CN109629231A - A kind of methyl class monomer plasma processing method of superhydrophobic surface material - Google Patents
A kind of methyl class monomer plasma processing method of superhydrophobic surface material Download PDFInfo
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- CN109629231A CN109629231A CN201811493229.8A CN201811493229A CN109629231A CN 109629231 A CN109629231 A CN 109629231A CN 201811493229 A CN201811493229 A CN 201811493229A CN 109629231 A CN109629231 A CN 109629231A
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- class monomer
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- superhydrophobic surface
- surface material
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/20—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin
- D06M14/22—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/32—Polyesters
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- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a kind of methyl class monomer plasma processing methods of superhydrophobic surface material, which is characterized in that place the material in being cleaned by ultrasonic in detergent, then with deionized water by its repeated washing it is multiple after, take out, be dried for standby；After methyl class monomer is mixed with solvent, obtained material is impregnated, is then dried for standby；Place the material in the reaction chamber of plasma apparatus, under conditions of reaction gas, radio frequency discharge is opened, material is handled.It is monomer that the present invention, which selects the relatively small methyl type organic of molecular weight, material surface is handled using capacitor and inductively-coupled discharge low pressure radio frequency plasma, monomer is graft-polymerized on the surface of the material under environment under low pressure, its surface chemical composition and surface roughness etc. are influenced, obtaining the present invention has lasting wear-resisting super-hydrophobic surface.Superhydrophobic surface material prepared by the present invention is nontoxic, has good durability, and operating procedure is simple, easy industrialization and environmental protection.
Description
Technical field
The present invention relates to a kind of methyl class monomer plasma processing methods of superhydrophobic surface material, belong to textile technology
Field.
Background technique
Textile fabric due to itself contain hole and it is rough cause using and wearing process in can fiber with
And accumulate dust between yarn and not only will affect the beautiful aging speed for increasing material in this way, while cause microorganism (fungi, it is mould
Bacterium, bacterium) attachment and growth, limit its answering at many fields (such as protective garment, stain-resistant textile and medical staff's clothes)
With.Therefore, how the hydrophobicity on textile material surface is to widen the emphasis research topic of textile material application field.Currently, fluorine
Polymer is most commonly used to prepare super-hydrophobic coat, but product made of fluoropolymer exists in use and after discarded
The problem of polluting environment, therefore must reduce and even forbid fluoropolymer-containing use.It is general to select the esters polymer containing alkyl
Fluoropolymer is substituted with silane quasi polymer, although-the CH contained by both polymer3、-CH2And-O-Si- group
Surface can be low not as good as fluoro-containing group, but its no pollution to the environment, it is considered to be most potential substitution fluoropolymer is used in combination
In the polymer of hydrophobic material preparation.
Common hydrophobic surface preparation method mainly has Static Spinning, sol-gel method and plasma method, these methods
The production of super-hydrophobic textile is promoted to obtain breakthrough.In particular, the material of corona treatment has the advantages that two: whole
A treatment process does not generate liquid debris；Modified effect is limited only to property of the surface of material without changing material script.
Summary of the invention
The technical problems to be solved by the present invention are: existing superhydrophobic surface material preparation process can cause environmental pollution
The problem of.
To solve the above-mentioned problems, The technical solution adopted by the invention is as follows:
A kind of methyl class monomer plasma processing method of superhydrophobic surface material, which is characterized in that including following step
It is rapid:
Step 1): place the material in being cleaned by ultrasonic in detergent, then with deionized water by its repeated washing it is multiple after, take
Out, it is dried for standby；
Step 2): after methyl class monomer is mixed with solvent, the material that step 1) obtains is impregnated, is then dried standby
With；
Step 3): the material that step 2) is obtained is placed in the reaction chamber of plasma apparatus, in the condition of reaction gas
Under, radio frequency discharge is opened, material is handled.
Preferably, the material in the step 1) is cotton, the fabric of chemical fibre material, yarn or fiber；Detergent is anhydrous
The mixed solution of ethyl alcohol or detergent 209 and natrium carbonicum calcinatum.
Preferably, the solvent in the step 2) is dehydrated alcohol；Mass concentration of the methyl class monomer in mixed liquor be
2%~100%.
Preferably, the discharge mode of the radio frequency discharge in the step 3) is the electric discharge of low pressure radio frequency inductive or capacitive coupling
Electric discharge；Charging method is continuous discharge.
It is highly preferred that the inductive discharge is single-turn circular coil electric discharge；The capacitively coupled discharge is discharged using parallel-plate.
Preferably, the supply frequency of radio frequency discharge is 2~60MHz in the step 3), and the adjustable extent of discharge power is 0
~500W, the adjustable extent for modulating pulse is 2%~100%.
Preferably, the reaction gas in the step 3) is argon gas, helium, oxygen or air.
Preferably, the step 3) specifically: the material for obtaining step 2) is placed in the reaction chamber of plasma apparatus,
It is vacuumized after closing reaction chamber, is less than 10Pa to intracavitary pressure, reaction gas is filled with into reaction chamber and makes pressure in reaction chamber
After stabilization, opens radio frequency discharge and material is handled；After processing reaction, it is filled with reaction gas, it is extensive to the pressure in reaction chamber
Again to atmospheric pressure, reaction chamber is opened, material is taken out, obtains superhydrophobic surface material.
Stablize it is highly preferred that being filled with pressure after reaction gas in the reaction chamber in 3~40Pa.
It is monomer that the present invention, which selects the relatively small methyl type organic of molecular weight, low using capacitor and inductively-coupled discharge
Pressure radio frequency plasma handles material surface, and monomer is graft-polymerized on the surface of the material under environment under low pressure, influences its table
Face chemical component and surface roughness etc., obtaining the present invention has lasting wear-resisting super-hydrophobic surface.It is prepared by the present invention super thin
Water surface material non-toxic has good durability, and operating procedure is simple, easy industrialization and environmental protection.
Compared with prior art, the invention has the following beneficial effects:
(1) processing method of the present invention is carried out under environment under low pressure, takes plasma surface modified and grafting
Polymerization technique, affected by environment small, technology path, operating procedure are simple, favorable repeatability, guarantee treatment process stability and
Consistency is advantageously implemented industrialization.
(2) processing method of the present invention is simple, safe, and monomer used is not fluorine-containing, does not need that other auxiliary agents are added,
Clean and environmental protection, process are simple, cost is relatively low, can bring significant economical and environmentally friendly benefit.
(3) present invention assigns material excellent durable super-hydrophobic property performance, and Static water contact angles test is greater than 150 °, roll angle
Less than 15 °；Hydrophobic excellent durability, after standard is soaped 1500 times, the Static water contact angles of material surface are still greater than 135 °, roll
Angle is still less than 35 °；Or the Static water contact angles of material surface are still greater than 130 ° after friction 2000 times, and after rubbing 500 times, material table
The roll angle in face is still 50 ° small.
Detailed description of the invention
Fig. 1 is the electron microscope of the cotton fabric processing front surface Static water contact angles in embodiment；
Fig. 2 is the electron microscope of super hydrophobic surface surface of cotton fabric Static water contact angles made from embodiment；
Fig. 3 is the water contact angle of plasma treated surface of cotton fabric and the variation relation of washing times in embodiment
Figure；
Fig. 4 is the water contact angle of plasma treated surface of cotton fabric and the variation relation of Rubbing number in embodiment
Figure.
Specific embodiment
In order to make the present invention more obvious and understandable, hereby with preferred embodiment, and attached drawing is cooperated to be described in detail below.
Embodiment 1
A kind of methyl class monomer plasma processing method of superhydrophobic surface material:
(1) cotton fabric is immersed in dehydrated alcohol (analysis pure, >=99.7%), and 30 DEG C, be cleaned by ultrasonic under the conditions of 40kHz
30min, is cleaned by ultrasonic 30min by deionized water 30 DEG C later under the conditions of 40kHZ, repeated washing is three times in deionized water
After take out, drying for standby；
(2) fabric after pre-treatment is cut into 40mm × 50mm, is placed into lauryl methacrylate (LMA) wine of 5g/L
In smart solution, bath raio 30:1 impregnates 10min in supersonic cleaning machine, dries at 60 DEG C after taking-up；
(3) cotton fabric that drying obtains is placed on to the bottom crown of reaction cavity, bottom crown spacing is 10.16cm in adjusting,
Reaction chamber is closed, 20mTorr is evacuated to, is passed through 99% ordinary purity argon gas, adjusting cavity internal pressure strong stability is in 220mTorr；
(4) radio-frequency power supply switch is opened, discharge parameter is adjusted, supply frequency is fixed as 13.56MHz, and discharge power is
50W；
(5) after handling 60s, power supply and vacuum pump is successively closed, cavity is opened after logical argon gas to standard atmospheric pressure, takes out cotton
Fabric.
The control of present invention fabric hydrophobic effect before and after the processing, as a result as follows:
By treated cotton fabric and processing before dacron compare, using contact angle measurement (WCA,
Science and Technology Ltd., Ningbo are detected when DropMeterTM Professional A-200, Hai Shumai) to material before and after the processing
Static contact angle test is carried out, drop amount is 5 μ L, photo opporunity 60s, carries out 5 tests to every group of material respectively, is averaged
Value；Rotor speed is set as (40 ± 2) r/min according to GB/T 3921-2008, and temperature is 40 DEG C, wash time 30min, soap
Piece liquor capacity concentration is 5g/L, bath raio 50:1, carries out wash durability test to fabric；Establishing criteria GB/T 3920-
2008 settings pressure 9N (44.8kPa), 60 times/min of friction velocity carry out wear-resisting property test to fabric.
By Fig. 3,4 it is found that handle before cotton fabric water contact angle be 86.3 °, treated Static water contact angles and rolling
Angle is respectively 153.4 ° and 13.38 °；Hydrophobic excellent durability, after standard is soaped 1500 times, the Static water contact angles of material surface
135 ° are still greater than, roll angle is still less than 35 °；Or the Static water contact angles of material surface are still greater than 130 ° after friction 2000 times, rub
After wiping 500 times, the roll angle of material surface is still 50 ° small, and material still shows preferable hydrophobic effect.
Embodiment 2
A kind of methyl class monomer plasma processing method of superhydrophobic surface material:
(1) using deionized water as solvent, configuration concentration is 209 solution of detergent of 2g/L, and appropriate natrium carbonicum calcinatum is added,
Solution PH=8 are adjusted, dacron is immersed in detergent solution with the bath raio of 50:1, is cleaned by ultrasonic 40min, then spends
Ion water washing 3-5 times, is put into baking oven and dries, and takes out spare；
(2) fabric after pre-treatment is cut into 40mm × 50mm, is placed into the lauryl methacrylate (LMA) of 35g/L
In alcoholic solution, bath raio 30:1 impregnates 10min in supersonic cleaning machine, dries at 60 DEG C after taking-up；
(3) cotton fabric that drying obtains is placed on to the bottom crown of reaction cavity, bottom crown spacing is 10.16cm in adjusting,
Reaction chamber is closed, 20mTorr is evacuated to, is passed through 99% ordinary purity argon gas, adjusting cavity internal pressure strong stability is in 220mTorr；
(4) radio-frequency power supply switch is opened, discharge parameter is adjusted, supply frequency is fixed as 13.56MHz, and discharge power is
90W；
(5) after handling 60s, power supply and vacuum pump is successively closed, opens cavity after logical argon gas to standard atmospheric pressure, taking-up is washed
Synthetic fibre fabric.
The control of present invention fabric hydrophobic effect before and after the processing, as a result as follows:
Treated dacron and the dacron before processing are compared, contact angle measurement is used
(detecting Science and Technology Ltd., Ningbo when WCA, DropMeterTM Professional A-200, Hai Shumai) is to before and after the processing
Material carry out static contact angle test, drop amount is 5 μ L, photo opporunity 60s, 5 tests are carried out to every group of material respectively,
It is averaged；Rotor speed is set as (40 ± 2) r/min according to GB/T 3921-2008, and temperature is 40 DEG C, and wash time is
30min, soap flakes liquor capacity concentration are 5g/L, bath raio 50:1, carry out wash durability test to fabric；Establishing criteria GB/T
3920-2008 sets pressure 9N (44.8kPa), 60 times/min of friction velocity, carries out wear-resisting property test to fabric.
The water contact angle of dacron is 127.6 ° before handling, and treated Static water contact angles and roll angle are respectively
151.4 ° and 15.7 °；Hydrophobic excellent durability, after standard is soaped 1500 times, the Static water contact angles of material surface are still greater than
131.3 °, roll angle is still less than 35 °；Or the Static water contact angles of material surface are still greater than 130.6 ° after friction 2000 times, friction
After 500 times, the roll angle of material surface is still 50 ° small, and material still shows preferable hydrophobic effect.
Embodiment 3
A kind of methyl class monomer plasma processing method of superhydrophobic surface material:
(1) using deionized water as solvent, configuration concentration is 209 solution of detergent of 2g/L, and appropriate natrium carbonicum calcinatum is added,
Solution PH=8 are adjusted, terylene non-woven fabric is immersed in detergent solution with the bath raio of 50:1, is cleaned by ultrasonic 40min, then uses
Deionized water is washed 3-5 times, is put into baking oven and is dried, and is taken out spare；
(2) fabric after pre-treatment is cut into 40mm × 50mm, is placed into the lauryl methacrylate (LMA) of 50g/L
In alcoholic solution, bath raio 30:1 impregnates 10min in supersonic cleaning machine, dries at 60 DEG C after taking-up；
(3) cotton fabric that drying obtains is placed on to the bottom crown of reaction cavity, bottom crown spacing is 10.16cm in adjusting,
Reaction chamber is closed, 20mTorr is evacuated to, is passed through 99% ordinary purity argon gas, adjusting cavity internal pressure strong stability is in 220mTorr；
(4) radio-frequency power supply switch is opened, discharge parameter is adjusted, supply frequency is fixed as 13.56MHz, and discharge power is
100W；
(5) after handling 120s, power supply and vacuum pump is successively closed, cavity is opened after logical argon gas to standard atmospheric pressure, takes out
Cotton fabric.
The control of present invention fabric hydrophobic effect before and after the processing, as a result as follows:
Treated terylene non-woven fabric and the terylene non-woven fabric before processing are compared, contact angle measurement is used
(detecting Science and Technology Ltd., Ningbo when WCA, DropMeterTM Professional A-200, Hai Shumai) is to before and after the processing
Material carry out static contact angle test, drop amount is 5 μ L, photo opporunity 60s, 5 tests are carried out to every group of material respectively,
It is averaged；Rotor speed is set as (40 ± 2) r/min according to GB/T 3921-2008, and temperature is 40 DEG C, and wash time is
30min, soap flakes liquor capacity concentration are 5g/L, bath raio 50:1, carry out wash durability test to fabric；Establishing criteria GB/T
3920-2008 sets pressure 9N (44.8kPa), 60 times/min of friction velocity, carries out wear-resisting property test to fabric.
The water contact angle of terylene non-woven fabric is 113.1 ° before handling, and treated Static water contact angles and roll angle are respectively
152.6 ° and 7.2 °；Hydrophobic excellent durability, after standard is soaped 1500 times, the Static water contact angles of material surface are still greater than
137 °, roll angle is still less than 30 °；Or the Static water contact angles of material surface are still greater than 133 ° after friction 2000 times, rub 500 times
Afterwards, the roll angle of material surface is still 40 ° small, and material still shows preferable hydrophobic effect.
Claims (9)
1. a kind of methyl class monomer plasma processing method of superhydrophobic surface material, which comprises the following steps:
Step 1): place the material in being cleaned by ultrasonic in detergent, then with deionized water by its repeated washing it is multiple after, take out, dry
It does spare；
Step 2): after methyl class monomer is mixed with solvent, the material that step 1) obtains is impregnated, is then dried for standby；
Step 3): the material that step 2) is obtained is placed in the reaction chamber of plasma apparatus, under conditions of reaction gas, is opened
Radio frequency discharge is opened, material is handled.
2. the methyl class monomer plasma processing method of superhydrophobic surface material as described in claim 1, which is characterized in that
Material in the step 1) is cotton, the fabric of chemical fibre material, yarn or fiber；Detergent is dehydrated alcohol or detergent 209
With the mixed solution of natrium carbonicum calcinatum.
3. the methyl class monomer plasma processing method of superhydrophobic surface material as described in claim 1, which is characterized in that
Solvent in the step 2) is dehydrated alcohol；Quality of the methyl class monomer in mixed liquor? concentration is 2%~100%.
4. the methyl class monomer plasma processing method of superhydrophobic surface material as described in claim 1, which is characterized in that
The discharge mode of radio frequency discharge in the step 3) is the electric discharge of low pressure radio frequency inductive or capacitively coupled discharge；Charging method is
Continuous discharge.
5. the methyl class monomer plasma processing method of superhydrophobic surface material as claimed in claim 4, which is characterized in that
The inductive discharge is single-turn circular coil electric discharge；The capacitively coupled discharge is discharged using parallel-plate.
6. the methyl class monomer plasma processing method of superhydrophobic surface material as described in claim 1, which is characterized in that
The supply frequency of radio frequency discharge is 2~60MHz in the step 3), and the adjustable extent of discharge power is 0~500W, modulates pulse
Adjustable extent be 2%~100%.
7. the methyl class monomer plasma processing method of superhydrophobic surface material as described in claim 1, which is characterized in that
Reaction gas in the step 3) is argon gas, helium, oxygen or air.
8. the methyl class monomer plasma of the superhydrophobic surface material as described in any one of claim 1 and 4-7 is handled
Method, which is characterized in that the step 3) specifically: the material for obtaining step 2) is placed in the reaction chamber of plasma apparatus
In, it is vacuumized after closing reaction chamber, is less than 10Pa to intracavitary pressure, reaction gas is filled with into reaction chamber and makes reaction chamber internal pressure
After strong stability, opens radio frequency discharge and material is handled；After processing reaction, it is filled with reaction gas, to the pressure in reaction chamber
Restore to atmospheric pressure, open reaction chamber, takes out material, obtain superhydrophobic surface material.
9. the methyl class monomer plasma processing method of superhydrophobic surface material as claimed in claim 8, which is characterized in that
Pressure is stablized in 3~40Pa after being filled with reaction gas in the reaction chamber.
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| CN110067129A (en) * | 2019-04-28 | 2019-07-30 | 东华大学 | The method that corona treatment nano-particles reinforcement coating prepares superhydrophobic fabric |
| CN110656484A (en) * | 2019-09-24 | 2020-01-07 | 东华大学 | Plasma treatment method of siloxane durable super-hydrophobic gradient film |
| CN111501325B (en) * | 2020-04-09 | 2021-09-17 | 东华大学 | Surface-wrinkled fiber material and preparation method thereof |
| WO2023279474A1 (en) * | 2021-07-08 | 2023-01-12 | 苏州大学 | Preparation method for ultra-infiltration coating |
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| CB03 | Change of inventor or designer information |
Inventor after: Guo Ying Inventor after: Xu Liyun Inventor after: Shi Jianjun Inventor after: Yu Jianyong Inventor before: Guo Ying Inventor before: Xu Liyun Inventor before: Shi Jianjun Inventor before: Yu Jianyong |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190416 |