CN109206658A - A kind of preparation method of super-hydrophobic blown rubber - Google Patents
A kind of preparation method of super-hydrophobic blown rubber Download PDFInfo
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- CN109206658A CN109206658A CN201710551396.2A CN201710551396A CN109206658A CN 109206658 A CN109206658 A CN 109206658A CN 201710551396 A CN201710551396 A CN 201710551396A CN 109206658 A CN109206658 A CN 109206658A
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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
- C08J9/405—Impregnation with polymerisable compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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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
- C08J9/365—Coating
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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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/16—Ethene-propene or ethene-propene-diene copolymers
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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Abstract
The present invention relates to a kind of preparation methods of super-hydrophobic blown rubber, chemical roughening method and sol-gel method is used to carry out modified foaming rubber so that super-hydrophobic blown rubber is made, hydrophilic radical is introduced on blown rubber surface by the coarsening solution with strong oxidizing property, it is subsequently added into the hydrophobic layer that organosilan brings it about hydrolysis and dehydrating condensation generation has low-surface-energy, and blown rubber surface is incorporated in a manner of chemical bond, to prepare super-hydrophobic blown rubber.Preparation process of the present invention is simple, and mild condition room temperature can be operated, and does not need special instruments and equipment.Modified feedstock used is cheap and easy to get, and material preparation cost is low.Prepared material has highly selective, high oil absorption ability, and can be used repeatedly, and durability is strong.
Description
Technical field
The present invention relates to functional material preparation technical fields, and in particular to a kind of preparation method of super-hydrophobic blown rubber.
Background technique
As the mankind rapidly develop the growing of oil demand, oil exploration industry and transport service, oil spilling thing is resulted in
Therefore Frequent Accidents are revealed with organic solvent, heavy economic losses is not only caused, also ecological environment and human survival are caused
It seriously threatens.Current oil spilling or the technology of organic solvent leakage processing focus on exploitation and improve oil absorption material, improve from water
Separation and the efficiency for collecting petroleum.At present the research and development of oil absorption material are become with the emphasis of oil spilling process field.It in recent years, will be super thin
Water super-oleophilic can be attached on three-dimensional porous material the research hotspot for becoming oil absorption material field, and functionalization new material can be with
For handling offshore oil leakage or the leakage of liquid organic reagent, it is very effective the adsorbent material of hydrocarbons.So far
The three-dimensional porous material with special surface wetability is prepared, and the material being applied in water-oil separating has very much, such as carbon
Three-dimensional material, Pintsch process melamine foams, carbon nano-tube/poly tetrafluoroethene composite material and the silica aerogel that nanotube is assembled into
Equal materials.But there are many problems in actual application for these materials, such as: preparation process is complicated, raw material are expensive,
Reaction reagent and equipment valuableness are low with the ability that recycles etc..The especially absorption of oil product and the reuse of salvage material effect
Rate restricts the extensive use of water-oil separating material.Therefore, develop one kind can by simple preparation process and preparation cost it is low
Honest and clean novel super hydrophobic material has very big realistic meaning.
Blown rubber is a kind of material haveing excellent performance for being widely used in many fields, intrinsic three-dimensional porous structure
Make it have the potentiality applied in water-oil separating field.Compared with other three-dimensional porous materials, sponge rubber is cheap and easily-available, tool
There are good mechanical property and longer service life.Therefore, using blown rubber as substrate, modifying super hydrophobicity is carried out to it, is obtained
To super-hydrophobic blown rubber can obtain wide application in fields such as water-oil separatings.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, the preparation for current three-dimensional porous super hydrophobic material is lacked
It falls into, develops a kind of new super-hydrophobic functional material that can be obtained by comparing simple, low cost preparation process, and energy
Carry out efficient water-oil separating.
Technical purpose of the invention is achieved by following technical proposals:
A kind of preparation method of super-hydrophobic blown rubber carries out as steps described below:
Step 1, blown rubber is placed in dehydrated alcohol and is cleaned by ultrasonic, taking-up, which places into deionized water, to be surpassed
Sound cleaning, so carries out alternately cleaning, until surface and internal impurity are properly washed, takes out after cleaning, dry in vacuum
It is dried in dry case；
In step 1, the foam pattern of blown rubber is open-cell foaming.
In step 1, the time being cleaned by ultrasonic in dehydrated alcohol is 30~90min, preferably 30-60min, is surpassed
Acoustical power is 100-150w.
In step 1, the time being cleaned by ultrasonic in deionized water is 30~90min, preferably 30-60min, is surpassed
Acoustical power is 100-150w.
In step 1, when alternately clean, alternately wash number is 1~5 time.
Step 2, blown rubber step 1 handled immerses in coarsening solution, is roughened under 20-25 degrees Celsius of room temperature, is made
It obtains coarsening solution and introduces hydrophilic radical on blown rubber surface, take out after roughening and cleaned repeatedly with deionized water, removed residual
The coarsening solution stayed places into vacuum oven and dries the blown rubber being roughened；
In step 2, coarsening solution is the solution with strong oxidizing property, such as the concentrated sulfuric acid of mass percent 98wt%；Matter
The mass ratio of the concentrated sulfuric acid of amount percentage 98wt% and the mixture of potassium permanganate, the concentrated sulfuric acid and potassium permanganate is (1-2):
(0.5—1)；The concentrated sulfuric acid of mass percent 98wt% and mixture with chrome green, the concentrated sulfuric acid and chrome green
Mass ratio is (1-2): (0.5-1)；The mixing of the concentrated sulfuric acid, potassium permanganate and chrome green of mass percent 98wt%
Object, the mass ratio of the concentrated sulfuric acid, potassium permanganate and chrome green are (1-2): (0.5-1): (0.5-1).
In step 2, the reaction condition of the roughening is that 0.5~6h is reacted under 20-25 degrees Celsius of room temperature, preferably 2-5
Hour.
Step 3, the blown rubber after step 2 roughening is immersed in reaction medium, organosilan and deionized water is added, stirs
It is reacted, the super-hydrophobic blown rubber is made and is solidified under the conditions of mixing.
In step 3, organosilan is first added, adds deionized water, or deionized water is first added, adds organic
Silane.
In step 3, the reaction medium is n-hexane, hexamethylene, methylene chloride, normal heptane, normal octane, benzene or diformazan
Benzene；The organosilan is trim,ethylchlorosilane, dimethyldichlorosilane, methyl trichlorosilane, ethyl trichlorosilane or just
Octyltrichlorosilane；Percentage by volume of the organosilan in reaction medium be 0.05~5vol%, preferably 1-4vol%, i.e.,
Organosilan volume/(the sum of organosilan and the volume of reaction medium).
In step 3, speed of agitator is 50~500 turns per minute, 100-300 turns preferably per minute.
In step 3, the volume ratio of organosilan and deionized water is 1:0.1~1:10, preferably 1:(3-8).
In step 3, it is 5~120min, preferably 30-60min that the reaction time is carried out under stirring condition；Temperature is room temperature
20-25 degrees Celsius.
In step 3, it is reacted, is placed in the blown rubber of surface covering hydrophobic silicone at room temperature after reaction
In vacuum oven, solidification drying is carried out, is made super-hydrophobic blown rubber, solidification temperature is 50~130 DEG C, preferably 60-100
Degree Celsius.
As shown in Figure 1, compared with original blown rubber, on super-hydrophobic blown rubber surface, one layer of coating of uniform fold,
It is observed that the surface coated uniform fold of blown rubber, without apparent uncovered area.In * 1000 times of multiplying power
Down it is observed that the coating is uniform space three-dimensional skeleton structure, this is MTCS hydrolytic crosslinking as a result, this proves to pass through
Modifying super hydrophobicity, coating obtained by MTCS hydrolytic crosslinking have successfully been attached to blown rubber surface, have provided ultra-hydrophobicity.
Fig. 1 (under) be the interior section for cutting off the blown rubber after modifying super hydrophobicity SEM image, it can be seen that even foaming rubber
The inner surface of glue is also covered with the super-hydrophobic coat of the equably MTCS of space three-dimensional skeleton structure, this is proved in blown rubber
Modifying super hydrophobicity in, super-hydrophobic coat has not been placed only in the outside of blown rubber, but uniform fold is in blown rubber
Each face on.Compared to the siloxanes super-hydrophobic coat of other sheets obtained by sol-gal process, this paper's is super thin
The tridimensional network of continuous uniform is presented in water coating, and help constructs micro-enzyme electrode, is more advantageous to and realizes super-hydrophobic spy
Property, binding test contact angular data, it is known that average contact angle angle is at 150 degree or more.
It as shown in Figure 2, is the stretching vibration of-OH at about~3600-3690cm-1.~1375cm-1 and~
It is symmetrical stretching vibration and the asymmetric stretching vibration of-CH3 respectively at 1457cm-1.At 2850cm-1 and 2930cm-1
The symmetrical stretching vibration of corresponding-CH2- and the peak of asymmetric stretching vibration reduce, this explanation is dense during chemistry roughening
Sulfuric acid is reacted with-the CH2- on main chain.There is a new absorption peak at~1697cm-1, it belongs to C=O's
Characteristic peak, this is roughening product of the concentrated sulfuric acid to sponge rubber.Compared with original EPDM sponge rubber, modifying super hydrophobicity sponge rubber
Glue respectively~762cm-1 ,~1006cm-1 ,~1113cm-1 and~1269cm-1 at there is stronger infrared absorption peak,
They belong to the vibration characteristic peak of Si-O-Si group.By the analysis of FT-IR spectrogram, illustrate the attachment of sponge rubber surface
Substance is exactly the polysiloxanes that MTCS hydrolytic crosslinking generates.
Fig. 3 is the xps energy spectrum figure of super-hydrophobic sponge rubber, by the fitting to the fine spectrogram of each element it is found that wherein C1s
The characteristic peak of 532.0eV belongs to the combination energy of corresponding element in C-O in 286.5eV and O1s spectrogram in spectrogram, in C1s spectrogram
The characteristic peak of 101.6eV belongs to the combination energy of corresponding element in Si-C in 283.1eV and Si2p spectrogram, and in O1s spectrogram
The characteristic peak of 102.9eV then belongs to the combination energy of corresponding element in Si-O-Si in 534.0eV and Si2p spectrogram.The above analysis knot
Fruit shows that modified material shows that hydrolytic crosslinking successfully has occurred in MTCS, and has been incorporated in EPDM sponge rubber surface, mentions for material
Low-surface-energy is supplied.And in the XPS analysis of the super-hydrophobic EPDM blown rubber of preparation, it can be seen that with the presence of N element.It is high
The substance of nitrogen content meeting endothermic decomposition during heated comes out the small-molecule substances such as NO2, NO, NH3, reduces temperature, meanwhile,
This small-molecule substance can be covered on the surface of the substance, play a dual role of completely cutting off air, this to make super-hydrophobic change
Property EPDM sponge rubber material have extraordinary flame retardant property.
The present invention provides a kind of preparation method of super-hydrophobic blown rubber, using blown rubber as substrate, first with roughening
Liquid is roughened blown rubber, introduces hydrophilic radical, the blown rubber being roughened, further using organic on its surface
Silicone layer with low-surface-energy is attached to blown rubber surface, obtains super-hydrophobic blown rubber by the reaction of silane.
In preparation process, required chlorosilane concentration is low, and reaction can carry out at room temperature.Compared with prior art, the present invention having
Following advantage:
(1) preparation process is simple, and reaction condition requirement is low, can react at room temperature, reaction process is mild, and it is special not need
Instrument and equipment.
(2) during the preparation process, the organosilan concentration needed is low, reduces preparation cost.
(3) modified material used in is commodity blown rubber, and no stringent technical parameter request is cheap and easily-available.
(4) material obtained has very strong grease selective power, and water-oil separating is high-efficient, and after reusing
Oil absorption capacity will not decline.
Detailed description of the invention
Fig. 1 is that super-hydrophobic sponge rubber outer surface (upper row in picture) and inner surface are (following in picture in the present invention
A line) SEM photograph.
Fig. 2 is the FT-IR spectrum of sponge rubber and super-hydrophobic sponge rubber after original sponge rubber, roughening in the present invention
Figure.
Fig. 3 is the XPS figure of super-hydrophobic sponge rubber prepared by the present invention.
Fig. 4 is the process flow diagram of preparation method of the present invention.
Fig. 5 is the contact angle test figure of Central Plains beginning blown rubber and water of the present invention (contact angle values are 104.2 °).
Fig. 6 is the contact angle test figure of super-hydrophobic blown rubber and water prepared by the present invention (contact angle values are 154 °).
Specific embodiment
Technical solution of the present invention is further illustrated combined with specific embodiments below.
The device parameter used is as shown in the table:
Protospongia rubber (blown rubber, i.e., open foaming) performance parameter is as shown in the table:
Method one:
Commercially available blown rubber is put into dehydrated alcohol and deionized water first and carries out 30~90min of ultrasonic cleaning respectively,
Alternately cleaning 1~5 time is taken out to be put into vacuum oven and be dried to remove blown rubber surface and internal impurity after cleaning
Dry 0.5~2h, immerses in the coarsening solution concentrated sulfuric acid after drying, 0.5~6h of roughening is carried out at room temperature, so that coarsening solution is in blown rubber
Surface introduces hydrophilic radical, takes out after roughening and is cleaned repeatedly with deionized water, removes remaining coarsening solution, places into true
Empty drying box dries 0.5~2h, is then dipped in reaction medium, and organosilan first is added to reaction medium, adds
Ionized water carries out 5~120min of reaction under agitation at room temperature, takes out and places in a vacuum drying oven, 50~
Solidified and dried 0.5~2h at 130 DEG C, super-hydrophobic blown rubber is made.
Method two:
Commercially available blown rubber is put into dehydrated alcohol and deionized water first and carries out 30~90min of ultrasonic cleaning respectively,
Alternately cleaning 1~5 time is taken out to be put into vacuum oven and be dried to remove blown rubber surface and internal impurity after cleaning
Dry 0.5~2h, immerses in the coarsening solution concentrated sulfuric acid after drying, 0.5~6h of roughening is carried out at room temperature, so that coarsening solution is in blown rubber
Surface introduces hydrophilic radical, takes out after roughening and is cleaned repeatedly with deionized water, removes extra coarsening solution, places into true
Empty drying box dries 0.5~2h, is then dipped in reaction medium, and deionized water first is added to reaction medium, has added
Machine silane carries out 5~120min of reaction under agitation at room temperature, takes out and places in a vacuum drying oven, 50~
Solidified and dried 0.5~2h at 130 DEG C, super-hydrophobic blown rubber is made.
The adjustment of preparation method is carried out using the technological parameter of the content of present invention, and hydrophobicity is carried out to blown rubber respectively and is changed
Property is as follows:
Embodiment 1
Commercially available foam sponge is first cut into the fritter of 20 × 15 × 5mm, be put into dehydrated alcohol and deionized water respectively into
Row ultrasonic cleaning 60h, alternately cleaning 4 times take out after cleaning to remove foam sponge surface and internal impurity and are put into vacuum
2h is dried in drying box, immerses in the coarsening solution concentrated sulfuric acid (98wt%) after drying, roughening 4h is carried out under 20-25 degrees Celsius of room temperature,
So that coarsening solution introduces hydrophilic radical on foam sponge surface, take out after roughening and cleaned repeatedly with deionized water, removes
Extra coarsening solution places into vacuum oven drying 2h, is then dipped in 50mL n-hexane, first adds into reaction system
Enter 500 μ L methyl trichlorosilanes, adds 500 μ L deionized waters and carried out at room temperature under the stirring condition of 200rpm revolving speed
60min is reacted, takes out and places in a vacuum drying oven, solidified and dried 2h at 105 DEG C, obtain super-hydrophobic foaming rubber
Glue, with water contact angle up to 154 °.
Embodiment 2
Commercially available foam sponge is first cut into the fritter of 20 × 15 × 5mm, be put into dehydrated alcohol and deionized water respectively into
Row ultrasonic cleaning 60h, alternately cleaning 4 times take out after cleaning to remove foam sponge surface and internal impurity and are put into vacuum
2h is dried in drying box, is immersed in the coarsening solution concentrated sulfuric acid after drying, roughening 4h is carried out at room temperature, so that coarsening solution is in foam sponge
Surface introduces hydrophilic radical, takes out after roughening and is cleaned repeatedly with deionized water, removes extra coarsening solution, places into true
Empty drying box dries 2h, is then dipped in 50mL toluene, and 500 μ L methyl trichlorosilanes are first added into reaction system, then
500 μ L deionized waters are added, under the stirring condition of 200rpm revolving speed, carry out reaction 60min at room temperature, taking-up is placed in true
In empty drying box, solidified and dried 2h at 105 DEG C, obtain super-hydrophobic blown rubber, with water contact angle up to 151 °.This reality
It applies a difference from Example 1 to be, reaction medium is changed to toluene, dosage 50mL.
Embodiment 3
Commercially available foam sponge is first cut into the fritter of 20 × 15 × 5mm, be put into dehydrated alcohol and deionized water respectively into
Row ultrasonic cleaning 60h, alternately cleaning 4 times take out after cleaning to remove foam sponge surface and internal impurity and are put into vacuum
2h is dried in drying box, is immersed in the coarsening solution concentrated sulfuric acid after drying, roughening 4h is carried out at room temperature, so that coarsening solution is in foam sponge
Surface introduces hydrophilic radical, takes out after roughening and is cleaned repeatedly with deionized water, removes extra coarsening solution, places into true
Empty drying box dries 2h, is then dipped in 50mL n-hexane, and 500 μ L trim,ethylchlorosilanes are first added into reaction system,
It adds 500 μ L deionized waters and carries out reaction 60min at room temperature under the stirring condition of 200rpm revolving speed, taking-up is placed in
In vacuum oven, solidified and dried 2h at 105 DEG C, obtain super-hydrophobic blown rubber, with water contact angle up to 154 °.This
Embodiment difference from Example 1 is that organosilan is changed to trim,ethylchlorosilane, and dosage is 500 μ L.
Embodiment 4
Commercially available foam sponge is first cut into the fritter of 20 × 15 × 5mm, be put into dehydrated alcohol and deionized water respectively into
Row ultrasonic cleaning 60h, alternately cleaning 4 times take out after cleaning to remove foam sponge surface and internal impurity and are put into vacuum
2h is dried in drying box, is immersed in the coarsening solution concentrated sulfuric acid after drying, roughening 4h is carried out at room temperature, so that coarsening solution is in foam sponge
Surface introduces hydrophilic radical, takes out after roughening and is cleaned repeatedly with deionized water, removes extra coarsening solution, places into true
Empty drying box dries 2h, is then dipped in 50mL n-hexane, and 500 μ L dodecyl trichlorine silicon are first added into reaction system
Alkane adds 500 μ L deionized waters and carries out reaction 40min at room temperature under the stirring condition of 200rpm revolving speed, and taking-up is put
It is placed in a vacuum drying oven, is solidified and dried 2h at 105 DEG C, obtain super-hydrophobic blown rubber, reached with water contact angle
153°.This embodiment differs from embodiment 1 in that the reaction time in reaction medium is changed to 40min, organosilan changes
For dodecyltrichlorosilane.
Embodiment 5
Commercially available foam sponge is first cut into the fritter of 20 × 15 × 5mm, be put into dehydrated alcohol and deionized water respectively into
Row ultrasonic cleaning 60h, alternately cleaning 4 times take out after cleaning to remove foam sponge surface and internal impurity and are put into vacuum
2h is dried in drying box, is immersed in the coarsening solution concentrated sulfuric acid after drying, roughening 4h is carried out at room temperature, so that coarsening solution is in foam sponge
Surface introduces hydrophilic radical, takes out after roughening and is cleaned repeatedly with deionized water, removes extra coarsening solution, places into true
Empty drying box dries 2h, is then dipped in 50mL n-hexane, is first added 500 μ L deionized waters into reaction system, then plus
Enter 500 μ L methyl trichlorosilanes and carry out reaction 60min at room temperature under the stirring condition of 200rpm revolving speed, taking-up is placed in
In vacuum oven, solidified and dried 2h at 105 DEG C, obtain super-hydrophobic blown rubber, with water contact angle up to 154 °.This
Embodiment and Examples 1 to 4 the difference is that, the order of addition of organosilan and deionized water is changed to that deionization is first added
Water adds organosilan.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (8)
1. a kind of preparation method of super-hydrophobic blown rubber, which is characterized in that carry out as steps described below:
Step 1, blown rubber is placed in dehydrated alcohol and is cleaned by ultrasonic, taking-up, which places into deionized water, carries out ultrasound clearly
It washes, so carries out alternately cleaning, until surface and internal impurity are properly washed, taken out after cleaning, in vacuum oven
Middle drying；The foam pattern of blown rubber is open-cell foaming；
Step 2, blown rubber step 1 handled immerses in coarsening solution, is roughened under 20-25 degrees Celsius of room temperature, so that slightly
Change liquid and introduce hydrophilic radical on blown rubber surface, takes out after roughening and cleaned repeatedly with deionized water, removed remaining
Coarsening solution places into vacuum oven and dries the blown rubber being roughened；In step 2, coarsening solution is with strong oxidizing property
Solution, such as the concentrated sulfuric acid of mass percent 98wt%；The mixing of the concentrated sulfuric acid and potassium permanganate of mass percent 98wt%
The mass ratio of object, the concentrated sulfuric acid and potassium permanganate is (1-2): (0.5-1)；The concentrated sulfuric acid of mass percent 98wt% and with three oxygen
Change the mixture of two chromium, the mass ratio of the concentrated sulfuric acid and chrome green is (1-2): (0.5-1)；Mass percent 98wt%'s
The mixture of the concentrated sulfuric acid, potassium permanganate and chrome green, the mass ratio of the concentrated sulfuric acid, potassium permanganate and chrome green are (1-
2): (0.5-1): (0.5-1)；
Step 3, the blown rubber after step 2 roughening is immersed in reaction medium, organosilan and deionized water, stirring bar is added
It is reacted, the super-hydrophobic blown rubber is made and is solidified under part；The reaction medium be n-hexane, hexamethylene, two
Chloromethanes, normal heptane, normal octane, benzene or dimethylbenzene；The organosilan is trim,ethylchlorosilane, dimethyldichlorosilane, first
Base trichlorosilane, ethyl trichlorosilane or n-octyl trichlorosilane；Percentage by volume of the organosilan in reaction medium be
0.05~5vol%；The volume ratio of organosilan and deionized water is 1:0.1~1:10.
2. a kind of preparation method of super-hydrophobic blown rubber according to claim 1, which is characterized in that in step 1,
The time being cleaned by ultrasonic in dehydrated alcohol is 30~90min, and preferably 30-60min, ultrasonic power is 100-150w；?
The time being cleaned by ultrasonic in deionized water is 30~90min, and preferably 30-60min, ultrasonic power is 100-150w；?
When alternately clean, alternately wash number is 1~5 time.
3. a kind of preparation method of super-hydrophobic blown rubber according to claim 1, which is characterized in that in step 2, institute
The reaction condition for stating roughening is that 0.5~6h is reacted under 20-25 degrees Celsius of room temperature, preferably 2-5 hours.
4. a kind of preparation method of super-hydrophobic blown rubber according to claim 1, which is characterized in that in step 3, first
Organosilan is added, adds deionized water, or deionized water is first added, adds organosilan.
5. a kind of preparation method of super-hydrophobic blown rubber according to claim 1, which is characterized in that in step 3, have
Percentage by volume of the machine silane in reaction medium is 1-4vol%, and the volume ratio of organosilan and deionized water is 1:(3-
8)。
6. a kind of preparation method of super-hydrophobic blown rubber according to claim 1, which is characterized in that in step 3, stir
Mixing revolving speed is 50~500 turns per minute, 100-300 turns preferably per minute.
7. a kind of preparation method of super-hydrophobic blown rubber according to claim 1, which is characterized in that in step 3, stir
It is 5~120min, preferably 30-60min that the reaction time is carried out under the conditions of mixing；Temperature is 20-25 degrees Celsius of room temperature.
8. a kind of preparation method of super-hydrophobic blown rubber according to claim 1, which is characterized in that in step 3,
It is reacted, is placed the blown rubber of surface covering hydrophobic silicone in a vacuum drying oven at room temperature after reaction, consolidate
Change drying, super-hydrophobic blown rubber is made, solidification temperature is 50~130 DEG C, preferably 60-100 degrees Celsius.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710551396.2A CN109206658A (en) | 2017-07-07 | 2017-07-07 | A kind of preparation method of super-hydrophobic blown rubber |
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| CN110669278A (en) * | 2019-11-17 | 2020-01-10 | 斯莱达医疗用品（惠州）有限公司 | Pipe for effectively reducing condensate water of breathing pipeline |
| CN115607748A (en) * | 2022-10-09 | 2023-01-17 | 电子科技大学长三角研究院(湖州) | Blood-compatible liquid-like super-smooth surface and preparation method thereof |
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