CN104562637B - Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions - Google Patents
Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions Download PDFInfo
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- CN104562637B CN104562637B CN201510030697.1A CN201510030697A CN104562637B CN 104562637 B CN104562637 B CN 104562637B CN 201510030697 A CN201510030697 A CN 201510030697A CN 104562637 B CN104562637 B CN 104562637B
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
Abstract
The invention discloses a method for constructing a surface of a fabric with ultraviolet protection and wash-resistant special wetting functions. The method comprises the following steps: dissolving titanium potassium oxalate in a mixed solution of water and diethylene glycol; uniformly stirring under the action of a magnetic rotor; filling the prepared solution in a hydrothermal reaction kettle; adding a clean fabric into the hydrothermal reaction kettle and putting the kettle in an oven for reaction for preparing a fabric with a nano-TiO2 membrane surface; soaking the fabric with the nano-TiO2 membrane surface in a silane solution to react; and then taking out the fabric to be dried to prepare the fabric having the fabric surface with ultraviolet protection and wash-resistant special wetting functions. The method has the advantages of simple process, easiness in operation, controllable reaction condition, wide application range, wide source of raw materials, low cost, no pollution, excellent anti-ultraviolet property, wash resistance, lasting and stable super-hydrophobic self-cleaning property and good oil-water separation, and the fabric is excellent in comfortableness and air permeability.
Description
Technical field
The present invention relates to a kind of constructing in fabric surface and there is ultraviolet protection and water-fastness special wellability titanium dioxide
The construction method of titanium film layer.
Background technology
Ultraviolet (being called for short UV) can be divided into long wave ultraviolet UVA (320～400nm), ultraviolet B radiation UVB by radiation wavelength
(280～320nm) and short wave ultraviolet UVC (200～280nm), wherein, the ultraviolet wavelength section easily human body damaged
It is 290～400nm.If ultraviolet light absorbance and reflectance on fabric is the highest, then ultraviolet ray transmissivity is the lowest, product
Barrier propterty the best.The mechanism of textile ultraviolet protection is mainly derived from the fabric absorption to ultraviolet itself at present
Shielding action, or utilize screener ultraviolet is absorbed and reflects.The process utilizing screener can obtain excellent anti-purple
Outside line performance, main processing method has 2 kinds: one to be to add inorganic or organic screen agent when fibre forming, is fabricated to anti-purple
Outer line fiber；Two is to select ultraviolet light screener by fabric through padding or top finish imparting fabric anti-ultraviolet function.But
The former treatment technology require high, cost is big, how with polyester and polypropylene as base material, it is difficult to be applied to natural fiber, and mixed
When spinning, effect is difficult to control to；The product function wash resistant degree of the latter is poor, and Fabric Style is affected, be not suitable for the most very much with
The performances such as frivolous, ventilative, moisture absorption are main summer clothes fabric.
From 1997 German botanist Barthlott find the self_cleaning effect of lotus leaf surface and super-hydrophobic phenomenon with
Coming, super hydrophobic surface has caused the great interest of scientific research personnel and has paid close attention to widely.So-called super hydrophobic surface refers to and water
The surface that the contact angle dripped is more than 150 ° and roll angle is less than 10 °.Research finds, the micro nano structure pair of these super hydrophobic surfaces
Super-hydrophobicity plays vital effect.Nano-TiO2There is uviolresistance, chemical stability, heat stability, avirulence
Deng, it was widely used in ultraviolet ray-resistant material, field of textiles in the last few years.At present, most importantly by sol-gel process or electrospinning
Method prepares super hydrophobic surface, but these methods need special experimental facilities, experimental period long, nano-TiO2Pattern can not
Control.Therefore, how to prepare surface and there is lasting super-hydrophobic automatic cleaning performance, good mechanical performance, chemical stability, profit
Separating property etc., it is possible in free of losses liquid transport, micropipette pipe, UV resistance product, functional material, automatically cleaning weaving
Product, being used widely in the field such as oil-water separation material, becomes people's problem demanding prompt solution.
Summary of the invention
The present invention seeks to: provide a kind of and there is constructing of ultraviolet protection and water-fastness special wellability function fabric surface
Method, uses one step hydro thermal method to prepare micro-nano structure TiO2Film layer is modified with silicon fluoride and is combined, and solution is prepared super-hydrophobic from clear
Clean surface operation complex process, poor stability, TiO2The uncontrollable problem of film shape.
The technical scheme is that
A kind of construction method with ultraviolet protection and water-fastness special wellability function fabric surface, the method include as
Lower step:
(1) being dissolved in by titanium potassium oxalate in the mixed solution of water and diethylene glycol, under the effect of magnetic rotor, stirring is all
Even, the above-mentioned solution prepared is loaded in hydrothermal reaction kettle, in described hydrothermal reaction kettle, adds the fabric cleaned up also
Put in baking oven and react, prepare and there is nano-TiO2The fabric of film surface；With
(2) by described, there is nano-TiO2The fabric of film surface is immersed in silicon fluoride solution reaction, then takes out clear
Wash drying, prepare and there is ultraviolet protection and the fabric on water-fastness special wellability function fabric surface.
Further, titanium potassium oxalate is dissolved in the mixed solution of water and diethylene glycol described in step (1), at magnetic force
The step stirred under the effect of rotor includes: the titanium potassium oxalate of 0.5～5mmol is dissolved in deionized water and diethylene glycol
Mixed solution in, stir under the effect of magnetic rotor.
Further, described in step (1), the volume ratio of water and diethylene glycol is 3:4～4:3.
Further, the fabric cleaned up described in step (1) for sequentially passing through water, dehydrated alcohol ultrasonic cleaning, and
The fabric of dry for standby.
Further, in described hydrothermal reaction kettle, add the fabric cleaned up described in step (1) and put into baking oven
The temperature range of middle reaction is 100～250 DEG C.
Further, in described hydrothermal reaction kettle, add the fabric cleaned up described in step (1) and put into baking oven
The response time of middle reaction is 0.5～30h.
Further, after step (1) terminates, before step (2) starts, in addition it is also necessary to deionized water wash described in have
Nano-TiO2Unnecessary reactant on the fabric of film surface.
Further, described in step (2), silicon fluoride solution is 1H, 1H, 2H, 2H-perfluoro decyl triethoxysilane,
Any one in 1H, 1H, 2H, 2H-perfluoro capryl triethoxysilane, chlorosilane and siloxane compound is configured to
Solution.
Further, silicon fluoride solution described in step (2) be volume fraction be 1-6% silicon fluoride solution, it prepares step
Suddenly it is: adding 38～48ml methanol in the centrifuge tube of dried and clean, be then slowly added dropwise 0.5～3ml1H, 1H, 2H, 2H-are complete
Fluorine decyl triethoxysilane, drips 1.5～9ml H under the stirring action of magnetic rotor2O。
Further, step (2) has nano-TiO by described2The fabric of film surface is immersed in silicon fluoride solution
The time of reaction is 1h, and the drying temperature then taking out drying is 140 DEG C.
The invention have the advantage that
(1) one step hydro thermal method is used to obtain nano-TiO2Surface, preparation technology is simple, easy to operate, the TiO of preparation2Film layer
Morphology controllable, good endurance, solve many traditional method preparation sections complicated, time-consuming length, stability, bad mechanical property,
TiO2The problems such as surface topography is uncontrollable.
(2) silicon fluoride modifies nano-TiO2Bafta is achieved with super-hydrophobic automatic cleaning surface at short notice, additionally, knit
Thing surface exhibits goes out good oil-water separation phenomenon, and under external force rubbing action, has lasting ultra-hydrophobicity.Cotton fine
Dimension element is rich in natural resources in the world, and low cost, biodegradable are good, chemical resistance is good, nonhazardous, can directly connect with food
Touch, solve cost of material high, the problems such as environmental pollution is serious, and can be in free of losses liquid transport, micropipette pipe, antifouling
Dye, ultraviolet ray-resistant material, super-hydrophobic textile, oil-water separation material etc. are extensively applied.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, required use in embodiment being described below
Accompanying drawing be briefly described, it should be apparent that, below describe in accompanying drawing be only some embodiments of the present invention, for this
From the point of view of the those of ordinary skill of field, on the premise of not paying creative work, it is also possible to obtain other according to these accompanying drawings
Accompanying drawing.Wherein,
Fig. 1 is of the present invention a kind of to have constructing of ultraviolet protection and water-fastness special wellability function fabric surface
The step schematic diagram of method；
Fig. 2 is a kind of Ti unit with ultraviolet protection and water-fastness special wellability function fabric surface of the present invention
Element distribution and EDS can spectrograms；
Fig. 3 is a kind of XPS with ultraviolet protection and water-fastness special wellability function fabric surface of the present invention
Spectrogram；
Fig. 4 is a kind of pattern with ultraviolet protection and water-fastness special wellability function fabric surface of the present invention
And contact angle；
Fig. 5 is a kind of side of constructing with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment one of method；
Fig. 6 is a kind of side of constructing with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment two of method；
Fig. 7 is a kind of side of constructing with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment three of method；
Fig. 8 is a kind of side of constructing with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment four of method；
Fig. 9 is of the present invention a kind of to have constructing of ultraviolet protection and water-fastness special wellability dacron surface
The SEM figure of the micro-nano structure surface prepared by embodiment five of method；
Figure 10 is of the present invention a kind of to have constructing of ultraviolet protection and water-fastness special wellability surface of cotton fabric
Method when hydro-thermal 180 DEG C, ultraviolet protection prepared by different time and water-fastness special wellability function fabric surface according to
AATCC standard washes the contact angle changing trend diagram of five times；With
Figure 11 is of the present invention a kind of to have constructing of ultraviolet protection and water-fastness special wellability surface of cotton fabric
Method is when hydro-thermal 20h, and ultraviolet protection prepared by different temperatures and water-fastness special wellability function fabric surface are according to AATCC
Standard washes the contact angle changing trend diagram of five times.
Detailed description of the invention
The present invention provides a kind of construction method with ultraviolet protection and water-fastness special wellability function fabric surface, bag
Include following steps:
A kind of construction method with ultraviolet protection and water-fastness special wellability function fabric surface, the method include as
Lower step:
(1) one step hydro thermal method prepares and has nano-TiO2The fabric of film surface；With
(2) silicon fluoride is modified to prepare and is had ultraviolet protection and the fabric on water-fastness special wellability function fabric surface.
Understandable, below in conjunction with detailed description of the invention for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from
The present invention is further detailed explanation.
A kind of construction method with ultraviolet protection and water-fastness special wellability function fabric surface, including:
Step one: one step hydro thermal method prepares has nano-TiO2The fabric of film surface；
In one embodiment, this step can specific as follows perform: first by fabric according to 3 × 3cm specification cutting 5 pieces,
Be placed in beaker sequentially passing through deionized water, the ultrasonic 5min of dehydrated alcohol, ultrasonic after put into 80 DEG C of baking oven and be dried, cooling
Standby.The titanium potassium oxalate of 0.5～5mol is dissolved in the mixed solution of water that volume ratio is 3:4～4:3 and diethylene glycol,
Stir under the effect of magnetic rotor, then the solution prepared is contained in hydrothermal reaction kettle, at described hydrothermal reaction kettle
Middle addition sequentially passes through water, dehydrated alcohol ultrasonic cleaning, and the fabric of dry for standby and puts in baking oven 100～250 DEG C of temperature
The lower reaction 0.5～30h of degree；
Step 2: silicon fluoride is modified to prepare has knitting of ultraviolet protection and water-fastness special wellability function fabric surface
Thing.
In one embodiment, this step can specific as follows perform: in the centrifuge tube of dried and clean add 38～
48ml methanol, the most slowly dropping 0.5～3ml 1H, 1H, 2H, 2H-perfluoro decyl triethoxysilane, 1H, 1H, 2H, 2H-are complete
Any one solution being configured in fluorine octyltri-ethoxysilane, chlorosilane and siloxane compound, adds magnetic force
Rotor is slowly added dropwise 1.5～9.0ml H when stirring2O, continuously stirred 1h at room temperature standing used after half a day.
Deposition nano-TiO prepared by above-mentioned hydro-thermal method2Fabric face is immersed in inside the silicon fluoride solution prepared, and takes after 1h
Go out, and dry at 140 DEG C.
It is that one of the present invention has ultraviolet protection and water-fastness special leaching that above-mentioned steps process see Fig. 1, Fig. 1
The step schematic diagram of the construction method on lubricant nature function fabric surface.As it is shown in figure 1, bafta first passes around hydro-thermal reaction builds two
Rank micro-nano structure TiO2@surface of cotton fabric, then modifies through silicon fluoride solution and obtains super-hydrophobic automatic cleaning function fabric surface.
Above-mentioned steps experimental results refers to Fig. 2-Fig. 4, and referring to Fig. 2, Fig. 2 is that one of the present invention has
Ultraviolet protection and the Ti Elemental redistribution on water-fastness special wellability function fabric surface and EDS can spectrograms.Top as shown in Figure 2
Micro-nano structure TiO for preparation2Surface of cotton fabric constituent content spectrogram；Lower section is the micro-nano structure TiO of preparation2Surface of cotton fabric
The scattergram of element ti, the SEM of embedding is fabric sweep limits, turns right successively as Elements C, O scattergram.
Referring to Fig. 3, Fig. 3 is that one of the present invention has ultraviolet protection and water-fastness special wellability function fabric
The XPS spectrum figure on surface.As shown in Fig. 3 (a), the deposition nano-TiO of preparation2Fabric face occurs in that obvious Ti peak, compared to
The nano-TiO of unmodified2Fabric, as shown in Fig. 3 (b), at the nano-TiO of silicon fluoride modified2Fabric face detects fluorine element
Signal peak, illustrates that silicon fluoride the most successfully modifies nano-TiO2Fabric face, and give fabric super-hydrophobic special wellability.
Referring to Fig. 4, Fig. 4 is that one of the present invention has ultraviolet protection and water-fastness special wellability function fabric
The pattern on surface and contact angle.As shown in Figure 4, the special wellability function fabric surface of preparation presents class " Flos Tagetis Erectae " shape
Micro nano structure, it is thus achieved that super hydrophobic surface, contact angle reaches more than 158 °.
Understandable for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from, below in conjunction with the accompanying drawings and embodiment
Further illustrate technical scheme.But the invention is not restricted to listed embodiment, also should be included in institute of the present invention
Other any known changes in the interest field required.
First, " embodiment " or " embodiment " referred to herein refers to may be included at least one realization side of the present invention
Special characteristic, structure or characteristic in formula.Different in this manual local " in one embodiment " occurred not refer both to
Same embodiment, is not single or the most mutually exclusive with other embodiments embodiment.
Secondly, the present invention utilizes structural representation etc. to be described in detail, when describing the embodiment of the present invention in detail, for ease of saying
Bright, schematic diagram can be disobeyed general ratio and be made partial enlargement, and described schematic diagram is example, and it should not limit the present invention at this
The scope of protection.Additionally, the three dimensions of length, width and the degree of depth should be comprised in actual fabrication.
It addition, the letter abbreviation said in the present invention, being the fixing abbreviation in this area, wherein subalphbet literary composition is explained such as
Under: TiO2@bafta: deposition has the surface of cotton fabric of titanium dioxide nanoparticle；PDES:1H, 1H, 2H, 2H-perfluoro decyl three
Ethoxysilane；PTES:1H, 1H, 2H, 2H-perfluoro capryl triethoxysilane；SEM schemes: electron scanning imaging figure；EDS schemes:
Can spectrogram；XPS spectrum figure: X-ray photoelectron spectroscopic analysis spectrogram.
More, below as a example by silicon fluoride solution is for PDES solution owing to implementing kind.
Embodiment one
Present embodiment prepares a kind of ultraviolet protection and water-fastness special wellability function fabric surface in accordance with the following steps:
Step one, one step hydro thermal method prepare has nano-TiO2The cotton of film surface
By cotton according to 3 × 3cm specification cutting 5 pieces, it is placed in beaker sequentially passing through deionized water, dehydrated alcohol ultrasonic
5min, ultrasonic after put into 80 DEG C of baking oven be dried, cool down standby.With electronic balance weighing 0.5mmol titanium potassium oxalate, it is dissolved in
In the mixed solution of 15ml deionized water and 20ml diethylene glycol, stir under the effect of magnetic rotor, be subsequently adding clear
The cotton of wash clean, is placed in hydrothermal reaction kettle and pressurizes and tighten, and hydrothermal reaction kettle is finally put into the reaction of 100 DEG C of baking oven
0.5h, reacts and thoroughly cleans up the reactant that surface of cotton fabric is unnecessary after terminating with deionized water.
Step 2, silicon fluoride are modified to prepare has ultraviolet protection and the cotton on water-fastness special wellability function fabric surface
In the centrifuge tube of dried and clean, add 38ml methanol, the most slowly dropping 0.5ml PDES, add magnetic rotor
It is slowly added dropwise 1.5ml H when stirring2O, continuously stirred 1h at room temperature standing used after half a day.By above-mentioned hydro-thermal
Deposition nano-TiO prepared by method2Surface of cotton fabric is immersed in inside the silicon fluoride solution prepared, and takes out after 1h, and 140
Dry at DEG C.
Ultraviolet protection and the appearance structure on water-fastness special wellability function fabric surface prepared by the present embodiment refer to
Fig. 5, Fig. 5 are a kind of construction method with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment one.
Embodiment two
Present embodiment prepares a kind of ultraviolet protection and water-fastness special wellability function fabric surface in accordance with the following steps:
Step one, one step hydro thermal method prepare has nano-TiO2The cotton of film surface
By cotton according to 3 × 3cm specification cutting 5 pieces, it is placed in beaker sequentially passing through deionized water, dehydrated alcohol ultrasonic
5min, ultrasonic after put into 80 DEG C of baking oven be dried, cool down standby.With electronic balance weighing 2mmol titanium potassium oxalate, it is dissolved in
In the mixed solution of 15ml deionized water and 20ml diethylene glycol, stir under the effect of magnetic rotor, be subsequently adding clear
The cotton of wash clean, is placed in hydrothermal reaction kettle and pressurizes and tighten, and hydrothermal reaction kettle is finally put into 150 DEG C of baking oven reaction 10h,
React and after terminating, thoroughly clean up the reactant that surface of cotton fabric is unnecessary with deionized water.
Step 2, silicon fluoride are modified to prepare has ultraviolet protection and the cotton on water-fastness special wellability function fabric surface
In the centrifuge tube of dried and clean, add 40ml methanol, the most slowly dropping 1.0ml PDES, add magnetic rotor
It is slowly added dropwise 4ml H when stirring2O, continuously stirred 1h at room temperature standing used after half a day.By above-mentioned hydro-thermal method
The deposition nano-TiO of preparation2Surface of cotton fabric is immersed in inside the silicon fluoride solution prepared, and takes out after 1h, and at 140 DEG C
Lower drying.
Ultraviolet protection and the appearance structure on water-fastness special wellability function fabric surface prepared by the present embodiment refer to
Fig. 6.Fig. 6 is a kind of construction method with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment two.
Embodiment three
Present embodiment prepares a kind of ultraviolet protection and water-fastness special wellability function fabric surface in accordance with the following steps:
Step one, one step hydro thermal method prepare has nano-TiO2The cotton of film surface
By cotton according to 3 × 3cm specification cutting 5 pieces, it is placed in beaker sequentially passing through deionized water, dehydrated alcohol ultrasonic
5min, ultrasonic after put into 80 DEG C of baking oven be dried, cool down standby.With electronic balance weighing 3mmol titanium potassium oxalate, it is dissolved in
In the mixed solution of 20ml deionized water and 15ml diethylene glycol, stir under the effect of magnetic rotor, be subsequently adding clear
The cotton of wash clean, is placed in hydrothermal reaction kettle and pressurizes and tighten, and hydrothermal reaction kettle is finally put into 180 DEG C of baking oven reaction 20h,
React and after terminating, thoroughly clean up the reactant that surface of cotton fabric is unnecessary with deionized water.
Step 2, silicon fluoride are modified to prepare has ultraviolet protection and the cotton on water-fastness special wellability function fabric surface
In the centrifuge tube of dried and clean, add 42ml methanol, the most slowly dropping 2ml PDES, add magnetic rotor and exist
It is slowly added dropwise 7ml H under the state of stirring2O, continuously stirred 1h, and at room temperature standing used after half a day.By above-mentioned hydro-thermal method
The deposition nano-TiO of preparation2Surface of cotton fabric is immersed in inside the silicon fluoride solution prepared, and takes out after 1h, and at 140 DEG C
Lower drying.
Ultraviolet protection and the appearance structure on water-fastness special wellability function fabric surface prepared by the present embodiment refer to
Fig. 7, Fig. 7 are a kind of construction method with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment three.
Embodiment four
Present embodiment prepares a kind of ultraviolet protection and water-fastness special wellability function fabric surface in accordance with the following steps:
Step one, one step hydro thermal method prepare has nano-TiO2The cotton of film surface
By cotton according to 3 × 3cm specification cutting 5 pieces, it is placed in beaker sequentially passing through deionized water, dehydrated alcohol ultrasonic
5min, ultrasonic after put into 80 DEG C of baking oven be dried, cool down standby.With electronic balance weighing 5mmol titanium potassium oxalate, it is dissolved in
In the mixed solution of 20ml deionized water and 15ml diethylene glycol, stir under the effect of magnetic rotor, be subsequently adding clear
The cotton of wash clean, is placed in hydrothermal reaction kettle and pressurizes and tighten, and hydrothermal reaction kettle is finally put into 250 DEG C of baking oven reaction 30h,
React and after terminating, thoroughly clean up the reactant that surface of cotton fabric is unnecessary with deionized water.
Step 2, silicon fluoride are modified to prepare has ultraviolet protection and the cotton on water-fastness special wellability function fabric surface
In the centrifuge tube of dried and clean, add 48ml methanol, the most slowly dropping 3ml PDES, add magnetic rotor and exist
It is slowly added dropwise 9ml H under the state of stirring2O, continuously stirred 1h at room temperature standing used after half a day.By above-mentioned hydro-thermal legal system
Standby deposition nano-TiO2Surface of cotton fabric is immersed in inside the silicon fluoride solution prepared, and takes out after 1h, and at 140 DEG C
Dry.
Ultraviolet protection and the appearance structure on water-fastness special wellability function fabric surface prepared by the present embodiment refer to
Fig. 8, Fig. 8 are a kind of construction method with ultraviolet protection and water-fastness special wellability surface of cotton fabric of the present invention
The SEM figure of the micro-nano structure surface prepared by embodiment four.
Embodiment five
Present embodiment prepares a kind of ultraviolet protection and water-fastness special wellability function fabric surface in accordance with the following steps:
Step one, one step hydro thermal method prepare has nano-TiO2The dacron surface of film surface
By terylene according to 3 × 3cm specification cutting 5 pieces, it is placed in beaker sequentially passing through deionized water, dehydrated alcohol ultrasonic
5min, ultrasonic after put into 80 DEG C of baking oven be dried, cool down standby.With electronic balance weighing 3mmol titanium potassium oxalate, it is dissolved in
In the mixed solution of 20ml deionized water and 15ml diethylene glycol, stir under the effect of magnetic rotor, be subsequently adding clear
The terylene of wash clean, is placed in hydrothermal reaction kettle and pressurizes and tighten, and hydrothermal reaction kettle is finally put into 150 DEG C of baking oven reaction 10h,
React the reactant thoroughly cleaning up dacron excess surface after terminating with deionized water.
Step 2, silicon fluoride are modified to prepare has ultraviolet protection and the terylene on water-fastness special wellability function fabric surface
Fabric
In the centrifuge tube of dried and clean, add 48ml methanol, the most slowly dropping 0.5ml PDES, add magnetic rotor
It is slowly added dropwise 1.5ml H when stirring2O, continuously stirred 1h at room temperature standing used after half a day.By above-mentioned hydro-thermal
Deposition nano-TiO prepared by method2Dacron surface is immersed in inside the silicon fluoride solution prepared, and takes out after 1h, and
Dry at 140 DEG C.
Ultraviolet protection and the appearance structure on water-fastness special wellability function fabric surface prepared by the present embodiment refer to
Fig. 9, Fig. 9 are a kind of construction method with ultraviolet protection and water-fastness special wellability dacron surface of the present invention
The micro-nano structure surface prepared by embodiment four SEM figure.
Following table is a kind of ultraviolet protection and the ultraviolet protection on water-fastness special wellability function fabric surface of the present invention
Energy data:
| Sample | UPF | T(UVA) | T(UVB) | UPFRating |
| Pristine | 3.95 | 30.74% | 23.77% | 0 |
| 180℃1h | 12.74 | 23.4% | 5.97% | 10 |
| 180℃2h | 47.08 | 5.16% | 1.98% | 45 |
| 180℃5h | 56.65 | 3.77% | 1.67% | 50+ |
| 180℃10h | 43.52 | 5.64% | 2.11% | 40 |
| 180℃20h | 50.98 | 3.81% | 1.89% | 50+ |
Table one
As shown in Table 1, the blank sample UV resistance coefficient not doing any process is 0, and sample prepared by 180 DEG C of 1h of hydro-thermal
UV resistance ability reaches 10, and sample prepared by 5h obtains splendid UV resistance effect, and nano-TiO2Nontoxic, can be direct
With contact skin, in fields such as UV resistance textile, functional materials, there is broad development prospect.
In above five embodiments, modify the ultraviolet protection of preparation and water-fastness spy by one step hydro thermal method and silicon fluoride
Different wellability function fabric surface has lasting hydrophobicity under external world's friction and washing effect, refers to Figure 10, Figure 10
A kind of there is the construction method on ultraviolet protection and water-fastness special wellability function fabric surface in hydro-thermal for of the present invention
When 180 DEG C, ultraviolet protection and water-fastness special wellability function fabric surface prepared by different time are washed according to AATCC standard
The contact angle changing trend diagram of five times.As shown in Figure 10,180 ° of C of hydro-thermal of preparation are washed not according to the 2A method of AATCC standard
With time special wellability function fabric surface, through 5 reinforcement circulation fabric faces and the contact angle variation tendency of water, from figure
10 it can be seen that after strengthening washing five times sample maintain preferable hydrophobicity, fabric face longitude and latitude interlacing point is to be vulnerable to most
The position of friction destruction, at these position nano-TiOs2Granule falls off or destroys, and causes bafta hydrophobic performance to have slightly
Degree declines.
It is that one of the present invention has ultraviolet protection and water-fastness special wellability function fabric refering to Figure 11, Figure 11
The construction method on surface when hydro-thermal 20h, ultraviolet protection prepared by different temperatures and water-fastness special wellability function fabric table
The contact angle changing trend diagram of five times is washed according to AATCC standard in face.As shown in figure 11, the water-fastness effect of sample of 200 DEG C of preparations
The most worst, but it is maintained at more than 140 °, this is because along with the rising of temperature, fibrous inside occurs swelling, is deposited on surface
TiO2Film layer occurs that explosion even comes off, and after AATCC standard is washed, fabric face nano-particle is under the effect of mechanical external force
Occurring friction to drop, surface topography destroys.
In sum, the invention discloses and a kind of there is ultraviolet protection and water-fastness special wellability function fabric surface
Construction method, this method takes full advantage of one step hydro thermal method on the basis of prior art and builds micro-nano second order TiO2Fabric harsh
Body structure surface modifies, with silicon fluoride, the method combined, it is thus achieved that super-hydrophobic automatic cleaning and oil-water separating function surface.It reacts bar
Part is gentle, and simple process easily operates, the nano-TiO of preparation2Morphology controllable, after friction, ultra-hydrophobicity is excellent, to environment without dirt
Dye, have a good application prospect, can free of losses liquid transport, micropipette pipe, UV resistance product, functional material, from
Cleaning fabric, profit detachable material etc. are well applied.
It should be noted that above example is only in order to illustrate technical scheme and unrestricted, although with reference to preferably
The present invention has been described in detail by embodiment, it will be understood by those within the art that, can be to the technology of the present invention
Scheme is modified or equivalent, and without deviating from the spirit and scope of technical solution of the present invention, it all should be contained at this
In the middle of bright right.
Claims (9)
1. a construction method with ultraviolet protection and water-fastness special wellability function fabric surface, it is characterised in that should
Method comprises the steps:
(1) being dissolved in by titanium potassium oxalate in the mixed solution of water and diethylene glycol, the volume ratio of described water and diethylene glycol is 3:4
～4:3, stir under the effect of magnetic rotor, the above-mentioned solution prepared is loaded in hydrothermal reaction kettle, at described water
Thermal response still add the fabric cleaned up and puts into reaction in baking oven, preparing and there is nano-TiO2The cotton of film surface；
With
(2) by described, there is nano-TiO2The fabric of film surface is immersed in silicon fluoride solution reaction, then takes out cleaning and dries
Dry, prepare and there is ultraviolet protection and the fabric on water-fastness special wellability function fabric surface.
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 1
Method, it is characterised in that: titanium potassium oxalate is dissolved in the mixed solution of water and diethylene glycol described in (1) by step, turns at magnetic force
Under the effect of son, the step that stirs includes: the titanium potassium oxalate of 0.5～5mmol is dissolved in deionized water and diethylene glycol
In mixed solution, stir under the effect of magnetic rotor.
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 1
Method, it is characterised in that: the fabric cleaned up described in step (1) is for sequentially passing through water, dehydrated alcohol ultrasonic cleaning, and dries
Standby fabric.
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 1
Method, it is characterised in that: in described hydrothermal reaction kettle, add the fabric cleaned up described in step (1) and put in baking oven anti-
The temperature range answered is 100～250 DEG C.
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 1
Method, it is characterised in that: in described hydrothermal reaction kettle, add the fabric cleaned up described in step (1) and put in baking oven anti-
The response time answered is 0.5～30h.
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 1
Method, it is characterised in that: after step (1) terminates, before step (2) starts, in addition it is also necessary to deionized water wash described in have and receive
Rice TiO2Unnecessary reactant on the fabric of film surface.
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 1
Method, it is characterised in that: described in step (2), silicon fluoride solution is 1H, 1H, 2H, 2H-perfluoro decyl triethoxysilane, 1H,
It is molten that any one in 1H, 2H, 2H-perfluoro capryl triethoxysilane, chlorosilane and siloxane compound is configured to
Liquid.
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 7
Method, it is characterised in that silicon fluoride solution described in step (2) be volume fraction be 1-6% silicon fluoride solution, its preparation steps
For: in the centrifuge tube of dried and clean, add 38～48ml methanol, be then slowly added dropwise 0.5～3ml 1H, 1H, 2H, 2H-perfluor
Decyl triethoxysilane, drips 1.5～9ml H under the stirring action of magnetic rotor2O。
The side of constructing with ultraviolet protection and water-fastness special wellability function fabric surface the most according to claim 1
Method, it is characterised in that step has nano-TiO by described in (2)2The fabric of film surface is immersed in silicon fluoride solution reaction
Time be 1h, the drying temperature then taking out drying is 140 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510030697.1A CN104562637B (en) | 2015-01-21 | 2015-01-21 | Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions |
| PCT/CN2016/070294 WO2016115980A1 (en) | 2015-01-21 | 2016-01-06 | Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions |
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| CN201510030697.1A CN104562637B (en) | 2015-01-21 | 2015-01-21 | Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions |
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| CN104562637B true CN104562637B (en) | 2017-01-11 |
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| WO (1) | WO2016115980A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104562637B (en) * | 2015-01-21 | 2017-01-11 | 苏州大学 | Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions |
| CN105568669B (en) * | 2015-12-31 | 2018-07-31 | 苏州榕绿纳米科技有限公司 | A kind of antibacterial fabric and preparation method thereof |
| CN107217368A (en) * | 2016-03-22 | 2017-09-29 | 孙彦飞 | A kind of waterproof antistatic cloth and its manufacture method |
| CN106495213B (en) * | 2016-11-24 | 2018-01-12 | 安徽理工大学 | A kind of TiO2Transparent self-supported membrane and its preparation method and application |
| CN106702718B (en) * | 2016-12-05 | 2019-05-14 | 苏州榕绿纳米科技有限公司 | A kind of special wellability uvioresistant function fabric construction method of super abrasive |
| CN111379163A (en) * | 2018-12-29 | 2020-07-07 | 江苏唐工纺实业有限公司 | Based on radial nano TiO2Preparation method of lyophobic polyester fabric |
| CN111172747A (en) * | 2019-12-30 | 2020-05-19 | 比音勒芬服饰股份有限公司 | Anti-ultraviolet fabric and preparation method and application thereof |
| CN112342792B (en) * | 2020-12-18 | 2021-11-26 | 福州大学 | Method for constructing surface of fabric with passive daytime radiation cooling function and special wettability function |
| CN115701463A (en) * | 2021-08-02 | 2023-02-10 | 安徽璜峪电磁技术有限公司 | Composite material constructed by multilevel structure and preparation method and application thereof |
| CN113774652B (en) * | 2021-09-10 | 2023-02-21 | 盐城工学院 | BiOCl-Bi 2 WO 6 Preparation method of functionalized cotton fabric |
| CN114434919A (en) * | 2022-01-25 | 2022-05-06 | 安徽工程大学 | Three-layer structure firefighter uniform with self-cleaning function and production method thereof |
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| CN1211500C (en) * | 2003-03-27 | 2005-07-20 | 厦门大学 | Metal surface anti-corrosion method based on surface nanometer construct |
| CN102277724B (en) * | 2011-06-28 | 2013-01-16 | 东华大学 | Method for clearing up nanometer uvioresistant antibacterial self-cleaning fabric |
| CN103409984B (en) * | 2013-07-15 | 2015-10-28 | 东华大学 | A kind of method at surface of cotton fabric low-temperature growth anatase titanium dioxide film |
| CN103871750B (en) * | 2014-03-20 | 2017-01-11 | 华中科技大学 | Anatase TiO2 nanometer tree array and application of anatase TiO2 nanometer tree array to solar cell preparation |
| CN104294592B (en) * | 2014-10-16 | 2017-01-11 | 苏州大学 | Preparation method of special-infiltration functional fabric surface with self-cleaning and oil-water separation functions |
| CN104562637B (en) * | 2015-01-21 | 2017-01-11 | 苏州大学 | Method for constructing surface of fabric with ultraviolet protection and wash-resistant special wetting functions |
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| WO2016115980A1 (en) | 2016-07-28 |
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