2) polyurethane sponge base material is impregnated in above-mentioned modifying agent stoste 12 hours, 120 is placed in after removing drying
Hardened 6 hours in DEG C baking oven, obtain super-hydrophobic modified sponge body material.
Products obtained therefrom outward appearance, hydrophobic performance, stability in use are similar to the products obtained therefrom of embodiment 1.
【Embodiment 3】
(1) 20 grams of hydrophobicity aerosil nano particles, 200 grams of dimethyl silicone polymers, 40 grams of prestoxs are weighed
Cyclotetrasiloxane is dissolved in 6 liters of n-hexanes, is positioned over single-necked flask and is extremely dissolved within 5 hours with puddler mechanical agitation, is obtained
The modifying agent for including nano material.
(2) polyurethane sponge base material is impregnated in above-mentioned modifying agent stoste 12 hours, 120 is placed in after removing drying
Hardened 6 hours in DEG C baking oven, obtain super-hydrophobic modified sponge body material.
Products obtained therefrom outward appearance, hydrophobic performance, cyclical stability are similar to the products obtained therefrom of embodiment 1, illustrate that the stoste is amplified
Good modification power can be still kept after production.
【Embodiment 4】
(1) 2 grams of super-hydrophobic silica nano particles are weighed, 0.6 gram of silicon fluoride is dissolved in 200 milliliters of ethanol, magneton
Stirring 4 hours, obtains modifying agent stoste.
(2) sponge base material is impregnated in modified solution 12 hours, taking-up is placed in dries 3 hours at room temperature, obtains
Super-hydrophobic cavernous body sample.
Products obtained therefrom outward appearance, hydrophobic performance, stability in use are similar to the products obtained therefrom of embodiment 1.
【Embodiment 5】
(1) 0.6 gram of super-hydrophobic silica nano particle is weighed, 0.6 gram of silicon fluoride is dissolved in 100 milliliters of ethanol, magnetic
Son stirring 4 hours, obtains modifying agent stoste.
(2) sponge base material is impregnated in modified solution 12 hours, taking-up is placed in dries 3 hours at room temperature, obtains
Super-hydrophobic cavernous body sample.
Products obtained therefrom outward appearance, hydrophobic performance, stability in use are similar to the products obtained therefrom of embodiment 1.
【Embodiment 6】
(1) 12 grams of super-hydrophobic silica nano particles are weighed, 6 grams of silicon fluorides are dissolved in 800 milliliters of ethanol, and magneton is stirred
Mix 4 hours, obtain modifying agent stoste.
(2) sponge base material is impregnated in modified solution 12 hours, taking-up is placed in dries 3 hours at room temperature, obtains
Super-hydrophobic cavernous body sample.
Products obtained therefrom outward appearance, hydrophobic performance, stability in use are similar to the products obtained therefrom of embodiment 1.
【Embodiment 7】
(1) 2 grams of super-hydrophobic silica nano particles are weighed, 0.6 gram of silicon fluoride is dissolved in 100 milliliters of ethanol, magneton
Stirring 4 hours is simultaneously ultrasonically treated, obtains the modifying agent for including nano material.
(2) sponge base material is impregnated in modified solution 12 hours, taking-up is placed in dries 3 hours at room temperature, obtains
Super-hydrophobic cavernous body sample.
Fig. 4 is embodiment 7 gained nano modifier stoste transmission electron microscope (TEM) photo, shows it in silicon fluoride
Favorable dispersibility in ethanol solution；
Fig. 5 is the static angle of wetting photo of product and water, shows products obtained therefrom angle of wetting>150 °, in addition, its outward appearance and reality
Apply a 1-6 product different, carbonarius is presented, but hydrophobic performance and its stability in use are similar to embodiment 1-6 products.
【Embodiment 8】
(1) 2 grams of super-hydrophobic silica nano particles are weighed, 0.6 gram of silicon fluoride is dissolved in 100 milliliters of ethanol, magneton
Stirring 4 hours is simultaneously ultrasonically treated, obtains the modifying agent for including nano material.
(2) sponge base material is impregnated in modified solution 12 hours, taking-up is placed in dries 3 hours at room temperature, obtains
Super-hydrophobic cavernous body sample.
Fig. 6 is the SEM photograph of the modified sponge substrate material surface of the gained of embodiment 8, and display copper nano-wire is on its surface
Mutually overlap joint, forms up-and-down Nanostructure Network and nano-scale groove pattern.
The embodiment the hydrophobicity of product, stability in use it is similar to Example 1.
【Embodiment 9】
(1) 2 grams of super-hydrophobic silica nano particles are weighed, 0.6 gram of silicon fluoride is dissolved in 100 milliliters of ethanol, magneton
Stirring 4 hours is simultaneously ultrasonically treated, obtains the modifying agent for including nano material.
(2) sponge base material is impregnated in modified solution 12 hours, taking-up is placed in dries 3 hours at room temperature, obtains
Super-hydrophobic cavernous body sample.
Fig. 7 is the gained nano modifier stoste TEM photos of embodiment 9, shows that it is dispersed in silicon fluoride ethanol solution
Well；The embodiment the hydrophobicity of product, stability in use it is similar to Example 1.
【Embodiment 10】
(1) 2 grams of silica nanometer bands are weighed, 0.6 gram of silicon fluoride is dissolved in 100 milliliters of ethanol, magneton is stirred 4 hours
And it is ultrasonically treated, obtain the modifying agent for including nano material.
(2) sponge base material is impregnated in modified solution 12 hours, taking-up is placed in dries 3 hours at room temperature, obtains
Super-hydrophobic cavernous body sample.
Fig. 8 is the gained modified sponge substrate material surface microscopic appearance SEM photograph of embodiment 10, shows silica nanometer
Band can also form coarse micro-nano structure in substrate material surface；The embodiment the hydrophobicity of product, stability in use with
Embodiment 1 is similar.
【Embodiment 11】
Under optimum controlling condition, the contact angle that modified sponge body material prepared by embodiment 1-10 enters water-filling is tested, really
Its fixed superhydrophobic property, as shown in table 1, present invention design preparation method resulting materials are respectively provided with superhydrophobic characteristic：
Table 1
Claims (5)
1. a kind of modifying agent for including nano material, nano material is dissolved in hydrophobic silicones compound ingredients, stirring
To being completely dissolved, the modifying agent for including nano material is obtained；Wherein, nano material be selected from silica nano particle,
Nano wire or nanobelt；The hydrophobic silicones compound ingredients is selected from dimethyl silicone polymer and octamethylcy-clotetrasiloxane
The n-hexane or ethyl acetate mixture of curing agent, or fluorine containing silane ethanol solution.
2. the modifying agent of nano material is included according to claim 1, it is characterised in that nano material and hydrophobic silicones
The mass ratio of compound ingredients is 0.05~0.2.
3. the modifying agent of nano material is included according to claim 1, it is characterised in that dimethyl silicone polymer and prestox
The mass ratio of cyclotetrasiloxane curing agent is 5~10；Dimethyl silicone polymer and the compound proportion of nano material are 1~6.
4. the modifying agent of nano material is included according to claim 1, it is characterised in that the quality of silicon fluoride and nano material
Than for 0.25~1；The concentration of fluorine containing silane ethanol solution is 3mg/mL~8mg/mL.
5. the modifying agent of nano material is included according to claim 1, it is characterised in that mixing time>4 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610580382.9A CN107325322A (en) | 2016-07-22 | 2016-07-22 | Modifying agent comprising nano material |
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| CN201610580382.9A CN107325322A (en) | 2016-07-22 | 2016-07-22 | Modifying agent comprising nano material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109320940A (en) * | 2018-08-27 | 2019-02-12 | 四川大学锦城学院 | A kind of modifying agent containing nano material |
| CN109610160A (en) * | 2018-11-07 | 2019-04-12 | 浙江大学 | A kind of preparation method of the silk fabric with excellent hydrophobic performance |
| CN114561039A (en) * | 2022-03-11 | 2022-05-31 | 沧州师范学院 | Preparation method of polysiloxane modified super-hydrophobic sponge for oil-water separation |
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|---|---|---|---|---|
| US20090011222A1 (en) * | 2006-03-27 | 2009-01-08 | Georgia Tech Research Corporation | Superhydrophobic surface and method for forming same |
| CN105251240A (en) * | 2015-11-17 | 2016-01-20 | 中国科学院兰州化学物理研究所 | Method for preparing novel super-hydrophobic polyurethane oil-water separation material with no solvent |
| CN105542221A (en) * | 2015-12-18 | 2016-05-04 | 河南大学 | Wear-resistant super-hydrophobic super-lipophilic polyurethane sponge and preparation method and application thereof in oil-water continuous separation |
-
2016
- 2016-07-22 CN CN201610580382.9A patent/CN107325322A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090011222A1 (en) * | 2006-03-27 | 2009-01-08 | Georgia Tech Research Corporation | Superhydrophobic surface and method for forming same |
| CN105251240A (en) * | 2015-11-17 | 2016-01-20 | 中国科学院兰州化学物理研究所 | Method for preparing novel super-hydrophobic polyurethane oil-water separation material with no solvent |
| CN105542221A (en) * | 2015-12-18 | 2016-05-04 | 河南大学 | Wear-resistant super-hydrophobic super-lipophilic polyurethane sponge and preparation method and application thereof in oil-water continuous separation |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109320940A (en) * | 2018-08-27 | 2019-02-12 | 四川大学锦城学院 | A kind of modifying agent containing nano material |
| CN109610160A (en) * | 2018-11-07 | 2019-04-12 | 浙江大学 | A kind of preparation method of the silk fabric with excellent hydrophobic performance |
| CN114561039A (en) * | 2022-03-11 | 2022-05-31 | 沧州师范学院 | Preparation method of polysiloxane modified super-hydrophobic sponge for oil-water separation |
| CN114561039B (en) * | 2022-03-11 | 2023-08-29 | 沧州师范学院 | Preparation method of polysiloxane modified super-hydrophobic sponge for oil-water separation |
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Application publication date: 20171107 |