CN109518468A - A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent - Google Patents

A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent Download PDF

Info

Publication number
CN109518468A
CN109518468A CN201811347432.4A CN201811347432A CN109518468A CN 109518468 A CN109518468 A CN 109518468A CN 201811347432 A CN201811347432 A CN 201811347432A CN 109518468 A CN109518468 A CN 109518468A
Authority
CN
China
Prior art keywords
finishing agent
fabric
superhydrophobic fabric
superhydrophobic
alcohol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811347432.4A
Other languages
Chinese (zh)
Inventor
张俊平
严杰
刘克静
赵林
曹晓君
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lanzhou Institute of Chemical Physics LICP of CAS
Original Assignee
Shandong Xinna Chaoshu New Materials Co Ltd
Shubo (shanghai) Nanotechnology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shandong Xinna Chaoshu New Materials Co Ltd, Shubo (shanghai) Nanotechnology Co Ltd filed Critical Shandong Xinna Chaoshu New Materials Co Ltd
Priority to CN201811347432.4A priority Critical patent/CN109518468A/en
Publication of CN109518468A publication Critical patent/CN109518468A/en
Pending legal-status Critical Current

Links

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/65Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/6436Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • D06M2101/12Keratin fibres or silk
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35Abrasion, pilling or fibrillation resistance
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50Modified hand or grip properties; Softening compositions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

It is that organosilicon and organosilan are added to hydrolytic condensation in alkaline alcohol-water solution and obtained the invention discloses a kind of organosilicon polymer superhydrophobic fabric finishing agent.The organosilicon superhydrophobic fabric finishing agent contains hydrophobic grouping and coupling group, and in dip-coating and high temperature cure process, coupling group can be chemically bonded with the fiber of fabric, and hydrophobic grouping can play super-hydrophobic effect.By fabric in 5-10 times of fabric of organosilicon finish solution of dilution dip-coating 2-10min, then in 80-180 DEG C of solidification 2-10min to get superhydrophobic fabric.The superhydrophobic fabric has many advantages, such as that ultra-hydrophobicity is excellent and water-fastness, it can be used for constructing for a variety of superhydrophobic fabrics, it is not required to pre-process fabric, greatlies simplify preparation process, and maintain the performances such as the intrinsic mechanical strength of fabric, flexibility, gloss and feel.

Description

A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent
Technical field
The present invention relates to a kind of preparation methods of superhydrophobic fabric finishing agent, and in particular to a kind of organosilicon polymer is super thin The preparation and its application method of water fabric finishing agent.
Background technique
Lotus leaf has the characteristics that mud is without contaminating out.It is inspired by lotus leaf effect, super hydrophobic surface receives significant attention.It is super thin Water surface refers to that water droplet is greater than 150 ° in its surface contact angle, and the lower surface of roll angle has excellent self-cleaning performance, The fields such as automatically cleaning textile, water-oil separating, anti-corrosion, anti-freeze are with a wide range of applications.The research of super hydrophobic surface is drawn Extensive interest is played.
Production, the life of textile and people are closely bound up.The research and development of functional textile is increasingly by weight Depending on significantly improving people's lives quality.Different from other function textile, superhydrophobic fabric is the same because having lotus leaf Self-cleaning effect and be concerned.The preparation of super hydrophobic surface, which generally requires, first constructs coarse surface texture, then carries out low Surface can be modified and be made.Textile itself has certain micron order texture structure, and therefore, the preparation of superhydrophobic fabric is concentrated In the preparation of novel fabric finishing agent and in terms of how improving itself and fabric being firmly combined property.The type of superhydrophobic fabric finishing agent It is very more, including fluorine silicon resin, fluorocarbon resin, organic siliconresin etc..But these finishing agents, which are used to prepare superhydrophobic fabric, to be deposited Water-wash resistance is poor, stability is not high, a series of problems, such as containing PFOS/PFOA, become the bottle of superhydrophobic fabric preparation and application Neck.Therefore, some to study the raising for focusing on superhydrophobic fabric stability, i.e., it is firm in conjunction with fabric how to improve fabric finishing agent In terms of solidity.Then patent CN102352549A is coated, is finally carried out low first in fabric surface dip-coating inorganic nano-particle Surface can change surname, obtain superhydrophobic fabric.Patent CN100595373C is using gold chloride and citric acid as catalyst, in cotton fabric table Face supported nano-gold particle then carries out low-surface-energy modification, obtains superhydrophobic fabric, and after repeatedly folding, ultra-hydrophobicity is good It is good.Patent CN102174737A, in fabric surface covalent bond polyalkyl methacrylate, has by irradiation grafting technology Certain water-fastness stability.Although these methods improve the stability of superhydrophobic fabric to a certain extent, still need By fabric surface activation, x ray irradiation x and low-surface-energy modification etc. multiple steps could complete, not only influence fabric intensity, Appearance, and complex process, the serious practical application for limiting superhydrophobic fabric.Therefore, how to be made super thin by simple method Water fabric finishing agent, and being applied to the excellent superhydrophobic fabric of processability by simple technique is that this field is urgently to be resolved Difficult point.
Summary of the invention
The purpose of the present invention is to solve problem of the existing technology, provide that a kind of organosilicon polymer is super-hydrophobic to be knitted The preparation method of object finishing agent;
It is a further object of the present invention to provide the specifically used methods of above-mentioned organosilicon polymer superhydrophobic fabric finishing agent.
(1) preparation of organosilicon polymer superhydrophobic fabric finishing agent
The preparation of organosilicon polymer superhydrophobic fabric finishing agent of the present invention is by organosilan and organosilicon in alkaline alcohol solution Middle hydrolytic condensation is made.Specific preparation process are as follows: organosilicon and organosilan are added in alkaline alcohol-water solution, 25 ~ 2 ~ 48h of hydrolytic condensation at 80 DEG C;It is cooled to room temperature, adjusts pH to neutrality, obtain superhydrophobic fabric finishing agent.
The organosilicon is poly dimethyl dimethoxysilane, polyphenylene silicone resin, polydimethyl siloxanes, poly- methyl second At least one of alkenyl silicone resin;Volume fraction of the organosilicon in alcohol-water solution is 0.5% ~ 5%.
The organosilan is tetraethoxysilane, sodium methyl silicate, potassium methyl silicate, waterglass, aminopropyl trimethoxy Base silane, 3- (the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, methyltriethoxysilane, ethyl triethoxysilane, second Alkenyl triethoxysilane, phenyl triethoxysilane, octyltri-ethoxysilane, dodecyl triethoxysilane, 16 At least one of alkyl triethoxysilane, octadecyltriethoxy silane and corresponding methoxy silane;Organosilan Volume fraction in alkaline alcohol-water solution is 1% ~ 4%.
It is described alkalinity alcohol-water solution in, alcohol be at least one of methanol, ethyl alcohol, isopropanol, ethylene glycol, glycerol, alcohol with The volume ratio of water is 9:1 ~ 1:1.
In the alkalinity alcohol-water solution, alkali be ammonium hydroxide, sodium hydroxide, potassium hydroxide, ethylenediamine, in triethylamine at least One kind, alkali are 0.2% ~ 2% in the concentration of alcohol-water solution.
Organosilicon polymer superhydrophobic fabric finishing agent prepared by the present invention contains hydrophobic grouping and coupling group, in dip-coating In high temperature cure process, coupling group can be chemically bonded with the fiber of fabric, and hydrophobic grouping can play super thin Water effect.
(2) preparation of superhydrophobic fabric
Superhydrophobic fabric finishing agent prepared by the present invention ethanol/water is diluted 5 ~ 10 times, superhydrophobic fabric finishing agent is added 0.1% ~ 1% acetic acid is as catalyst;Fabric is dipped in wherein 2 ~ 10min of standing, then in 80 ~ 180 DEG C of 2 ~ 10min of solidification, i.e., Obtain superhydrophobic fabric.
In order to improve the dispersing uniformity of superhydrophobic fabric finishing agent, after superhydrophobic fabric finishing agent is diluted with ethyl alcohol, 3 ~ 5min of re-ultrasonic dispersion.
The fabric is polyester, cotton, wool, silk, acrylic fibers, nylon, polyurethane and its blended fabric etc..Time of immersion and Solidification temperature is according to fabric composition and weaving different from.
(3) super-hydrophobicity and estimation of stability
1, water droplet rolling angle measures
Test method: based on some substrate material surfaces (such as fabric) it is macroscopically very coarse, carry out contact angle test when be to be difficult The profile of observed drop.And classical contact angle test method is highly dependent on the analysis of droplet profile.Therefore according to report Method carries out surface wettability evaluation (Fig. 1) instead of the contact angle and roll angle of water with the rolling angle of water.The test of rolling angle Method are as follows: sample is fixed on sample stage (Fig. 1 b), then is placed on the sloping platform of Contact-angle measurement system.Syringe is placed in Above tilting table, fixed syringe needle to substrate distance is 10 mm, and a drop water is dripped to needle contact to substrate.Internal diameter is 110μM syringe needle is used to be added dropwise 10 ± 0.3μThe water droplet of L volume.Since the measurement of rolling angle tilting 50o.Drop is at least It can be dripped on three ground of sample surfaces.If all drops can be flicked or be tumbled in sample surfaces, tilt angle just reduces by 2 O, same step repeat until a drop or much to drip drop cannot be tumbled from surface for until.All water droplets can be complete from surface The minimum cant for tumbling or flicking is regarded as rolling angle.
Measurement result: rolling angle < 10 ° illustrate that obtained superhydrophobic fabric has excellent super-hydrophobicity (Fig. 2).
2, washing fastness
Test method: being added 32L water and 96g liquid detergent in washing machine, by sample in washing machine and other 10 piece 20 × 20 The cotton of cm washs ten circulations together at room temperature, and 45min is a circulation.After each wash cycle, cloth is spent Ionized water washes clean tests its rolling angle after 60 DEG C of oven dryings.
Measurement result: after washing 20 times, rolling angle is still below 15 °, and water droplet is easily tumbled from surface, and ultra-hydrophobicity is excellent, Illustrate that the made superhydrophobic fabric of the present invention has good washing fastness.
3, wearability
Test method: sample is fixed on after stainless steel column in moving back and forth on wear medium by tear strength of 10 kPa, 40 Cm is an abrasion cycles (Fig. 3).In order to simulate actual use situation as far as possible, wear test use respectively A4 paper, polyester cloth Ι and 2000 mesh sand paper are that wear medium is tested.After abrasion 10,50,100 and 200 times, its corresponding rolling angle is measured.
Test result: under 10KPa load after reciprocating friction 200 times, rolling angle is still below 15 °, and water droplet is easily tumbled from surface, Ultra-hydrophobicity is excellent, illustrates that the made superhydrophobic fabric tool of the present invention has good wearability.
The present invention has the advantage that compared with the existing technology
1, the preparation method and simple process of superhydrophobic fabric finishing agent, reaction condition temperature is at low cost, is convenient for large-scale production;
2, the application method of superhydrophobic fabric finishing agent is simple, can be used for constructing for a variety of superhydrophobic fabrics, be not required to fabric into Row pretreatment, greatlies simplify preparation process, and maintain the property such as the intrinsic mechanical strength of fabric, flexibility, gloss and feel Energy;
3, the made superhydrophobic fabric of the present invention has excellent super-hydrophobicity and good mechanical stability.
Detailed description of the invention
Fig. 1 is the schematic device (a) and specimen holder (b) for measuring water rolling angle.
Fig. 2 is photo of the water droplet on superhydrophobic fabric.
Fig. 3 is the wear test schematic diagram for evaluating sample mechanical stability.
Specific embodiment
Make furtherly below by preparation and application of the specific embodiment to superhydrophobic fabric finishing agent of the present invention It is bright.
Embodiment 1
(1) preparation of superhydrophobic fabric finishing agent: take 0.6mL phenyl triethoxysilane, 0.2mL tetraethoxysilane and 0.1mL 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane, is added in 50mL ethanol-water solution (ethanol/water=7:1v/ V), magnetic agitation 10min obtains uniform solution;0.2mL ammonium hydroxide and 1mL polyphenylene silicone resin are added, is reacted at 50 DEG C 24h;It is cooled to room temperature, with 1M salt acid for adjusting pH to neutrality, obtains superhydrophobic fabric finishing agent.
(2) preparation of superhydrophobic fabric: measuring 10mL fabric finishing agent, dilutes 5 times, magnetic agitation 5min with ethyl alcohol, surpasses Sound disperses 5min.Then 10cm × 10cm polyester textile is immersed, 0.3% acetic acid is added, is standing and soaking 5min, then will knit Object handles 8min at 120 DEG C, and superhydrophobic fabric can be obtained.
Super-hydrophobicity and estimation of stability: rolling angle < 10 ° are carried out to superhydrophobic fabric;After washing 20 times, rolling angle is still low In 15 °, water droplet is easily tumbled from surface;Under 10KPa load after reciprocating friction 200 times, rolling angle is still below 15 °, water droplet Yi Congbiao Face tumbles, and has excellent super-hydrophobicity and mechanical stability.
Embodiment 2
(1) preparation of superhydrophobic fabric finishing agent: take 8mL hexadecyl, 2mL ethyl triethoxysilane and 5mL 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane, is added to (ethyl alcohol/different in 400mL ethyl alcohol/isopropanol-water solutions Propanol/water=6:3:1v/v/v), magnetic agitation 5min obtains uniform solution;Add 2mL ethylenediamine, 8mL poly dimethyl two Methoxyl group silicone resin and the poly- methyl vinyl silicone of 2mL, in 25 DEG C of reaction 36h;With 1M salt acid for adjusting pH to neutrality, obtain Superhydrophobic fabric finishing agent.
(2) preparation of superhydrophobic fabric: 100mL fabric finishing agent is measured, is diluted to 8 times of its volume with ethyl alcohol, magnetic force Stir 5min, ultrasonic disperse 5min.Then 50cm × 50cm cotton fabric is immersed, 0.1% acetic acid is added, is standing and soaking 3min, then fabric is handled into 3min at 160 DEG C, superhydrophobic fabric can be obtained.
Super-hydrophobicity and estimation of stability: rolling angle < 10 ° are carried out to superhydrophobic fabric;After washing 20 times, rolling angle is still low In 15 °, water droplet is easily tumbled from surface;Under 10KPa load after reciprocating friction 200 times, rolling angle is still below 15 °, water droplet Yi Congbiao Face tumbles, and has excellent super-hydrophobicity and mechanical stability.
Embodiment 3
(1) preparation of superhydrophobic fabric finishing agent: by 20mL methyltriethoxysilane, 5 potassium methyl silicates and 12mL aminopropyl Trimethoxy silane is added in 1L ethyl alcohol/Glycol Mixture (ethyl alcohol/glycol/water=2:2:1v/v/v), mechanical stirring 5min obtains uniform solution;10mL 1M sodium hydrate aqueous solution and 8mL poly dimethyl dimethoxy silicone resin are added, 40 DEG C of reaction 12h;With 1M salt acid for adjusting pH to neutrality, superhydrophobic fabric finishing agent is obtained.
(2) preparation of superhydrophobic fabric: 500mL fabric finishing agent is measured, with ethanol/water solution (ethanol/water=1:1v/v) 10 times, mechanical stirring 5min, ultrasonic disperse 5min of dilution.Then the wool of 50cm × 50cm, silk are immersed, are added 0.1% acetic acid is standing and soaking 4min, then fabric is handled 4min at 80 DEG C, and superhydrophobic fabric can be obtained.
Super-hydrophobicity and estimation of stability: rolling angle < 10 ° are carried out to superhydrophobic fabric;After washing 20 times, rolling angle is still low In 15 °, water droplet is easily tumbled from surface;Under 10KPa load after reciprocating friction 200 times, rolling angle is still below 15 °, water droplet Yi Congbiao Face tumbles, and has excellent super-hydrophobicity and mechanical stability.
Embodiment 4
(1) preparation of superhydrophobic fabric finishing agent: by 1mL vinyltriethoxysilane and 1mL dodecyl triethoxysilicane Alkane is added in 100mL ethyl alcohol/Glycerine-Aqueous Solution (ethyl alcohol/glycerin/water=6.9:0.1:1), and magnetic agitation 5min obtains uniform Solution;0.4mL triethylamine and the poly- methyl vinyl silicone of 3mL and 1mL polyphenylene silicone resin are added, is reacted at 70 DEG C 4h;With 1M salt acid for adjusting pH to neutrality, superhydrophobic fabric finishing agent is obtained.
(2) preparation of superhydrophobic fabric: measuring 80mL fabric finishing agent, dilutes 6 times, magnetic agitation 5min with ethyl alcohol, surpasses Sound disperses 5min.Then 20cm × 20cm polyester/cotton blended cloth (20% cotton), acrylic fabric are immersed, 0.6% vinegar is added Acid is standing and soaking 6min, then fabric is handled 5min at 120 DEG C, and superhydrophobic fabric can be obtained.
Super-hydrophobicity and estimation of stability: rolling angle < 10 ° are carried out to superhydrophobic fabric;After washing 20 times, rolling angle is still low In 15 °, water droplet is easily tumbled from surface;Under 10KPa load after reciprocating friction 200 times, rolling angle is still below 15 °, water droplet Yi Congbiao Face tumbles, and has excellent super-hydrophobicity and mechanical stability.
Embodiment 5
(1) preparation of superhydrophobic fabric finishing agent: by 1mL potassium methyl silicate, 4mL octadecyltriethoxy silane and 1mL ammonia Propyl trimethoxy silicane is added in 5L ethyl alcohol/Glycol Mixture (ethanol/water=2:1:1), and magnetic agitation 5min is obtained Uniform solution;10mL ammonium hydroxide and 80mL polydimethyl siloxanes and the poly- methyl vinyl silicone of 120mL are added, at 40 DEG C React 8h;With 1M salt acid for adjusting pH to neutrality, superhydrophobic fabric finishing agent is obtained.
(2) preparation of superhydrophobic fabric: measuring 1L fabric finishing agent, dilutes 10 times, mechanical stirring 5min with ethyl alcohol, ultrasound Disperse 5min.Then 100cm × 100cm cotton fabric is immersed, 0.2% acetic acid is added, is standing and soaking 3min, then by fabric 4min is handled at 120 DEG C, superhydrophobic fabric can be obtained.Super-hydrophobicity and estimation of stability are carried out to it.
Super-hydrophobicity and estimation of stability: rolling angle < 10 ° are carried out to superhydrophobic fabric;After washing 20 times, rolling angle is still low In 15 °, water droplet is easily tumbled from surface;Under 10KPa load after reciprocating friction 200 times, rolling angle is still below 15 °, water droplet Yi Congbiao Face tumbles, and has excellent super-hydrophobicity and mechanical stability.

Claims (8)

1. a kind of preparation method of organosilicon polymer superhydrophobic fabric finishing agent, is that organosilicon and organosilan are added to alkali In property alcohol-water solution, 2 ~ 48h of hydrolytic condensation at 25 ~ 80 DEG C;It is cooled to room temperature, adjusts pH to neutrality, obtain super-hydrophobic knit Object finishing agent.
2. the preparation method of organosilicon polymer superhydrophobic fabric finishing agent as described in claim 1, it is characterised in that: described to have Machine silicon is poly dimethyl dimethoxysilane, in polyphenylene silicone resin, polydimethyl siloxanes, poly- methyl vinyl silicone It is at least one;And volume fraction of the organosilicon in alcohol-water solution is 0.5% ~ 5%.
3. the preparation method of organosilicon polymer superhydrophobic fabric finishing agent as described in claim 1, it is characterised in that: described to have Machine silane is tetraethoxysilane, sodium methyl silicate, potassium methyl silicate, waterglass, aminopropyl trimethoxysilane, 3- (2,3- The third oxygen of epoxy) propyl trimethoxy silicane, methyltriethoxysilane, ethyl triethoxysilane, vinyl triethoxyl silicon Alkane, phenyl triethoxysilane, octyltri-ethoxysilane, dodecyl triethoxysilane, cetyl triethoxysilicane At least one of alkane, octadecyltriethoxy silane and corresponding methoxy silane;And organosilan is water-soluble in alkaline alcohol- Volume fraction in liquid is 1% ~ 4%.
4. the preparation method of organosilicon polymer superhydrophobic fabric finishing agent as described in claim 1, it is characterised in that: the alkali Property alcohol-water solution in, alcohol is at least one of methanol, ethyl alcohol, isopropanol, ethylene glycol, glycerol, and the volume ratio of alcohol and water is 9: 1~1:1。
5. the preparation method of organosilicon polymer superhydrophobic fabric finishing agent as described in claim 1, it is characterised in that: the alkali Property alcohol-water solution in, alkali be at least one of ammonium hydroxide, sodium hydroxide, potassium hydroxide, ethylenediamine, triethylamine, alkali is in alcohol-water The mass concentration of solution is 0.2% ~ 2%.
6. the organosilicon polymer superhydrophobic fabric finishing agent of method preparation as described in claim 1 is used to prepare super-hydrophobic knit Object, it is characterised in that: superhydrophobic fabric finishing agent ethyl alcohol or/and water are diluted 5 ~ 10 times, superhydrophobic fabric finishing agent is added The acetic acid of volume 0.1% ~ 1% is as catalyst;By fabric be dipped in wherein standing 2 ~ 10min, then 80 ~ 180 DEG C solidify 2 ~ 10min to get arrive superhydrophobic fabric.
7. organosilicon polymer superhydrophobic fabric finishing agent as claimed in claim 6 is used to prepare superhydrophobic fabric, feature exists In: after superhydrophobic fabric finishing agent is diluted with ethyl alcohol, 3 ~ 5min of re-ultrasonic dispersion.
8. organosilicon polymer superhydrophobic fabric finishing agent as claimed in claim 6 is used to prepare superhydrophobic fabric, feature exists In: the fabric is polyester, cotton, wool, silk, acrylic fibers, nylon, polyurethane and its blended fabric.
CN201811347432.4A 2018-11-13 2018-11-13 A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent Pending CN109518468A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811347432.4A CN109518468A (en) 2018-11-13 2018-11-13 A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811347432.4A CN109518468A (en) 2018-11-13 2018-11-13 A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent

Publications (1)

Publication Number Publication Date
CN109518468A true CN109518468A (en) 2019-03-26

Family

ID=65776585

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811347432.4A Pending CN109518468A (en) 2018-11-13 2018-11-13 A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent

Country Status (1)

Country Link
CN (1) CN109518468A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111116920A (en) * 2019-12-26 2020-05-08 福建省晋江新德美化工有限公司 Branched polyamino long-chain alkyl polysiloxane, waterproof soft organic silicon finishing agent and preparation method thereof
CN111494987A (en) * 2020-04-27 2020-08-07 广州大学 Fluorine-free super-hydrophobic fabric and preparation method thereof
CN111501352A (en) * 2020-04-24 2020-08-07 山东鑫纳超疏新材料有限公司 Preparation method of water-based fluorine-free stable super-hydrophobic fabric
CN111576036A (en) * 2020-05-20 2020-08-25 浙江海明实业有限公司 Nano antifouling, antibacterial and breathable environment-friendly fabric and preparation process thereof
CN113249972A (en) * 2021-06-11 2021-08-13 中国科学院兰州化学物理研究所 Preparation method of high-pressure-resistance easy-to-clean super-hydrophobic fabric
WO2022223934A1 (en) * 2021-04-22 2022-10-27 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for coating textile materials
IT202100017357A1 (en) * 2021-07-01 2023-01-01 Univ Degli Studi Di Bergamo SOL-GEL COMPOSITION FOR THE WATER-REPELLENT FINISHING OF FABRICS AND RELATIVE PREPARATION PROCEDURE

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000014299A1 (en) * 1998-09-07 2000-03-16 The Procter & Gamble Company Raw materials or blanks having super hydrophobic coating
CN102978954A (en) * 2012-12-21 2013-03-20 中国科学院兰州化学物理研究所 Method for preparing good-stability super-hydrophobic fabrics
CN104294608A (en) * 2014-09-29 2015-01-21 大连工业大学 Method for preparing hydrophobic material on basis of polymethylhydrosiloxane
CN104789124A (en) * 2014-12-30 2015-07-22 中国科学院兰州化学物理研究所 A preparing method of a stable superamphiphobic surface
CN105544187A (en) * 2016-02-04 2016-05-04 苏州蓝锐纳米科技有限公司 Super-hydrophobic fabric and preparation method thereof
CN106592222A (en) * 2016-12-29 2017-04-26 东华大学 Fluoride-free water-repellent textile fabric finishing method based on ultraviolet light curing reaction
CN108003753A (en) * 2017-12-25 2018-05-08 山东国舜建设集团有限公司 A kind of super-hydrophobic long lasting anticorrosion coating of automatically cleaning and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000014299A1 (en) * 1998-09-07 2000-03-16 The Procter & Gamble Company Raw materials or blanks having super hydrophobic coating
CN102978954A (en) * 2012-12-21 2013-03-20 中国科学院兰州化学物理研究所 Method for preparing good-stability super-hydrophobic fabrics
CN104294608A (en) * 2014-09-29 2015-01-21 大连工业大学 Method for preparing hydrophobic material on basis of polymethylhydrosiloxane
CN104789124A (en) * 2014-12-30 2015-07-22 中国科学院兰州化学物理研究所 A preparing method of a stable superamphiphobic surface
CN105544187A (en) * 2016-02-04 2016-05-04 苏州蓝锐纳米科技有限公司 Super-hydrophobic fabric and preparation method thereof
CN106592222A (en) * 2016-12-29 2017-04-26 东华大学 Fluoride-free water-repellent textile fabric finishing method based on ultraviolet light curing reaction
CN108003753A (en) * 2017-12-25 2018-05-08 山东国舜建设集团有限公司 A kind of super-hydrophobic long lasting anticorrosion coating of automatically cleaning and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
叶文波 等: "超疏水聚硅氧烷涂层的制备及其性能", 《应用化学》 *
朱万强等: "《涂料基础教程》", 30 June 2012 *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111116920A (en) * 2019-12-26 2020-05-08 福建省晋江新德美化工有限公司 Branched polyamino long-chain alkyl polysiloxane, waterproof soft organic silicon finishing agent and preparation method thereof
CN111116920B (en) * 2019-12-26 2022-06-21 福建省晋江新德美化工有限公司 Branched polyamino long-chain alkyl polysiloxane, waterproof soft organic silicon finishing agent and preparation method thereof
CN111501352A (en) * 2020-04-24 2020-08-07 山东鑫纳超疏新材料有限公司 Preparation method of water-based fluorine-free stable super-hydrophobic fabric
CN111501352B (en) * 2020-04-24 2022-05-17 山东鑫纳超疏新材料有限公司 Preparation method of water-based fluorine-free stable super-hydrophobic fabric
CN111494987A (en) * 2020-04-27 2020-08-07 广州大学 Fluorine-free super-hydrophobic fabric and preparation method thereof
CN111494987B (en) * 2020-04-27 2022-01-11 广州大学 Fluorine-free super-hydrophobic fabric and preparation method thereof
CN111576036A (en) * 2020-05-20 2020-08-25 浙江海明实业有限公司 Nano antifouling, antibacterial and breathable environment-friendly fabric and preparation process thereof
WO2022223934A1 (en) * 2021-04-22 2022-10-27 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for coating textile materials
FR3122190A1 (en) * 2021-04-22 2022-10-28 Commissariat A L'energie Atomique Et Aux Energies Alternatives Process for coating textile materials
CN113249972A (en) * 2021-06-11 2021-08-13 中国科学院兰州化学物理研究所 Preparation method of high-pressure-resistance easy-to-clean super-hydrophobic fabric
CN113249972B (en) * 2021-06-11 2022-02-01 中国科学院兰州化学物理研究所 Preparation method of high-pressure-resistance easy-to-clean super-hydrophobic fabric
IT202100017357A1 (en) * 2021-07-01 2023-01-01 Univ Degli Studi Di Bergamo SOL-GEL COMPOSITION FOR THE WATER-REPELLENT FINISHING OF FABRICS AND RELATIVE PREPARATION PROCEDURE

Similar Documents

Publication Publication Date Title
CN109518468A (en) A kind of preparation and application of organosilicon polymer superhydrophobic fabric finishing agent
Gao et al. Rational construction of highly transparent superhydrophobic coatings based on a non-particle, fluorine-free and water-rich system for versatile oil-water separation
CN102978954B (en) Method for preparing good-stability super-hydrophobic fabrics
CN110714325B (en) Nano silicon dioxide-fluorine-free super-hydrophobic finishing agent and preparation method and application thereof
Guo et al. Fabrication of superhydrophobic cotton fabric with multiple durability and wearing comfort via an environmentally friendly spraying method
CN104562709B (en) A kind of preparation method of durable superhydrophobic fabric
Gao et al. Preparation and characterization of superhydrophobic organic-inorganic hybrid cotton fabrics via γ-radiation-induced graft polymerization
US20080090004A1 (en) Hydrophobic and Lyophobic Coating
CN104594028A (en) Method for preparing durable cellulose fiber fabric with super-hydrophobic surface
CN106592222A (en) Fluoride-free water-repellent textile fabric finishing method based on ultraviolet light curing reaction
CN106637959A (en) Ultraviolet curing reaction-based fluoride-free and water-repellent finishing method of cotton fabric
CN107201648B (en) Preparation method of self-cleaning fabric
WO2009061364A2 (en) Textiles treated with copolymers of epoxy compounds and amino silanes having enhanced wet-strength
CN109930386A (en) A kind of preparation method of the washable superhydrophobic fabric of pressure resistance
EP2215303A2 (en) Textiles treated with copolymers of epoxy compounds and amino silanes having enhanced wet-strength
CN111472171A (en) Super-hydrophobic fabric and preparation method thereof
CN109837758A (en) A kind of preparation method of fabric super hydrophobic surface
CN110512428B (en) Durable fluoride-free super-hydrophobic fabric finishing liquid and method for finishing fabric by using same
Xie et al. Facile fabrication of superhydrophobic polyester fabric based on rapid oxidation polymerization of dopamine for oil–water separation
CN107059406A (en) The preparation method of super-hydrophobic terylene
Altangerel et al. Superhydrophobic modification and characterization of cashmere fiber surfaces by wet coating techniques of silica nanoparticles
Luo et al. Superhydrophobic and oleophobic textiles with hierarchical micro-nano structure constructed by sol–gel method
CN106633049A (en) Vat dye ozone-proof fastness improver as well as preparation method and application thereof
Kong et al. Functionalization of PET fabric via silicone based organic–inorganic hybrid coating
Yan et al. Engineering polydimethylsiloxane with two-dimensional graphene oxide for an extremely durable superhydrophobic fabric coating

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20190327

Address after: 265400 No. 6 Dongsheng Road, Zhaoyuan City, Yantai City, Shandong Province

Applicant after: Shandong Xinna Chaoshu New Materials Co., Ltd.

Applicant after: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences

Address before: 201600 Shanghai Songjiang District, Shihui Road 259, Zhongshan Street, 2nd Floor 201

Applicant before: Shubo (Shanghai) Nanotechnology Co., Ltd.

Applicant before: Shandong Xinna Chaoshu New Materials Co., Ltd.

SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190326