CN107312196A - super-hydrophobic sponge material and preparation method thereof - Google Patents
super-hydrophobic sponge material and preparation method thereof Download PDFInfo
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- CN107312196A CN107312196A CN201610580920.4A CN201610580920A CN107312196A CN 107312196 A CN107312196 A CN 107312196A CN 201610580920 A CN201610580920 A CN 201610580920A CN 107312196 A CN107312196 A CN 107312196A
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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
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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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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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 present invention relates to a kind of super-hydrophobic sponge material and preparation method thereof, the problem of existing adsorption recovery material hydrophobic effect is poor is mainly solved.The present invention is by using a kind of super-hydrophobic sponge material, including sponge material and nano modifier, the sponge material is melamine sponge or polyurethane sponge, the nano modifier is by the way that nano material is dissolved in hydrophobic silicones compound ingredients, the technical scheme that stirring is obtained and preparation method thereof to after being completely dissolved preferably solves above mentioned problem, in being prepared available for super-hydrophobic sponge material.
Description
Technical field
The present invention relates to a kind of super-hydrophobic sponge material and preparation method thereof.
Background technology
With economic rapid growth, the petroleum consumption cumulative year after year of China, external dependence degree also expands year by year, in order to
Reduce dependence of China's economic development to oil exporting country, in recent years, China more payes attention to the exploitation of offshore oil, but therewith
What is come is increasing sea oil spill accident, causes serious energy waste, environmental pollution or even potential safety hazard.According to statistics,
The spilling oil mass of China littoral sea ship and offshore drilling platform oil spill accident in recent years is up to 37000 tons or so, wherein 50 tons
Major oil spill accident above has 69, about 8000 tons of an oil spillage of most serious.Moreover, by artificial origin and nature
The oil leak that the factors such as corrosion are caused shows ascendant trend year by year.These all further exacerbate China's oil shortage of resources
Situation, seriously constrains domestic economy sustainable development, causes serious ecological environment disaster.Therefore, in order to ensure China
The sustainable stable development of Petroleum Industry, is oil in the urgent need to researching and developing the oil loss control technology with independent intellectual property right
The engineering that gas is reclaimed and oil leak Emergency recovery is equipped smoothly is implemented to lay the foundation.
In spill response control operation process, the larger heavy oil of commercial oil skimmer processing viscosity is highly effective but right
In the less oil of viscosity, because the oily collection mode that encloses for the features such as its diffusion area is big, oil reservoir is thin, being difficult with traditional comes clear
Reason.Secondary destruction or pollution are not only brought to ecological environment using means such as dispersant, microorganism eutrophication and burnings, and
Waste the energy oil product of worsening shortages.Adsorption separation technology is as a kind of principle is ripe and the oil loss of economical and efficient the most
Control device, it is considered to be one of main flow direction of oil spilling control technology development.This technology it is crucial with adsorbing separation material
The exploitation of material, traditional oil spilling handles sorbing material based on activated carbon, asphalt felt and a variety of natural plants, goes out again in recent years
Macroporous absorption material (CN 103951843 A, the 2014.07.30, full text using macromolecule sponge as substrate are showed；CN
102989414 B, 2014.09.10, in full；Zhang,Z.；Sèbe,G.；Rentsch,D.；Zimmermann,T.；
Tingaut,P.Chemistry of Materials 2014,26,2659；Si,Y.；Yu,J.；Tang,X.；Ge,J.；Ding,
B.Nat Commun 2014,5；Yang,Y.；Yi,H.；Wang,C.ACS Sustainable Chemistry&
Engineering 2015,3,3012.).These material generally existings protect oil cut rate reduction after being used for a long time, using effect is deteriorated,
It is difficult to processing thin layer oil slick and oil-water emulsion, adds the complex operation, with high costs that the later stage reclaims oil product, seriously hinder many
The commercial applications process of hole oleophilic oil material.Therefore we are using the reconstruct of surface and interface asperity and hydrophobic functional group branch
Modification is connect, the water-oil separating nanoscale interfacial materials with special wellability are formed, develops the water-oil separating material that can be mass-produced
The technical method of material, overcomes many defects of existing oil absorption material, fast and effectively realizes that water-oil separating is reclaimed.
The content of the invention
One of technical problems to be solved by the invention be the problem of existing adsorption recovery material hydrophobic effect is poor there is provided
A kind of new super-hydrophobic sponge material, the super-hydrophobic sponge material has the preferable advantage of hydrophobic effect.The present invention to be solved
Technical problem two be to provide a kind of preparation method with the corresponding super-hydrophobic sponge material of one of technical problem that is solving.
One of to solve the above problems, the technical solution adopted by the present invention is as follows：A kind of super-hydrophobic sponge material, it is described to receive
Rice modifying agent is by the way that nano material is dissolved in hydrophobic silicones compound ingredients, and stirring is obtained to after being completely dissolved；Its
In, the nano material is selected from nano particle, the nano wire of carbon-based, copper race Metal Substrate, copper family metal oxide or silica
Or nanobelt；The hydrophobic silicones compound ingredients is dimethyl siloxane mixing ring DMC toluene cyclohexanone solution, or
Ethanol solution containing vinyl chlorosilane.
In above-mentioned technical proposal, it is preferable that the sponge material is melamine sponge or polyurethane sponge, carbon-based nano
Material granule is CNT, carbon nano-fiber, graphene；Copper race metal-based nano particle is nano silver wire/rod, silver nanoparticle
Grain, copper nano-wire, copper nano particles；Copper family metal oxide is nano wire, the nanobelt of cuprous oxide or cupric oxide.
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；Dimethyl siloxane mixing ring DMC and the compound proportion of nano material are 1~6；Vinyl chlorosilane and nano material
Mass ratio be 0.25~1；The concentration of the ethanol solution containing vinyl chlorosilane is 3mg/mL~8mg/mL；Mixing time>4 is small
When.
For solve the above problems two, the technical solution adopted by the present invention is as follows：A kind of preparation of super-hydrophobic sponge material
Method, comprises the following steps：
(1) by the sponge material supersound washing in deionized water, absolute ethyl alcohol respectively, then it is impregnated in acid solution
Etching, drains and is placed in the dry for standby in drying box；
(2) nano modifier is prepared；
(3) the dried sponge material for obtaining step (1) is immersed in the nano modifier in step (2), at least
Drying is taken out after 30min；
(4) hardened at a temperature of dried sponge material sample being placed in into 120~200 DEG C, obtain super-hydrophobic sponge material
Material.
In above-mentioned technical proposal, it is preferable that acid solution is chromic acid solution.
In above-mentioned technical proposal, it is preferable that the supersound washing time in step (1)>15 minutes；Etching is with acid strength
1M, etch period is 10~30 minutes, sponge material drying time ＞ 1 hour after etching, and drying temperature is 60~80 DEG C.
In above-mentioned technical proposal, it is preferable that step is dried at room temperature in (3), drying time>3 hours.
In above-mentioned technical proposal, it is preferable that firm time is>2 hours.
On the one hand the purpose of the present invention is a kind of based on super-hydrophobic oleophylic nanometer surface and interface to obtain, available for spill response
The material of control, is on the other hand that, to solve the technological problemses that commercial oil absorption material synthetic method complexity, cost are high, proposition is a kind of
Simple infusion process is only needed to produce hydrophobic, high oil absorption multiplying power sponge material modification method for preparing.It is proposed by the present invention to be based on commercialization
The preparation method of sponge (melamine sponge, polyurethane sponge etc.), using commercial sponge block as substrate, is carved by acidic liquid
Erosion, apply leaching toluene cyclohexanone solution containing nano particle or nano wire etc. self-control modifier obtain with nanometer surface and interface and
The sponge material of special wetting characteristics.The hydrophobic carbon adsorbing material preparation method that this patent is proposed is simple, product hydrophobicity, follows
Ring performance and demulsification ability are excellent, and are easy to reclaim Reusability, can be mass-produced, contribute to product from experiment
Room prepares the conversion to commercial Application.Modified sponge material produced by the invention has good ultra-hydrophobicity (wetting
Angle>153 °), by acid etching and the micro-roughened surface produced by the load of nano material, it can be present in air and receive
In rice groove, air film blocks the contact between drop and the surface of solids, produces super-hydrophobic effect.At the same time, by institute's saw lumber
Material can greatly reduce the radial distance of sponge material free internal space via simple compression, produce excellent demulsification performance,
Achieve preferable technique effect.
Brief description of the drawings
Fig. 1 be the gained sponge material surface of embodiment 1 before modified after SEM (SEM) characterization result；
Fig. 2 is modified sponge material product and water drop contact photo in embodiment 1；
Fig. 3 is the experimental result that the products obtained therefrom of embodiment 1 is positioned in water body；
Fig. 4 is that the product that embodiment 1 is obtained is combined the reality that the quick adsorption in 25 seconds reclaims oil slick with self priming pump
Passport control examination of passports piece；
Fig. 5 is to be immersed in water body that good water-resisting ability can be kept after the made sample of embodiment 1 is combined with self priming pump
Experiment photo；
Fig. 6 removes the stereoscopic aobvious of situation for micron order oil droplet in water body before and after product treatment oil-water emulsion in embodiment 1
Micro mirror observes result.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Embodiment
【Embodiment 1】
(1) first, by melamine sponge supersound washing 15 minutes in deionized water and absolute ethyl alcohol respectively, it is placed on
It is placed in being cut into 4 × 4 × 4cm after drying 1 hour in 80 DEG C of baking ovens in stainless steel pallet3Fritter is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 30 minutes, then cleaned with deionized water to washing lotion
PH=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 2 grams of hydrophobicity aerosil nano particles are weighed, 8.2 grams of dimethyl siloxane mixing ring DMC are dissolved in
In 200 milliliters of toluene cyclohexanone, it is positioned over single-necked flask and is extremely dissolved within 6 hours with puddler mechanical agitation；
(4) take out the solution prepared to pour into beaker, sponge fritter is impregnated wherein 30 minutes；
(5) sponge fritter is put in stainless steel pallet, at room temperature aeration-drying 3 hours；
(6) the sponge fritter obtained after drying is placed in 120 DEG C of baking ovens and heats 6 hours, finally gives product hydrophobicity sea
It is continuous.
Fig. 1 be the gained sponge material surface of embodiment 1 before modified after SEM (SEM) characterize, by right
Than the two internal three-dimensional porous structure all for crosslinking net of display, wherein macropore diameter scope is 50~400 μm.But without
The fiber surface of modified sample is smooth, and the concavo-convex fold constituted by modified sample surfaces by a large amount of nano particles
Covered, cause roughness to be substantially improved；
Fig. 2 is modified sponge material product and water drop contact photo in embodiment 1, shows its surface and the infiltration angle of water
>150 °, with very strong hydrophobic property；
Fig. 3 shows that the products obtained therefrom of embodiment 1 is positioned in water body and can swum on the water surface, is immersed in surface in water body and shows
Existing glittering air film, it was demonstrated that the air film of the nanometer channel entrainment of material body surface and interface formation can effectively obstruct water body and enter sea
In continuous material void；
Fig. 4 is that the product that embodiment 1 is obtained is combined the reality that the quick adsorption in 25 seconds reclaims oil slick with self priming pump
Passport control examination of passports piece, it was demonstrated that resulting materials have stronger oil-wet behavior；
Fig. 5 is to be immersed in water body that good water-resisting ability can be kept after the made sample of embodiment 1 is combined with self priming pump
Experiment photo, further testimonial material has good hydrophobicity；
Fig. 6 removes the stereoscopic aobvious of situation for micron order oil droplet in water body before and after product treatment oil-water emulsion in embodiment 1
Micro mirror observes result, it was demonstrated that material has excellent demulsification ability.
【Embodiment 2】
(1) first, by melamine sponge supersound washing 20 minutes in deionized water and absolute ethyl alcohol respectively, it is placed on
It is placed in being cut into 1 × 1 × 1cm after drying 1 hour in 60 DEG C of baking ovens in stainless steel pallet3Fritter is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 30 minutes, then cleaned with deionized water to washing lotion
PH=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 0.4 gram of nanometer silica line is weighed, 2.4 grams of dimethyl siloxane mixing ring DMC are dissolved in 60 milliliters of toluene
In cyclohexanone, it is positioned over single-necked flask and is extremely dissolved within 4 hours with puddler mechanical agitation；
(4) sponge fritter is impregnated in modified solution 2 hours, while being placed in ultrasonic disperse in ultrasonic cleaning machine；
(5) sponge fritter is put in stainless steel pallet, at room temperature aeration-drying 3 hours；
(6) the sponge fritter obtained after drying is placed in 150 DEG C of baking ovens and hardens 4 hours, finally gives product hydrophobicity sea
It is continuous.
The surface and interface microtexture of gained sample has close coarse structure with sample in embodiment 1, its hydrophobic test
As a result show same excellent hydrophobic property, with reference to same model self priming pump formed the oil-water separation of system also with reality
The products obtained therefrom of example 1 is similar.
【Embodiment 3】
(1) first, by polyurethane sponge supersound washing 15 minutes in deionized water and absolute ethyl alcohol respectively, it is placed on not
It is placed in being cut into 4 × 4 × 4cm after drying 1 hour in 70 DEG C of baking ovens in rust steel tray3Fritter is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 1 hour, then cleaned with deionized water to washing lotion pH
=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 2 grams of hydrophobicity aerosil nano particles, 11.2 grams of dimethyl siloxane mixing ring DMC dissolvings are weighed
In 200 milliliters of toluene cyclohexanone, it is positioned over single-necked flask and is extremely dissolved within 5 hours with puddler mechanical agitation；
(4) take out the solution prepared to pour into beaker, sponge fritter is impregnated wherein 30 minutes, taking-up is placed at room temperature
Drying 3 hours, the process is repeated 3 times；
(5) the sponge fritter that last time is infiltrated after being modified and drying is placed in 120 DEG C of baking ovens and heats 6 hours, finally
Obtain product hydrophobicity sponge.
Gained sample hydrophobicity, oil and water separation capability etc. are similar with the products obtained therefrom of example 1.
【Embodiment 4】
(1) first, by melamine sponge, supersound washing removes table in 15 minutes in deionized water and absolute ethyl alcohol respectively
Face pollutant that may be present, be placed in stainless steel pallet be placed in 80 DEG C of baking ovens dry 1 hour after be cut into 4 × 4 × 4cm3
Fritter is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 1 hour, then cleaned with deionized water to washing lotion pH
=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 11 grams of dimethyl siloxane mixing ring DMC are weighed to be dissolved in 200 milliliters of toluene cyclohexanone, single port is positioned over
Flask and with puddler mechanical agitation 4 hours；
(4) take out the solution prepared to pour into beaker, sponge fritter is impregnated wherein 12 hours, taking-up is placed at room temperature
Ventilation 5 hours；
(5) modified sponge fritter is placed in 200 DEG C of baking ovens and heats 2 hours, finally give product hydrophobicity sponge.
Gained sample hydrophobicity, oil and water separation capability etc. are similar with the products obtained therefrom of example 1.
【Embodiment 5】
(1) first, by polyurethane sponge, supersound washing removes surface in 15 minutes in deionized water and absolute ethyl alcohol respectively
Pollutant that may be present, be placed in stainless steel pallet be placed in 80 DEG C of baking ovens dry 1 hour after be cut into 4 × 4 × 4cm3It is small
Block is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 1 hour, then cleaned with deionized water to washing lotion pH
=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 2 grams of super-hydrophobic silica nano particles are weighed, 0.6 gram of vinyl chlorosilane is dissolved in 200 milliliters of ethanol
In, magneton is stirred 4 hours；
(4) sponge fritter is impregnated in modified solution 24 hours, taking-up is placed in divulges information 5 hours at room temperature, finally obtains
Super-hydrophobic sponge material product
Gained sample hydrophobicity, oil and water separation capability etc. are similar with the products obtained therefrom of example 1.
【Embodiment 6】
(1) first, by melamine sponge, supersound washing removes table in 15 minutes in deionized water and absolute ethyl alcohol respectively
Face pollutant that may be present, be placed in stainless steel pallet be placed in 80 DEG C of baking ovens dry 1 hour after be cut into 4 × 4 × 4cm3
Fritter is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 1 hour, then cleaned with deionized water to washing lotion pH
=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 2 grams of super-hydrophobic silica nano particles are weighed, 2 grams of vinyl chlorosilanes are dissolved in 200 milliliters of ethanol,
Magneton is stirred 6 hours and ultrasonically treated；
(4) sponge fritter is impregnated in modified solution 10 hours, taking-up is placed in dries 3 hours at room temperature, the process weight
It is multiple 3 times, finally give super-hydrophobic sponge material sample.
Gained sample hydrophobicity, oil and water separation capability etc. are similar with the products obtained therefrom of example 1.
【Embodiment 7】
Under optimum controlling condition, the contact angle that modified sponge material prepared by embodiment 1-6 enters water-filling is tested, it is determined
Superhydrophobic property, as shown in table 1, present invention design preparation method resulting materials are respectively provided with superhydrophobic characteristic：
Table 1
| Embodiment | The contact angle of water |
| 1 | 153.1° |
| 2 | 156.4° |
| 3 | 152.2° |
| 4 | 155.3° |
| 5 | 156.3° |
| 6 | 154.9° |
【Embodiment 8】
(1) first, by melamine sponge supersound washing 15 minutes in deionized water and absolute ethyl alcohol respectively, it is placed on
It is placed in being cut into 4 × 4 × 4cm after drying 1 hour in 80 DEG C of baking ovens in stainless steel pallet3Fritter is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 30 minutes, then cleaned with deionized water to washing lotion
PH=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 4 grams of fine copper nano wires are weighed, 8.2 grams of dimethyl siloxane mixing ring DMC are dissolved in 200 milliliters of toluene hexamethylenes
In ketone, it is positioned over single-necked flask and is extremely dissolved within 6 hours with puddler mechanical agitation；
(4) take out the solution prepared to pour into beaker, sponge fritter is impregnated wherein 30 minutes；
(5) sponge fritter is put in stainless steel pallet, at room temperature aeration-drying 3 hours；
(6) the sponge fritter obtained after drying is placed in 120 DEG C of baking ovens and heats 6 hours, finally gives product hydrophobicity sea
It is continuous.
Copper red color is presented in gained color sample, with the hydrophobic similar temperament of gained sample of embodiment 1, can be suspended in water body and realize
The function such as oil slick adsorption recovery and water-oil separating.
【Embodiment 9】
(1) first, by polyurethane sponge, supersound washing removes surface in 15 minutes in deionized water and absolute ethyl alcohol respectively
Pollutant that may be present, be placed in stainless steel pallet be placed in 80 DEG C of baking ovens dry 1 hour after be cut into 4 × 4 × 4cm3It is small
Block is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 1 hour, then cleaned with deionized water to washing lotion pH
=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 2 grams of cuprous oxide over-expense nanostructured powders are weighed, 0.6 gram of vinyl chlorosilane is dissolved in 200 milliliters of ethanol
In, magneton is stirred 4 hours；
(4) sponge fritter is impregnated in modified solution 24 hours, taking-up is placed in divulges information 5 hours at room temperature, finally obtains
Super-hydrophobic sponge material product.
Gained sample hydrophobicity and oil and water separation capability and embodiment 1 are similar.
【Embodiment 10】
(1) first, by polyurethane sponge, supersound washing removes surface in 15 minutes in deionized water and absolute ethyl alcohol respectively
Pollutant that may be present, be placed in stainless steel pallet be placed in 80 DEG C of baking ovens dry 1 hour after be cut into 4 × 4 × 4cm3It is small
Block is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 1 hour, then cleaned with deionized water to washing lotion pH
=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 2 grams of nano silver wire powders are weighed, 8.2 grams of dimethyl siloxane mixing ring DMC are dissolved in 200 milliliters of toluene rings
In hexanone, magneton is stirred 6 hours；
(4) sponge fritter is impregnated in modified solution 24 hours, taking-up is placed in divulges information 5 hours at room temperature, then is positioned over
Hardened 6 hours in 120 DEG C of baking ovens, finally obtain super-hydrophobic sponge material product.
Gained sample hydrophobicity and oil and water separation capability and embodiment 1 are similar.
【Embodiment 11】
(1) first, by polyurethane sponge, supersound washing removes surface in 15 minutes in deionized water and absolute ethyl alcohol respectively
Pollutant that may be present, be placed in stainless steel pallet be placed in 80 DEG C of baking ovens dry 1 hour after be cut into 4 × 4 × 4cm3It is small
Block is standby；
(2) then sponge material is impregnated in 1M chromic acid solution 1 hour, then cleaned with deionized water to washing lotion pH
=7, taking-up is placed in 80 DEG C of baking ovens and dried 3 hours；
(3) 2 grams of nano cuprous oxide wires are weighed, 0.6 gram of vinyl chlorosilane is dissolved in 200 milliliters of ethanol, and magneton is stirred
Mix 4 hours；
(4) sponge fritter is impregnated in modified solution 24 hours, taking-up is placed in divulges information 5 hours at room temperature, finally obtains
Super-hydrophobic sponge material product.
Gained sample hydrophobicity and oil and water separation capability and embodiment 1 are similar.
【Embodiment 12】
Under optimum controlling condition, the contact angle that modified sponge material prepared by embodiment 8-11 enters water-filling is tested, it is determined that
Its superhydrophobic property, as shown in table 1, present invention design preparation method resulting materials are respectively provided with superhydrophobic characteristic：
Table 2
| Embodiment | The contact angle of water |
| 8 | 155.1° |
| 9 | 153.2° |
| 10 | 155.3° |
| 11 | 151.8° |
Obviously, above-described embodiment, just to illustrate the validity and practicality of the preparation method, is not to embodiment party
The restriction of formula, such as base material use commercial sponge in the invention, naturally it is also possible to be changed to stainless (steel) wire, copper mesh,
Other various forms of changes of filter membrane (paper), polyester textile etc., there is no need and unable to enter one by one for various embodiments
Row is exhaustive, and the obvious changes or variations thus amplified is in scope of patent protection of the present invention.
Claims (8)
1. a kind of super-hydrophobic sponge material, including sponge material and nano modifier, the nano modifier is by by nanometer material
Material is dissolved in hydrophobic silicones compound ingredients, and stirring is obtained to after being completely dissolved；Wherein, the nano material is selected from carbon
Base, copper race Metal Substrate, nano particle, nano wire or the nanobelt of copper family metal oxide or silica；The hydrophobicity has
Organic silicon compound ingredients is dimethyl siloxane mixing ring DMC toluene cyclohexanone solution, or the ethanol containing vinyl chlorosilane
Solution.
2. super-hydrophobic sponge material according to claim 1, it is characterised in that the sponge material be melamine sponge or
Polyurethane sponge, c-based nanomaterial particle is CNT, carbon nano-fiber, graphene；Copper race metal-based nano particle is
Nano silver wire/rod, silver nano-grain, copper nano-wire, copper nano particles；Copper family metal oxide is cuprous oxide or cupric oxide
Nano wire, nanobelt.
3. super-hydrophobic sponge material according to claim 1, it is characterised in that nano material and hydrophobic silicones compound
The mass ratio of ingredients is 0.05~0.2；Dimethyl siloxane mixing ring DMC and the compound proportion of nano material are 1~6；Ethene
Base chlorosilane and the mass ratio of nano material are 0.25~1；The concentration of vinyl chlorosilane ethanol solution is 3mg/mL~8mg/
mL；Mixing time>4 hours.
4. the preparation method of super-hydrophobic sponge material as claimed in claim 1, comprises the following steps：
(1) by the sponge material supersound washing in deionized water, absolute ethyl alcohol respectively, then it is impregnated in acid solution quarter
Erosion, drains and is placed in the dry for standby in drying box；
(2) nano modifier is prepared；
(3) the dried sponge material for obtaining step (1) is immersed in the nano modifier in step (2), at least 30min
After take out drying；
(4) hardened at a temperature of dried sponge material sample being placed in into 120~200 DEG C, obtain super-hydrophobic sponge material.
5. the preparation method of super-hydrophobic sponge material according to claim 1, it is characterised in that acid solution is chromic acid solution.
6. the preparation method of super-hydrophobic sponge material according to claim 1, it is characterised in that the supersound washing in step (1)
Time>15 minutes；Etching is 1M with acid strength, and etch period is 10~30 minutes, sponge material drying time ＞ 1 after etching
Hour, drying temperature is 60~80 DEG C.
7. the preparation method of super-hydrophobic sponge material according to claim 1, it is characterised in that step is done at room temperature in (3)
It is dry, drying time>3 hours.
8. the preparation method of super-hydrophobic sponge material according to claim 1, it is characterised in that firm time is>2 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610580920.4A CN107312196A (en) | 2016-07-22 | 2016-07-22 | super-hydrophobic sponge material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610580920.4A CN107312196A (en) | 2016-07-22 | 2016-07-22 | super-hydrophobic sponge material and preparation method thereof |
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Cited By (5)
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| CN107876033A (en) * | 2017-11-16 | 2018-04-06 | 武汉工程大学 | The method that solution dipping method prepares the hydrophobic oleophilic oil melamine sponge of carbon nano-tube modification |
| CN110240731A (en) * | 2019-05-23 | 2019-09-17 | 东南大学 | A kind of preparation method of graphene with high specific surface-metal oxide composite sponge |
| CN110393949A (en) * | 2019-06-24 | 2019-11-01 | 舟山市质量技术监督检测研究院 | A kind of super-hydrophobic super-oleophylic polyurethane sponge material and preparation method thereof |
| CN110773137A (en) * | 2019-10-22 | 2020-02-11 | 同济大学 | Silicon dioxide nanorod-melamine foam compound and preparation method thereof |
| CN114832781A (en) * | 2022-04-28 | 2022-08-02 | 西南石油大学 | Super-hydrophobic/super-oleophylic sponge oil-water separation material and preparation method thereof |
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| CN102358067A (en) * | 2011-07-27 | 2012-02-22 | 江南大学 | Super-hydrophobic textile and processing method thereof |
| CN103173998A (en) * | 2011-12-23 | 2013-06-26 | 中国科学院兰州化学物理研究所 | Preparation method of superhydrophobic woven fabric for oil-water separation |
| 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 |
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| CN102358067A (en) * | 2011-07-27 | 2012-02-22 | 江南大学 | Super-hydrophobic textile and processing method thereof |
| CN103173998A (en) * | 2011-12-23 | 2013-06-26 | 中国科学院兰州化学物理研究所 | Preparation method of superhydrophobic woven fabric for oil-water separation |
| 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 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107876033A (en) * | 2017-11-16 | 2018-04-06 | 武汉工程大学 | The method that solution dipping method prepares the hydrophobic oleophilic oil melamine sponge of carbon nano-tube modification |
| CN110240731A (en) * | 2019-05-23 | 2019-09-17 | 东南大学 | A kind of preparation method of graphene with high specific surface-metal oxide composite sponge |
| CN110240731B (en) * | 2019-05-23 | 2021-06-25 | 东南大学 | Preparation method of graphene-metal oxide composite sponge with high specific surface area |
| CN110393949A (en) * | 2019-06-24 | 2019-11-01 | 舟山市质量技术监督检测研究院 | A kind of super-hydrophobic super-oleophylic polyurethane sponge material and preparation method thereof |
| CN110773137A (en) * | 2019-10-22 | 2020-02-11 | 同济大学 | Silicon dioxide nanorod-melamine foam compound and preparation method thereof |
| CN114832781A (en) * | 2022-04-28 | 2022-08-02 | 西南石油大学 | Super-hydrophobic/super-oleophylic sponge oil-water separation material and preparation method thereof |
| CN114832781B (en) * | 2022-04-28 | 2023-06-06 | 西南石油大学 | Super-hydrophobic/super-oleophylic sponge oil-water separation material and preparation method thereof |
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Application publication date: 20171103 |