CN107384104A - A kind of super hydrophobic coating and its preparation method and application - Google Patents
A kind of super hydrophobic coating and its preparation method and application Download PDFInfo
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- CN107384104A CN107384104A CN201710567491.1A CN201710567491A CN107384104A CN 107384104 A CN107384104 A CN 107384104A CN 201710567491 A CN201710567491 A CN 201710567491A CN 107384104 A CN107384104 A CN 107384104A
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/047—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with fluoropolymers
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- D06N2209/00—Properties of the materials
- D06N2209/14—Properties of the materials having chemical properties
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- D06N2209/00—Properties of the materials
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Abstract
The present invention discloses a kind of super hydrophobic coating, it is by dodecafluoroheptyl methacrylate, methyl propenoic acid glycidyl, azodiisobutyronitrile and sodium hydrogensulfite is reacted forms a kind of polymer, the polymer is PGMA r PDFMA, and the invention also discloses the preparation method and application of above-mentioned super hydrophobic coating.The super hydrophobic coating of the present invention has stronger durability in use, and super hydrophobic coating preparation method of the present invention is simple, and application is convenient to, and can form super hydrophobic coating layer in fabric face.
Description
Technical field
The invention belongs to hydrophobic coating technical field, is related to a kind of super hydrophobic coating (polymer P GMA-r-PDFMA), this
Invention further relates to the preparation method and application of above-mentioned super hydrophobic coating.
Background technology
Liquid in the wetability of body surface is weighed by the size of surface static contact angle, works as body surface
Static contact angle is higher than 150 °, and such a body surface is referred to as super hydrophobic surface.The surface wettability of object is mainly by microcosmic knot
What structure and chemical composition together decided on.Manually preparing super hydrophobic surface mainly has two kinds of approach to be respectively：(1) polished by physics
Or the method for chemical experiment constructs coarse result in the surface of solids；(2) on a solid surface in grafting low chemical energy point
Son.
In recent years, super hydrophobic surface causes the very big concern of all trades and professions because of performances such as its automatically cleaning and water repellents.With lotus leaf
Similar, water droplet not only easily tumbles in super hydrophobic surface, and can take away the dust granule on surface during tumbling, from
And play self-cleaning effect.Existing super-hydrophobic self-cleaning coating has waterproof, antifog, snow defence, anti-pollution, resist blocking and that, antioxygen
The many merits such as change and anticorrosion, can be widely applied to agricultural, military project, building, traffic, weaving, medical treatment, anti-corrosion and daily life
Deng field.But find in long-term use：The problem of durability is poor mostly be present in existing super-hydrophobic self-cleaning coating.
The content of the invention
The first object of the present invention is to provide a kind of super hydrophobic coating (polymer P GMA-r-PDFMA) have in use
There is stronger durability.
The second object of the present invention is the preparation method for providing above-mentioned super hydrophobic coating.
The third object of the present invention is to provide application process of the above-mentioned super hydrophobic coating on fabric.
The first technical scheme of the present invention is
By dodecafluoroheptyl methacrylate (DFMA), methyl propenoic acid glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite
Reacted to form a kind of polymer, the polymer is PGMA-r-PDFMA, and its reaction equation is as follows：
Second of technical scheme of the present invention is the preparation side of super hydrophobic coating (polymer P GMA-r-PDFMA)
Method, specifically implement according to following steps：
Step 1, methyl propenoic acid glycidyl is taken, methyl propenoic acid glycidyl is filtered using alumina chromatographic column,
Remove polymerization inhibitor；
Step 2, dodecafluoroheptyl methacrylate, the methyl propenoic acid glycidyl after step 1 processing are weighed respectively
And azodiisobutyronitrile and sodium hydrogensulfite；
Step 3, all materials weighed in step 2 are added in container together, then tetrahydrofuran are added into container,
The container is sealed and is passed through nitrogen, discharges the oxygen in container；
Step 4, after the completion for the treatment of step 3, whole container is positioned in oil bath constant temperature pot and heated, and under the protection of nitrogen
Open magnetic agitation, make dodecafluoroheptyl methacrylate in container, methyl propenoic acid glycidyl, azodiisobutyronitrile and
Sodium hydrogensulfite fully reacts, and question response pours out the reactant formed in container after terminating, and is stood under normal temperature, treats tetrahydrochysene furan
Mutter untill being evaporated completely, obtain super hydrophobic coating PGMA-r-PDFMA, its reaction equation is as follows：
The characteristics of second of technical scheme of the invention, also resides in：
In step 2：Dodecafluoroheptyl methacrylate, the methyl propenoic acid glycidyl after step 1 processing and idol
Mol ratio between nitrogen bis-isobutyronitrile and sodium hydrogensulfite is 3~9：1：0.04~0.2：0.04~0.2.
In step 4：Temperature in oil bath constant temperature pot is 65 DEG C~75 DEG C, and the magnetic agitation time is 35min~45min.
The third technical scheme of the present invention is that super hydrophobic coating (polymer P GMA-r-PDFMA) is on fabric
Application process, specifically implement according to following steps：
Step 1, methyl propenoic acid glycidyl is taken, methyl propenoic acid glycidyl is filtered using alumina chromatographic column,
Remove polymerization inhibitor；
Step 2, dodecafluoroheptyl methacrylate, the methyl propenoic acid glycidyl after step 1 processing are weighed respectively
And azodiisobutyronitrile and sodium hydrogensulfite；
Step 3, all materials weighed in step 2 are added in container together, then tetrahydrofuran are added into container,
The container is sealed and is passed through nitrogen, discharges the oxygen in container；
Step 4, after the completion for the treatment of step 3, whole container is positioned in oil bath constant temperature pot and heated, and under the protection of nitrogen
Open magnetic agitation, make dodecafluoroheptyl methacrylate in container, methyl propenoic acid glycidyl, azodiisobutyronitrile and
Sodium hydrogensulfite fully reacts, and question response pours out the reactant formed in container after terminating, and is stood under normal temperature, treats tetrahydrochysene furan
Mutter untill being evaporated completely, obtain super hydrophobic coating PGMA-r-PDFMA, its reaction equation is as follows：
Step 5, fabric first cleaned with detergent, 4h~6h is soaked in absolute ethyl alcohol, then rinsed with clear water dry
Only, finally dry, obtain the fabric of cleaning；
Step 6, the super hydrophobic coating PGMA-r-PDFMA obtained through step 4 first dissolved with tetrahydrofuran, added
0.5mL~1mL triethylamines, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration；Then will be obtained through step 5 clean
Net fabric is soaked in the modification liquid made；Finally dry, one layer of super hydrophobic coating (PGMA- is loaded with fabric face
R-PDFMA) layer.
The characteristics of the third technical scheme of the invention, also resides in：
In step 2：Dodecafluoroheptyl methacrylate, the methyl propenoic acid glycidyl after step 1 processing and idol
Mol ratio between nitrogen bis-isobutyronitrile and sodium hydrogensulfite is 3~9：1：0.04~0.2：0.04~0.2.
In step 4：Temperature in oil bath constant temperature pot is 65 DEG C~75 DEG C, and the magnetic agitation time is 35min~45min.
In step 5：Wash number is 3 times~5 times, and drying temperature is 70 DEG C~90 DEG C.
In step 6：Soak time is 1h~24h, and drying temperature is 110 DEG C~130 DEG C.
The beneficial effects of the present invention are：
The super hydrophobic coating (polymer P GMA-r-PDFMA) of the present invention is good with durability in use, acidproof, resistance to
Many advantages, such as alkali and washing fastness.
The preparation method of super hydrophobic coating (polymer P GMA-r-PDFMA) of the present invention has the following advantages that：(1) one is used
High fluorine-containing and containing epoxy radicals polymer is prepared in footwork, and this method is simple, without multi-stage synthesis polymer；(2) preparation
Method has universality, available for the processing of multiple fiber or material, it is all had superhydrophobic characteristic.
Super hydrophobic coating (polymer P GMA-r-PDFMA) of the present invention is applied on fabric, can be formed on fabric super thin
Water coating, the super-hydrophobic coat have had the advantage that：(1) hydrophobic performance of the super-hydrophobic coat prepared by is stable, permanent effective
And with good acidproof, alkaline-resisting, salt tolerant, resistance to supersound washing performance；(2) super-hydrophobic coat prepared by, which has, preferably to be repeated
Utilization ability and service life.
Brief description of the drawings
Fig. 1 is the electron microscope that common bafta is shot under 5000 times of ESEMs；
Fig. 2 is the electron microscope that common bafta is shot under 20000 times of ESEMs；
The super hydrophobic coating that Fig. 3 is the present invention is shot in surface of cotton fabric formation dope layer after under 1000 times of ESEMs
Electron microscope；
The super hydrophobic coating that Fig. 4 is the present invention is clapped in surface of cotton fabric formation dope layer after under 10000 times of ESEMs
The electron microscope taken the photograph；
Fig. 5 is the super hydrophobic coating of the invention water contact angle test chart after surface of cotton fabric forms dope layer；
Fig. 6 is that super hydrophobic coating of the invention the first durability test result after surface of cotton fabric forms dope layer is bent
Line；
Fig. 7 is that super hydrophobic coating of the invention second of durability test result after surface of cotton fabric forms dope layer is bent
Line；
Fig. 8 is that super hydrophobic coating of the invention the third durability test result after surface of cotton fabric forms dope layer is bent
Line；
Fig. 9 is that super hydrophobic coating of the invention the 4th kind of durability test result after surface of cotton fabric forms dope layer is bent
Line.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of super hydrophobic coating of the present invention, is sweet by dodecafluoroheptyl methacrylate (DFMA), Glycidyl methacrylate
Oily (GMA), azodiisobutyronitrile and a kind of reacted polymer of composition of sodium hydrogensulfite, the polymer is PGMA-r-PDFMA,
Its reaction equation is as follows：
A kind of preparation method of super hydrophobic coating of the present invention, specifically implements according to following steps：
Step 1, methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina layer
Post filtering is analysed, removes polymerization inhibitor.
Step 2, according to mol ratio be 3~9：1：0.04~0.2：0.04~0.2 weighs the difluoro of methacrylic acid ten respectively
Heptyl ester (DFMA), methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and bisulfite after step 1 processing
Sodium；
Wherein, dodecafluoroheptyl methacrylate (DFMA) and methyl propenoic acid glycidyl (GMA) are raw material, azo two
Isobutyronitrile and sodium hydrogensulfite are initiator.
Step 3, all materials weighed in step 2 are added in container together, then tetrahydrofuran are added into container,
The container is sealed and is passed through nitrogen 45min~55min, it is therefore intended that：Discharge the oxygen in container；
Wherein, tetrahydrofuran is solvent, and nitrogen is protection gas, and container can use round-bottomed flask.
Step 4, after the completion for the treatment of step 3, whole container is positioned in oil bath constant temperature pot and heated, and under the protection of nitrogen
Magnetic agitation is opened, makes dodecafluoroheptyl methacrylate (DFMA) in container, methyl propenoic acid glycidyl (GMA), even
Nitrogen bis-isobutyronitrile and sodium hydrogensulfite fully react, and question response pours out the reactant formed in container after terminating, under normal temperature
Stand, untill treating that tetrahydrofuran is evaporated completely, (being usually 1h~3h) obtains super hydrophobic coating PGMA-r-PDFMA；
Wherein, the temperature in oil bath constant temperature pot is 65 DEG C~75 DEG C, and the magnetic agitation time is 35min~45min；
Its reaction equation is as follows：
A kind of application process of the super hydrophobic coating of the present invention on fabric, specifically implements according to following steps：
Step 1, methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina layer
Post filtering is analysed, removes polymerization inhibitor.
Step 2, according to mol ratio be 3~9：1：0.04~0.2：0.04~0.2 weighs the difluoro of methacrylic acid ten respectively
Heptyl ester (DFMA), methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and bisulfite after step 1 processing
Sodium；
Wherein, dodecafluoroheptyl methacrylate (DFMA) and methyl propenoic acid glycidyl (GMA) are raw material, azo two
Isobutyronitrile and sodium hydrogensulfite are initiator.
Step 3, all materials weighed in step 2 are added in container together, then tetrahydrofuran are added into container,
The container is sealed and is passed through nitrogen 45min~55min, it is therefore intended that：Discharge the oxygen in container；
Wherein, tetrahydrofuran is solvent, and nitrogen is protection gas, and container can use round-bottomed flask.
Step 4, after the completion for the treatment of step 3, whole container is positioned in oil bath constant temperature pot and heated, and under the protection of nitrogen
Magnetic agitation is opened, makes dodecafluoroheptyl methacrylate (DFMA) in container, methyl propenoic acid glycidyl (GMA), even
Nitrogen bis-isobutyronitrile and sodium hydrogensulfite fully react, and question response pours out the reactant formed in container after terminating, under normal temperature
Stand, untill treating that tetrahydrofuran is evaporated completely, (being usually 1h~3h) obtains super hydrophobic coating PGMA-r-PDFMA；
Wherein, the temperature in oil bath constant temperature pot is 65 DEG C~75 DEG C, and the magnetic agitation time is 35min~45min；
Its reaction equation is as follows：
Step 5, fabric first cleaned with detergent, 4h~6h is soaked in absolute ethyl alcohol, then rinsed with clear water dry
Only, finally dry, obtain the fabric of cleaning；
Wherein, wash number is 3 times~5 times, and drying temperature is 70 DEG C~90 DEG C.
Step 6, the super hydrophobic coating PGMA-r-PDFMA obtained through step 4 first dissolved with tetrahydrofuran, added
0.5mL~1mL triethylamines, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration；Then will be obtained through step 5 clean
Net fabric is soaked in the modification liquid made；Finally dry, one layer of super hydrophobic coating (PGMA- is loaded with fabric face
R-PDFMA) layer；
Wherein, soak time is 1h~24h, and drying temperature is 110 DEG C~130 DEG C.
Embodiment 1
The preparation method of super hydrophobic coating：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 9 according to mol ratio：1：0.06：0.1 weighs dodecafluoroheptyl methacrylate (DFMA), processing respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite afterwards；By all materials weighed together
It is added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen 45min,
Discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 65 DEG C and heated, and in nitrogen
Magnetic agitation 35min is opened under the protection of gas, makes dodecafluoroheptyl methacrylate (DFMA), the metering system in round-bottomed flask
Acid glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite are fully reacted, and question response will be formed after terminating in round-bottomed flask
Reactant pour out, stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtain super hydrophobic coating PGMA-r-PDFMA, its
Reaction equation is as follows：
Application process of the super hydrophobic coating on fabric, specifically implements according to following steps：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 9 according to mol ratio：1：0.06：0.1 weighs dodecafluoroheptyl methacrylate (DFMA), processing respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite afterwards；By all materials weighed together
It is added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen 45min,
Discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 65 DEG C and heated, and in nitrogen
Magnetic agitation 35min is opened under the protection of gas, makes dodecafluoroheptyl methacrylate (DFMA), the metering system in round-bottomed flask
Acid glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite are fully reacted, and question response will be formed after terminating in round-bottomed flask
Reactant pour out, stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtain super hydrophobic coating PGMA-r-PDFMA, its
Reaction equation is as follows：
Fabric is first cleaned 3 times with detergent, 4h is soaked in absolute ethyl alcohol, is then rinsed well with clear water, finally
Dried under the conditions of 70 DEG C, obtain the fabric of cleaning；Obtained super hydrophobic coating PGMA-r-PDFMA is first molten with tetrahydrofuran
Solution, 1mL triethylamines are added, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration, then the fabric of cleaning is soaked in and matched somebody with somebody
In the modification liquid made, soak time 1h, most dried under the conditions of 110 DEG C, fabric face be loaded with one layer it is super-hydrophobic
Coating (PGMA-r-PDFMA) layer.
Embodiment 2
The preparation method of super hydrophobic coating：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 8 according to mol ratio：1：0.05：0.15 weighs dodecafluoroheptyl methacrylate (DFMA), place respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite after reason；The all materials one that will be weighed
Rise and be added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen
55min, discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 75 DEG C and heated,
And magnetic agitation 45min is opened under the protection of nitrogen, make dodecafluoroheptyl methacrylate (DFMA) in round-bottomed flask, first
Base glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite fully react, question response terminate after by round-bottomed flask
The reactant of interior formation is poured out, and is stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtains super hydrophobic coating PGMA-r-
PDFMA, its reaction equation are as follows：
Application process of the super hydrophobic coating on fabric, specifically implements according to following steps：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 8 according to mol ratio：1：0.05：0.15 weighs dodecafluoroheptyl methacrylate (DFMA), place respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite after reason；The all materials one that will be weighed
Rise and be added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen
55min, discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 75 DEG C and heated,
And magnetic agitation 45min is opened under the protection of nitrogen, make dodecafluoroheptyl methacrylate (DFMA) in round-bottomed flask, first
Base glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite fully react, question response terminate after by round-bottomed flask
The reactant of interior formation is poured out, and is stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtains super hydrophobic coating PGMA-r-
PDFMA, its reaction equation are as follows：
Fabric is first cleaned 5 times with detergent, 6h is soaked in absolute ethyl alcohol, is then rinsed well with clear water, finally
Dried under the conditions of 90 DEG C, obtain the fabric of cleaning；Obtained super hydrophobic coating PGMA-r-PDFMA is first molten with tetrahydrofuran
Solution, 0.85mL triethylamines are added, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration, then the fabric of cleaning is soaked
In the modification liquid made, soak time 5h, most dried under the conditions of 120 DEG C, being loaded with one layer in fabric face surpasses
Hydrophobic coating (PGMA-r-PDFMA) layer.
Embodiment 3
The preparation method of super hydrophobic coating：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 6 according to mol ratio：1：0.07：0.09 weighs dodecafluoroheptyl methacrylate (DFMA), place respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite after reason；The all materials one that will be weighed
Rise and be added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen
48min, discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 68 DEG C and heated,
And magnetic agitation 38min is opened under the protection of nitrogen, make dodecafluoroheptyl methacrylate (DFMA) in round-bottomed flask, first
Base glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite fully react, question response terminate after by round-bottomed flask
The reactant of interior formation is poured out, and is stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtains super hydrophobic coating PGMA-r-
PDFMA, its reaction equation are as follows：
Application process of the super hydrophobic coating on fabric, specifically implements according to following steps：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 6 according to mol ratio：1：0.07：0.09 weighs dodecafluoroheptyl methacrylate (DFMA), place respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite after reason；The all materials one that will be weighed
Rise and be added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen
48min, discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 68 DEG C and heated,
And magnetic agitation 38min is opened under the protection of nitrogen, make dodecafluoroheptyl methacrylate (DFMA) in round-bottomed flask, first
Base glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite fully react, question response terminate after by round-bottomed flask
The reactant of interior formation is poured out, and is stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtains super hydrophobic coating PGMA-r-
PDFMA, its reaction equation are as follows：
Fabric is first cleaned 3 times with detergent, 4.5h is soaked in absolute ethyl alcohol, is then rinsed well with clear water, most
Dried under the conditions of 75 DEG C, obtain the fabric of cleaning；Obtained super hydrophobic coating PGMA-r-PDFMA is first used into tetrahydrofuran
Dissolving, 0.75mL triethylamines are added, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration, then the fabric of cleaning is soaked
Steep in the modification liquid made, soak time 10h, most dried under the conditions of 115 DEG C, one layer is loaded with fabric face
Super hydrophobic coating (PGMA-r-PDFMA) layer.
Embodiment 4
The preparation method of super hydrophobic coating：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 5 according to mol ratio：1：0.04：0.2 weighs dodecafluoroheptyl methacrylate (DFMA), processing respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite afterwards；By all materials weighed together
It is added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen 50min,
Discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 70 DEG C and heated, and in nitrogen
Magnetic agitation 40min is opened under the protection of gas, makes dodecafluoroheptyl methacrylate (DFMA), the metering system in round-bottomed flask
Acid glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite are fully reacted, and question response will be formed after terminating in round-bottomed flask
Reactant pour out, stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtain super hydrophobic coating PGMA-r-PDFMA, its
Reaction equation is as follows：
Application process of the super hydrophobic coating on fabric, specifically implements according to following steps：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 5 according to mol ratio：1：0.04：0.2 weighs dodecafluoroheptyl methacrylate (DFMA), processing respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite afterwards；By all materials weighed together
It is added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen 50min,
Discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 70 DEG C and heated, and in nitrogen
Magnetic agitation 40min is opened under the protection of gas, makes dodecafluoroheptyl methacrylate (DFMA), the metering system in round-bottomed flask
Acid glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite are fully reacted, and question response will be formed after terminating in round-bottomed flask
Reactant pour out, stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtain super hydrophobic coating PGMA-r-PDFMA, its
Reaction equation is as follows：
Fabric is first cleaned 4 times with detergent, 5h is soaked in absolute ethyl alcohol, is then rinsed well with clear water, finally
Dried under the conditions of 73 DEG C, obtain the fabric of cleaning；Obtained super hydrophobic coating PGMA-r-PDFMA is first molten with tetrahydrofuran
Solution, 0.6mL triethylamines are added, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration, then the fabric of cleaning is soaked in
In the modification liquid made, soak time be 15h most dried under the conditions of 110 DEG C, fabric face be loaded with one layer it is super thin
Water paint (PGMA-r-PDFMA) layer.
Embodiment 5
The preparation method of super hydrophobic coating：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 3 according to mol ratio：1：0.08：0.08 weighs dodecafluoroheptyl methacrylate (DFMA), place respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite after reason；The all materials one that will be weighed
Rise and be added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen
52min, discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 72 DEG C and heated,
And magnetic agitation 42min is opened under the protection of nitrogen, make dodecafluoroheptyl methacrylate (DFMA) in round-bottomed flask, first
Base glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite fully react, question response terminate after by round-bottomed flask
The reactant of interior formation is poured out, and is stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtains super hydrophobic coating PGMA-r-
PDFMA, its reaction equation are as follows：
Application process of the super hydrophobic coating on fabric, specifically implements according to following steps：
Methyl propenoic acid glycidyl (GMA) is taken, methyl propenoic acid glycidyl (GMA) is used into alumina chromatographic column mistake
Filter, remove polymerization inhibitor；It is 3 according to mol ratio：1：0.08：0.08 weighs dodecafluoroheptyl methacrylate (DFMA), place respectively
Methyl propenoic acid glycidyl (GMA) and azodiisobutyronitrile and sodium hydrogensulfite after reason；The all materials one that will be weighed
Rise and be added in round-bottomed flask, then tetrahydrofuran is added into round-bottomed flask, the round-bottomed flask is sealed and is passed through nitrogen
52min, discharge the oxygen in round-bottomed flask；Whole round-bottomed flask is positioned in the oil bath constant temperature pot that temperature is 72 DEG C and heated,
And magnetic agitation 42min is opened under the protection of nitrogen, make dodecafluoroheptyl methacrylate (DFMA) in round-bottomed flask, first
Base glycidyl (GMA), azodiisobutyronitrile and sodium hydrogensulfite fully react, question response terminate after by round-bottomed flask
The reactant of interior formation is poured out, and is stood under normal temperature, untill treating that tetrahydrofuran is evaporated completely, obtains super hydrophobic coating PGMA-r-
PDFMA, its reaction equation are as follows：
Fabric is first cleaned 4 times with detergent, 5.5h is soaked in absolute ethyl alcohol, is then rinsed well with clear water, most
Dried under the conditions of 75 DEG C, obtain the fabric of cleaning；Obtained super hydrophobic coating PGMA-r-PDFMA is first used into tetrahydrofuran
Dissolving, 0.5mL triethylamines are added, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration, then the fabric of cleaning is soaked
In the modification liquid made, soak time 24h, most dried under the conditions of 115 DEG C, being loaded with one layer in fabric face surpasses
Hydrophobic coating (PGMA-r-PDFMA) layer.
As shown in figure 1, under 5000 times of multiplication factors, it can be seen that：Substantially put down on the surface that common cotton-textile fibres interweave
Sliding and close structure；As shown in Fig. 2 it can be seen that under 20000 times of multiplication factors：The surface of single fiber in common bafta
The pattern of unusual light is presented, this can ensure that bafta has many excellent properties in itself, such as：Gas permeability.
The super hydrophobic coating (polymer P GMA-r-PDFMA) of the present invention is applied on bafta, in surface of cotton fabric shape
Into one layer of super hydrophobic coating layer；As shown in Figures 3 and 4, it can be seen that：There are a large amount of small projections on the surface of bafta,
But the gap between cotton-textile fibres is still it can be clearly seen that this shows：Super hydrophobic coating is formed in surface of cotton fabric
Outward appearance will not produce great changes after layer, not influence the gas permeability of bafta.
The super hydrophobic coating (polymer P GMA-r-PDFMA) of the present invention is applied on bafta, in surface of cotton fabric shape
Into one layer of super hydrophobic coating layer, its ultra-hydrophobicity is tested, its result is as shown in figure 5, as can be seen from Figure 5：Cover
Have that bafta and the common bafta of the super hydrophobic coating layer are entirely different, and WCA can reach 163 °, and this shows：It is super thin to be covered with this
The bafta of water paint layer obtains ultra-hydrophobicity.
The super hydrophobic coating (polymer P GMA-r-PDFMA) of the present invention is applied on bafta, in surface of cotton fabric shape
Into one layer of super hydrophobic coating layer, following test has been carried out respectively to the durability of the super hydrophobic coating layer of formation：
The first durability test, as shown in Figure 6：
It is different that ultrasound in ultrasonic washer is placed in after the cotton-spinning fabric of surface formation super hydrophobic coating layer is cut into one piece
Time, it is to be dried in 120 DEG C of baking oven to place into temperature, takes 5 different orientation survey contact angles at random, is recorded average
Value；
As can be seen from Figure 6：With the extension of supersound washing time, surface forms the cotton-spinning fabric of super hydrophobic coating layer
On water contact angle slightly decline, but the bafta has remained in that preferable hydrophobic performance；In supersound washing after 150min,
The water contact angle of the cotton-spinning fabric remains to be kept for 154 °.
Second of durability test, as shown in Figure 7：
The cotton-spinning fabric that surface is formed to super hydrophobic coating layer cuts the HCl solution that immersion concentration is 0.01g/mL after one piece
Middle a period of time, place into 120 DEG C of baking ovens and dry, take 5 different orientation survey contact angles at random, record average value；
As can be seen from Figure 7：The hydrophobic performance for the hydrophobic coating layer that acid solution is formed to surface of cotton fabric has necessarily
Influence, but soak 150min after, the bafta still shows super-hydrophobicity.
The third durability test, as shown in Figure 8：
It is 0.01g/mL Na to immerse concentration after the cotton-spinning fabric of surface formation super hydrophobic coating layer is cut into one piece2CO3It is molten
A period of time, places into 120 DEG C of baking ovens and dries, take 5 different orientation survey contact angles at random, record average value in liquid；
As can be seen from Figure 8：Soaked in alkaline solution a period of time, surface forms the cotton spinning of super hydrophobic coating layer
The hydrophobic performance of thing is gradually reduced, but water contact angle remains to reach 151 ° after 125min.
4th kind of durability test, as shown in Figure 9：
It is 0.01g/mLNaOH solution to immerse concentration after the cotton-spinning fabric of surface formation super hydrophobic coating layer is cut into one piece
For a period of time, place into 120 DEG C of baking ovens and dry, take 5 different orientation survey contact angles at random, record average value；
As can be seen from Figure 9：Alkaline solution has destruction to the super hydrophobic coating layer that surface of cotton fabric is formed, and dredges
Water-based to increase gradual decrease over time, after soaking 100min in NaOH solution, hydrophobic angle reduces to 148 °, but still shows
Go out with hydrophobic performance.
Claims (9)
- A kind of 1. super hydrophobic coating, it is characterised in that be by dodecafluoroheptyl methacrylate, methyl propenoic acid glycidyl, Azodiisobutyronitrile and sodium hydrogensulfite is reacted forms a kind of polymer, the polymer are PGMA-r-PDFMA, its reaction equation It is as follows：
- 2. a kind of preparation method of super hydrophobic coating, it is characterised in that specifically implement according to following steps：Step 1, methyl propenoic acid glycidyl is taken, methyl propenoic acid glycidyl is filtered using alumina chromatographic column, removed Polymerization inhibitor；Step 2, weigh respectively dodecafluoroheptyl methacrylate, through step 1 processing after methyl propenoic acid glycidyl and Azodiisobutyronitrile and sodium hydrogensulfite；Step 3, all materials weighed in step 2 are added in container together, then tetrahydrofuran is added into container, by this Container seals and is passed through nitrogen, discharges the oxygen in container；Step 4, after the completion for the treatment of step 3, whole container is positioned in oil bath constant temperature pot and heated, and opened under the protection of nitrogen Magnetic agitation, make dodecafluoroheptyl methacrylate, methyl propenoic acid glycidyl, azodiisobutyronitrile and sulfurous in container Sour hydrogen sodium fully reacts, and question response pours out the reactant formed in container after terminating, and is stood under normal temperature, treats that tetrahydrofuran is waved Untill distributing, super hydrophobic coating PGMA-r-PDFMA is obtained, its reaction equation is as follows：
- 3. the preparation method of a kind of super hydrophobic coating according to claim 2, it is characterised in that in the step 2：Methyl Dodecafluorhe-ptylacrylate, methyl propenoic acid glycidyl and azodiisobutyronitrile and bisulfite after step 1 processing Mol ratio between sodium is 3~9：1：0.04~0.2：0.04~0.2.
- 4. the preparation method of a kind of super hydrophobic coating according to claim 2, it is characterised in that in the step 4：Oil bath Temperature in constant temperature pot is 65 DEG C~75 DEG C, and the magnetic agitation time is 35min~45min.
- 5. application process of a kind of super hydrophobic coating on fabric, it is characterised in that specifically implement according to following steps：Step 1, methyl propenoic acid glycidyl is taken, methyl propenoic acid glycidyl is filtered using alumina chromatographic column, removed Polymerization inhibitor；Step 2, weigh respectively dodecafluoroheptyl methacrylate, through step 1 processing after methyl propenoic acid glycidyl and Azodiisobutyronitrile and sodium hydrogensulfite；Step 3, all materials weighed in step 2 are added in container together, then tetrahydrofuran is added into container, by this Container seals and is passed through nitrogen, discharges the oxygen in container；Step 4, after the completion for the treatment of step 3, whole container is positioned in oil bath constant temperature pot and heated, and opened under the protection of nitrogen Magnetic agitation, make dodecafluoroheptyl methacrylate, methyl propenoic acid glycidyl, azodiisobutyronitrile and sulfurous in container Sour hydrogen sodium fully reacts, and question response pours out the reactant formed in container after terminating, and is stood under normal temperature, treats that tetrahydrofuran is waved Untill distributing, super hydrophobic coating PGMA-r-PDFMA is obtained, its reaction equation is as follows：Step 5, fabric first cleaned with detergent, 4h~6h is soaked in absolute ethyl alcohol, is then rinsed well with clear water, most After dry, obtain cleaning fabric；Step 6, the super hydrophobic coating PGMA-r-PDFMA obtained through step 4 first dissolved with tetrahydrofuran, add 0.5mL~ 1mL triethylamines, it is 9mg/mL transparency liquids, as modification liquid to be configured to concentration；Then the clean fabric that will be obtained through step 5 It is soaked in the modification liquid made；Finally dry, one layer of super hydrophobic coating PGMA-r-PDFMA layer is loaded with fabric face.
- A kind of 6. application process of the super hydrophobic coating according to claim 5 on fabric, it is characterised in that the step In 2：Dodecafluoroheptyl methacrylate, through step 1 processing after methyl propenoic acid glycidyl and azodiisobutyronitrile and Mol ratio between sodium hydrogensulfite is 3~9：1：0.04~0.2：0.04~0.2.
- A kind of 7. application process of the super hydrophobic coating according to claim 5 on fabric, it is characterised in that the step In 4：Temperature in oil bath constant temperature pot is 65 DEG C~75 DEG C, and the magnetic agitation time is 35min~45min.
- A kind of 8. application process of the super hydrophobic coating according to claim 5 on fabric, it is characterised in that the step In 5：Wash number is 3 times~5 times, and drying temperature is 70 DEG C~90 DEG C.
- A kind of 9. application process of the super hydrophobic coating according to claim 5 on fabric, it is characterised in that the step In 6：Soak time is 1h~24h, and drying temperature is 110 DEG C~130 DEG C.
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