CN102409527A - Plasma finishing method for endowing fabric durable super-hydrophobic property - Google Patents

Plasma finishing method for endowing fabric durable super-hydrophobic property Download PDF

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Publication number
CN102409527A
CN102409527A CN2011103198167A CN201110319816A CN102409527A CN 102409527 A CN102409527 A CN 102409527A CN 2011103198167 A CN2011103198167 A CN 2011103198167A CN 201110319816 A CN201110319816 A CN 201110319816A CN 102409527 A CN102409527 A CN 102409527A
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China
Prior art keywords
fabric
plasma
terylene
monomer
dacron
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Pending
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CN2011103198167A
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Chinese (zh)
Inventor
刘今强
刘婷婷
李永强
李立名
缪华丽
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Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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Zhejiang Sci Tech University ZSTU
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Priority to CN2011103198167A priority Critical patent/CN102409527A/en
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Abstract

The invention discloses a plasma finishing method for endowing a fabric durable super-hydrophobic property. The method comprises the following steps of: (1) washing a fabric with water and drying, wherein the drying temperature is 80-100 degrees centigrade; (2) preparing monomer solution of which the concentration is greater than 99%; soaking the dried fabric in the prepared monomer solution for 2-5 min at normal temperature; mangling liquid by using a small mangle car; making the liquid content of terylene be 60-90%; (3) putting the soaked terylene attached with monomer in an outer electrode normal pressure plasma reaction chamber; leading Ar with the flow of 1.2-2.0 L/min, wherein the voltage is controlled at 95-115 V and the processing time is 60-240 s. The plasma finishing method has the advantages of good durable super-hydrophobic effect, simple operation process, easy industrialization and environmental protection.

Description

A kind ofly give fabric durable super-hydrophobic plasma method for sorting
Technical field
The invention belongs to textile field, be specifically related to a kind of plasma method for sorting of fabric.
Background technology
Terylene is to weave in the world with output maximum in the chemical fibre, most widely used kind, and terylene accounts for more than 60% of world's synthetic fiber output at present.Its textile product obtains the extensive concern and the research of textile industry circle to functionalization, intelligent direction development.
The purpose of water repellent finish is to make fabric difficult wetting by water institute, and produces certain anti-soil effect and don't influence its wearing comfortableness, increases value-added content of product, reduces washing times, and prolongs its service life.According to wetting theory analysis, the surface energy of water than higher be 72.6mJ/m 2, the surface energy of water-proof material must be worth less than this.At present; The general employing of the water repellent finish of fabric is padded technology a kind of finishing agent with special molecular structure is distributed in the space between fabric face or yarn; Finishing agent is membranaceous at fabric face in the process of baking; And can be firm attached on the fiber or with fiber generation chemical bond, thereby reduce fabric face tension force.
Chemical constitution according to water repellent itself; Studied or used water repellent kind a lot, mainly contain metallic soap class (aluminium soap and zirconium soap), wax and waxy substance, metal complex, pyridine derivatives, methylol compound, silicone based (polysiloxanes) and fluorochemical etc.But because poor durability, perhaps fiber itself there is damage, influence the feel and the style of fabric, and a variety of causes such as smell, color, the water repellent of using always at present mainly is organosilicon and fluorochemical.But, utilize water repellent that fabric is carried out chemical finishing and have a big problem usually, in the arrangement process, can pollute environment.
It is thus clear that above water repellent is at tradition dipping and pad in the application of technology and all have certain limitation, it is simple therefore to develop a cover technology, and it is good to refuse the water effect, pollutes few technology and seems particularly important.
Summary of the invention
Refuse the environmental problem brought in durability and the arrangement process of water effect to fabric; The present invention adopts a kind of standard atmosphere plasma modified technology of novel environment friendly; Under atmospheric pressure composite unit is put in order terylene, makes monomer in fabric face polymerization deposition, and durability is super-hydrophobic effective; Whole process need not to vacuumize, simple, the easy industrialization of operating procedure.
The technical scheme that the present invention adopts is following: a kind ofly give fabric durable super-hydrophobic plasma method for sorting, concrete steps are following:
(1) extracting waste weaving polyester fabric carries out refining treatment, and clear water is cleaned, dried then, and bake out temperature is 80-100 ℃; Or get the direct clear water of coloured weaving polyester fabric and clean, dry, bake out temperature is 80-100 ℃;
(2) be ready to concentration greater than 99% monomer solution, under normal temperature condition, the dacron of oven dry be immersed in 2-5min in the ready monomer solution, after the laboratory mangle mangle, making the terylene liquid carrying rate is 60-90%;
(3) terylene with monomer after will flooding places external electrode formula atmospheric plasma reative cell, feeds the Ar of 1.2-2.0L/min flow; The power-on switch is regulated atmospheric plasma equipment, controls its voltage between 95-115V; This moment, plasma discharge evenly stablize, and processing time 60s-240s is deposited on the dacron monomer polymerization, reached power cutoff after the stipulated time, the taking-up sample.
Of the present inventionly give fabric durable super-hydrophobic plasma method for sorting, the monomer in the monomer solution in the step (2) is the ring-type methylsiloxane, and the general formula of ring-type methylsiloxane is Si nO n(CH 3) nR n, n=3-9 wherein, R is CH 3Or CH=CH 2
Of the present inventionly give fabric durable super-hydrophobic plasma method for sorting, the discharge mode of the atmospheric plasma equipment in the step (3) is the glow discharge of normal pressure class.
The present invention has following beneficial effect:
(1) treatment process of the present invention belongs to the serialization finishing technique of complete dry state, but the conserve water resource, and do not have water pollution, can bring remarkable economical and environmental benefit.
(2) treatment conditions of the present invention need not vacuum, and energy savings, operating procedure are simple, and then help combining the industrialization practical application more.
(3) simple, the safety of method for sorting of the present invention need not add other auxiliary agents, need not to carry out other physics or chemical reaction, and the surplus solution behind the dipping is reusable, and not only clean environment firendly has reduced operation more greatly, has reduced cost.
(4) the present invention takes brand-new atmospheric plasma surface modification and plasma polymerization deposition one-step method; The technology path of common plasma subtraction+chemical addition is thoroughly simplified; Guarantee the stability and the uniformity of finishing technique, make it more effectively, more to meet the practical application needs.
(5) the present invention can give fabric good durability ultra-hydrophobicity, and water contact angle is tested greater than 150 oIt is good to refuse the water durability, and standard is soaped after 30 times the fabric contact angle still greater than 135 o, hydrophobic grade still reaches the 70-80 branch according to AATCC trickle grading standard.
(6) the present invention only acts on the surface to the modification of material, does not destroy the good characteristic of its body, has improved the flexibility of dacron simultaneously, and colored terylene fabric apparent colour is not had influence.
Description of drawings
Fig. 1 a is the surface sweeping electromicroscopic photograph of dacron (2000 *) of being untreated:
Fig. 1 b is the surface sweeping electromicroscopic photograph of dacron after the plasma treatment (2000 *).
The specific embodiment
Embodiment below in conjunction with concrete specifies the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
(1) preparation of dacron:
White weaving polyester fabric is carried out refining processing, and treatment conditions are: the heavy 200g of fabric; Detergent 2g/L; Alkali 2g/L, bath raio 1:30; 90 ℃ of temperature, time 50min.Get the 20cm*10cm dacron, fabric is carried out clear water clean, dry, bake out temperature is 100 ℃.
(2) under normal temperature condition, be ready to concentration for 99% octamethylcy-clotetrasiloxane solution in glass, above-mentioned dacron is immersed in 5min in the solution, after the laboratory mangle mangle, control terylene liquid carrying rate is 90%.
(3) terylene is put into the atmospheric plasma process chamber, feed 99% ordinary purity argon gas of 1.8L/min flow.
(4) power-on switch is regulated atmospheric plasma equipment, and controlling its voltage is 115V, and be 240s discharge time, reaches power cutoff after the stipulated time.
(5) close the valve that leads to argon gas, ventilated one minute, take out fabric.
Embodiment 2:
(1) preparation of dacron:
White weaving polyester fabric is carried out refining processing, and treatment conditions are: the heavy 200g of fabric; Detergent 2g/L; Alkali 2g/L, bath raio 1:30; 90 ℃ of temperature, time 50min.Get the 20cm*10cm dacron, fabric is carried out clear water clean, dry, bake out temperature is 90 ℃.
(2) under normal temperature condition, be ready to concentration for 99% octamethylcy-clotetrasiloxane solution in glass, above-mentioned dacron is immersed in 4min in the solution, after the laboratory mangle mangle, control terylene liquid carrying rate is 80%.
(3) terylene is put into the atmospheric plasma process chamber, feed 99% ordinary purity argon gas of 1.5L/min flow.
(4) power-on switch is regulated atmospheric plasma equipment, and controlling its voltage is 110V, and be 120s discharge time, reaches power cutoff after the stipulated time.
(5) close the valve that leads to argon gas, ventilated one minute, take out fabric.
Embodiment 3:
(1) preparation of dacron:
White weaving polyester fabric is carried out refining processing, and treatment conditions are: the heavy 200g of fabric; Detergent 2g/L; Alkali 2g/L, bath raio 1:30; 90 ℃ of temperature, time 50min.Get the 20cm*10cm dacron, fabric is carried out clear water clean, dry, bake out temperature is 80 ℃.
(2) under normal temperature condition, be ready to concentration for 99% decamethylcyclopentaandoxane solution in glass, above-mentioned dacron is immersed in 2min in the solution, after the laboratory mangle mangle, control terylene liquid carrying rate is 60%.
(3) terylene is put into the atmospheric plasma process chamber, feed 99% ordinary purity argon gas of 1.2L/min flow.
(4) power-on switch is regulated atmospheric plasma equipment, and controlling its voltage is 95V, and be 60s discharge time, reaches power cutoff after the stipulated time.
(5) close the valve that leads to argon gas, ventilated one minute, take out fabric.
Embodiment 4:
(1) preparation of dacron:
Get the blue dacron of 20cm*10cm, fabric is carried out clear water clean, dry, bake out temperature is 90 ℃.
(2) under normal temperature condition, be ready to concentration for 99% hexamethyl cyclotrisiloxane solution in glass, above-mentioned dacron is immersed in 5min in the solution, after the laboratory mangle mangle, control terylene liquid carrying rate is 80%.
(3) terylene is put into the atmospheric plasma process chamber, feed 99% ordinary purity argon gas of 1.5L/min flow.
(4) power-on switch is regulated atmospheric plasma equipment, and controlling its voltage is 110V, and be 120s discharge time, reaches power cutoff after the stipulated time.
(5) close the valve that leads to argon gas, ventilated one minute, take out fabric.
Embodiment 5:
(1) preparation of dacron:
Get the blue dacron of 20cm*10cm, fabric is carried out clear water clean, dry, bake out temperature is 80 ℃.
(2) under normal temperature condition, be ready to concentration for 99% decamethylcyclopentaandoxane solution in glass, above-mentioned dacron is immersed in 3min in the solution, after the laboratory mangle mangle, control terylene liquid carrying rate is 70%.
(3) terylene is put into the atmospheric plasma process chamber, feed 99% ordinary purity argon gas of 1.2L/min flow.
(4) power-on switch is regulated atmospheric plasma equipment, and controlling its voltage is 100V, and be 60s discharge time, reaches power cutoff after the stipulated time.
(5) close the valve that leads to argon gas, ventilated one minute, take out fabric.
The present invention puts the performance test and the former state contrast of back fabric in order, and the result is following:
(1) refuses the evaluation of water effect after dacron is handled
With dacron and the comparison sample dacron after the above-mentioned instance 1-5 processing; Balance is 24 hours under similarity condition; Use droplet morphology analyzer (German KRUSS company, DSA 10MK2 type) test water contact angle, when water droplet and reading after fabric contacts 60s; Diverse location at same sample is measured 5 times, averages; With reference to AATCC-22-1996 trickle property experimental standard test fabric WATER REPELLENCY, the result is like following table 1, shown in 2.By interpretation of result, after employing the inventive method is implemented, given dacron good ultra-hydrophobicity.
 
The test of table 1 water contact angle
Sample To the contact angle of water ( o
Appearance is untreated /
Embodiment 1 157
Embodiment 2 155
Embodiment 3 149
Embodiment 4 151
Embodiment 5 148
Table 2 is refused the evaluation of water grade
Sample Refuse the water grade Refuse the water grade after washing 10 times Refuse the water grade after washing 20 times Refuse the water grade after washing 30 times
Appearance is untreated 0-1 / / /
Embodiment 1 5 5 5 4-5
Embodiment 2 5 5 4-5 4
Embodiment 3 5 5 4-5 4
Embodiment 4 5 5 4-5 3-4
Embodiment 5 5 5 4-5 3-4
(2) dacron is handled the scanning electron microscopic observation of back surface topography
Use the surface topography of JSM-5610LV type scanning electron microscopic observation arrangement front and back dacron.Like Fig. 1 a, Fig. 1 b and shown in Figure 2, after the inventive method was handled, PET fiber surface coated the even and smooth film of one deck, and experiment proves the polysiloxanes polymeric membrane, and the existence of this layer film makes fabric have good hydrophobic effect.
The surface topography of undressed terylene former state, shown in Fig. 1 a, PET fiber surface is smooth, is orientated regular.Can find that through Fig. 1 b the terylene after handling through the present invention has formed the continuous and uniform film of one deck between fiber and fiber.Experiment shows; The dacron that is attached with monomer is when plasma treatment, and the polymerizable monomer plasma produces all kinds of spikes, and this moment, the monomer of fiber surface can produce free radical with the high energy particle collision in the space; At this moment, active group is exactly to generate at specimen surface.Free radical that these free radical monomers generate with the space again or the combined with radical of closing on are on every side grown up gradually, form to have highly cross-linked network structure film, shown in Fig. 1 b.In addition, the chain rupture polarization can take place in the big molecule of ring-type methylsiloxane and terylene under action of plasma, has increased the adhesion of methylsiloxane and fiber, makes nonpolar methyl do vertical intensive aligning at fiber surface.Final effect has less critical surface tension and bigger contact angle when having impelled fabric face to meet water, thereby gives the ultra-hydrophobicity of the good and good endurance of fabric.

Claims (3)

1. give fabric durable super-hydrophobic plasma method for sorting for one kind, it is characterized in that the step of this method is following:
(1) extracting waste weaving polyester fabric carries out refining treatment, and clear water is cleaned, dried then, and bake out temperature is 80-100 ℃; Or get the direct clear water of coloured weaving polyester fabric and clean, dry, bake out temperature is 80-100 ℃;
(2) be ready to concentration greater than 99% monomer solution, under normal temperature condition, the dacron of oven dry be immersed in 2-5min in the ready monomer solution, after the laboratory mangle mangle, making the terylene liquid carrying rate is 60-90%;
(3) terylene with monomer after will flooding places external electrode formula atmospheric plasma reative cell, feeds the argon gas of 99% ordinary purity of 1.2-2.0L/min flow; The power-on switch is regulated atmospheric plasma equipment, controls its voltage between 95-115V; This moment, plasma discharge evenly stablize, and processing time 60s-240s is deposited on the dacron monomer polymerization, reached power cutoff after the stipulated time, the taking-up sample.
2. as claimed in claim 1ly give fabric durable super-hydrophobic plasma method for sorting, it is characterized in that: the monomer in the monomer solution in the step (2) is the ring-type methylsiloxane, and the general formula of ring-type methylsiloxane is Si nO n(CH 3) nR n, n=3-9 wherein, R is CH 3Or CH=CH 2
According to claim 1 or claim 2 give fabric durable super-hydrophobic plasma method for sorting, it is characterized in that: the discharge mode of the atmospheric plasma equipment in the step (3) is the glow discharge of normal pressure class.
CN2011103198167A 2011-10-20 2011-10-20 Plasma finishing method for endowing fabric durable super-hydrophobic property Pending CN102409527A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103266393A (en) * 2013-05-14 2013-08-28 东华大学 Preparation method for water-repellent oil-repellent flame-retardant protective suit fabric
CN104372608A (en) * 2014-11-12 2015-02-25 江南大学 Method for preparing super-hydrophobic fabric by adopting sol-gel electrochemical deposition
CN104911907A (en) * 2015-06-08 2015-09-16 浙江理工大学 Low-pressure plasma sorting method endowing cotton fabric with fluoride-free water repellent function
CN105862386A (en) * 2016-04-25 2016-08-17 东莞市联洲知识产权运营管理有限公司 Method for preparing fluorescent-yellow dacron-cotton shell fabric
CN109322143A (en) * 2018-12-07 2019-02-12 东华大学 A kind of type siloxane monomer plasma processing method of superhydrophobic surface material
CN109629231A (en) * 2018-12-07 2019-04-16 东华大学 A kind of methyl class monomer plasma processing method of superhydrophobic surface material
CN110067129A (en) * 2019-04-28 2019-07-30 东华大学 The method that corona treatment nano-particles reinforcement coating prepares superhydrophobic fabric
CN110644240A (en) * 2019-07-26 2020-01-03 南通大学 Preparation method of multifunctional durable and self-repairing super-hydrophobic fabric surface
CN110656484A (en) * 2019-09-24 2020-01-07 东华大学 Plasma treatment method of siloxane durable super-hydrophobic gradient film
CN111094480A (en) * 2017-09-22 2020-05-01 3M创新有限公司 Polycarbodiimide-containing compositions, methods, and articles
CN112301725A (en) * 2019-08-02 2021-02-02 香港纺织及成衣研发中心 Waterproof fabric obtained by plasma technology and preparation method thereof
CN113550144A (en) * 2021-08-18 2021-10-26 江南大学 Preparation method of antibacterial hydrophobic denim fabric

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103266393B (en) * 2013-05-14 2015-05-13 东华大学 Preparation method for water-repellent oil-repellent flame-retardant protective suit fabric
CN103266393A (en) * 2013-05-14 2013-08-28 东华大学 Preparation method for water-repellent oil-repellent flame-retardant protective suit fabric
CN104372608A (en) * 2014-11-12 2015-02-25 江南大学 Method for preparing super-hydrophobic fabric by adopting sol-gel electrochemical deposition
CN104372608B (en) * 2014-11-12 2020-10-23 江南大学 Method for preparing super-hydrophobic fabric through sol-gel electrochemical deposition
CN104911907A (en) * 2015-06-08 2015-09-16 浙江理工大学 Low-pressure plasma sorting method endowing cotton fabric with fluoride-free water repellent function
CN105862386A (en) * 2016-04-25 2016-08-17 东莞市联洲知识产权运营管理有限公司 Method for preparing fluorescent-yellow dacron-cotton shell fabric
CN111094480A (en) * 2017-09-22 2020-05-01 3M创新有限公司 Polycarbodiimide-containing compositions, methods, and articles
CN109322143A (en) * 2018-12-07 2019-02-12 东华大学 A kind of type siloxane monomer plasma processing method of superhydrophobic surface material
CN109629231A (en) * 2018-12-07 2019-04-16 东华大学 A kind of methyl class monomer plasma processing method of superhydrophobic surface material
CN110067129A (en) * 2019-04-28 2019-07-30 东华大学 The method that corona treatment nano-particles reinforcement coating prepares superhydrophobic fabric
CN110644240A (en) * 2019-07-26 2020-01-03 南通大学 Preparation method of multifunctional durable and self-repairing super-hydrophobic fabric surface
CN112301725A (en) * 2019-08-02 2021-02-02 香港纺织及成衣研发中心 Waterproof fabric obtained by plasma technology and preparation method thereof
CN112301725B (en) * 2019-08-02 2023-04-07 香港纺织及成衣研发中心 Waterproof fabric obtained by plasma technique
CN110656484A (en) * 2019-09-24 2020-01-07 东华大学 Plasma treatment method of siloxane durable super-hydrophobic gradient film
CN113550144A (en) * 2021-08-18 2021-10-26 江南大学 Preparation method of antibacterial hydrophobic denim fabric
CN113550144B (en) * 2021-08-18 2022-04-05 江南大学 Preparation method of antibacterial hydrophobic denim fabric

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Application publication date: 20120411