CN109322165B - A kind of preparation method and application of Waterproof Breathable type cotton fabric coating - Google Patents

A kind of preparation method and application of Waterproof Breathable type cotton fabric coating Download PDF

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Publication number
CN109322165B
CN109322165B CN201811385862.5A CN201811385862A CN109322165B CN 109322165 B CN109322165 B CN 109322165B CN 201811385862 A CN201811385862 A CN 201811385862A CN 109322165 B CN109322165 B CN 109322165B
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preparation
waterproof breathable
cotton fabric
coating
fiber element
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CN109322165A (en
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张平
邓健
彭雄义
彭帅
梁永红
殷国益
粟斯伟
蔡映杰
王强
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Hubei Longchuan Tiao Garment Co.,Ltd.
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Wuhan Textile University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/04Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06N3/042Acrylic polymers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0061Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0068Polymeric granules, particles or powder, e.g. core-shell particles, microcapsules
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/007Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
    • D06N3/0077Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2205/00Condition, form or state of the materials
    • D06N2205/08Microballoons, microcapsules
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2209/00Properties of the materials
    • D06N2209/12Permeability or impermeability properties
    • D06N2209/126Permeability to liquids, absorption
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2209/00Properties of the materials
    • D06N2209/14Properties of the materials having chemical properties
    • D06N2209/142Hydrophobic

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

Abstract

The present invention relates to the preparation methods and application of a kind of Waterproof Breathable type cotton fabric coating, it is characterized in that first preparing hollow porous fiber element microballoon;Then the monomers such as acrylic acid, allyl glycidyl ether, butyl acrylate are polymerize and is emulsified, polyacrylate emulsion is made;Hollow porous fiber element microballoon/polyacrylate multiple emulsion finally is obtained by hollow porous fiber element microballoon and polyacrylate emulsion are compound, this lotion is Waterproof Breathable type cotton fabric coating;The coating agent carries out top finish to cotton fabric, and Waterproof Breathable type coated cotton fibers are made.The resistance to hydrostatic pressure of Waterproof Breathable type coated cotton fibers prepared by the present invention reaches 6400~7250Pa, and vapor transfer rate reaches 250~270g/ (m2For 24 hours), hence it is evident that higher than the coated cotton fibers of buying;After 10 washings, indices are not decreased obviously coated cotton fibers, illustrate that the stability of coated cotton fibers and durability are fine.

Description

A kind of preparation method and application of Waterproof Breathable type cotton fabric coating
Technical field
The invention belongs to fabric coating technical fields, and in particular to a kind of preparation side of Waterproof Breathable type cotton fabric coating Method and application.
Background technique
Waterproof moisture permeating fabric is also known as " fabric that can be breathed ", refers to that water does not penetrate into fabric under a certain pressure, and human body The sweat gas distributed can be spread by fabric is transmitted to the external world, will not make one to feel hair in skin and check room accumulation or condensation Bored functional fabric.Waterproofness refers to the impedance behavior generated when fabric penetrates the external water with certain pressure;Moisture-inhibiting The performance of the absorption in the fabric of property, that is, sweat, transmitting, diffusion.
Currently, coated fabric has lot of advantages, coating can assign fabric different functions, such as: waterproof, fire-retardant, anti- Electrostatic and Waterproof Breathable etc., coated fabric generally use coating agent and fabric progress top finish are made.The type of coating agent is numerous It is more, wherein polyacrylate coating agent and urethane type coatings agent are current widely used fabric coating finishing agents.Poly- third Olefin(e) acid esters lotion has the soft fabric being processed into, glue film transparency height, weatherability as a kind of water-proof moisture-permeation coating agent The performances such as good, the good anti-suede of water resistant, but since waterproof and moisture permeability is relatively low, the poor disadvantage of comfort makes its application It is limited.A variety of modifications are carried out for polyacrylate dispersion defect, such as: epoxy resin or polyurethane-modified acrylic acid lotion; It is cross-linking modified;Inorganic nano material modified etc., these, which are modified, has certain effect for different types of fabric, however, with In the coating agent of waterproof and moisture permeability of cotton fabric, there is not been reported.
The modified research of the waterproofing and moisture-penetration performances of fabric is more, such as: Chinese Patent Application No. 200310120808.5 is announced Waterproof, cold-proof, moisture-inhibiting polyurethane coating cloth and its production technology, it is main that the coating agent of the patent report, which is with polyurethane, Raw material is made.Chinese Patent Application No. 200710145401.6 discloses a kind of water-proof moisture-permeation coating agent composition and its application, The patent adds micropore lignin fine powder in polyurethane coating agent.Existing technology is much obtained simply to compound Coating agent, for the coated fabric that needs are washed, the effective component of these coating agents is inevitably lost in water-washing process.Coating cotton Fabric is widely used in textile, occupies higher proportion, but due to its in terms of Waterproof Breathable not all roses, Waterproof Breathable There are also biggish rooms for promotion for modified aspect.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, a kind of preparation of Waterproof Breathable type cotton fabric coating is provided Method and application.The present invention is prepared for a kind of hollow porous fiber element microballoon/polyacrylate multiple emulsion, which is used for After the top finish of cotton fabric, the waterproofing and moisture-penetration performances of coated cotton fibers are significantly improved, and waterproof performance is mainly by cotton fabric table The polyacrylate coatings film in face generates, and water vapour permeability mainly provides channel by the emptying aperture diameter inside cellulose microsphere.
A kind of preparation method of Waterproof Breathable type cotton fabric coating of the present invention, which is characterized in that the method It comprises the following steps:
(1) preparation of oil-in-water emulsion: being swollen 2~4h for cellulose in glacial acetic acid, be then dissolved in acetic anhydride and In the mixed solution of acetic acid, sulfuric acid is added dropwise into system, wherein the volume ratio of acetic anhydride and acetic acid is 1: 1~1.5, sulfuric acid Dosage is the 1.0~1.5% of acetic anhydride and acetic acid total volume, and 2~5h is reacted at 55 DEG C and uses sodium hydroxide after reaction Sulfuric acid in neutralization system is 7~8 to pH, then pours into above-mentioned reactant and is settled out cellulose acetate in distilled water, finally By the multiple centrifugal elutriation of gained cellulose acetate to neutrality, then it is dried in vacuo;Resulting dry cellulose acetate is dissolved in dichloro Methane obtains the solution of clear, sorbester p17 is added in Xiang Shangshu solution, is uniformly mixed, wherein cellulose acetate, The weight ratio of sorbester p17 is 1: 0.1~0.15, and above-mentioned mixed liquor is added in the aqueous solution of dodecyl sodium sulfate, is constantly stirred Mix, obtain oil-in-water emulsion, wherein methylene chloride, sodium dodecyl sulfate aqueous solution volume ratio be 1: 5~7;Dodecyl The mass fraction of sulfonic acid sodium water solution is 0.75~1.0%;
(2) preparation of hollow porous fiber element microballoon: the methylene chloride in control condition slow evaporation oil-in-water emulsion steams 4~6h is sent out, is centrifuged evaporation residue to obtain cellulose microsphere, the cellulose microsphere obtained by distilled water flushing is to remove Dodecyl sodium sulfate therein is removed, is then cleaned multiple times with ethyl alcohol again to remove sorbester p17, is finally dried in vacuo, obtained pure Hollow porous fiber element microballoon, hollow porous fiber element microballoon is as shown in Figure 1;
(3) suitable neopelex, sim alkylphenol polyoxyethylene the preparation of polyacrylate emulsion: are weighed Ether emulsifier, acrylic acid, allyl glycidyl ether, butyl acrylate and ammonium persulfate etc., wherein neopelex (g), Polyethylene Octylphenol Ether emulsifier (g), acrylic acid (mol), allyl glycidyl ether (mol), butyl acrylate (mol) and the mass volume ratio of ammonium persulfate (g) are as follows: 0.5~1: 1~2: 0.1~0.2: 0.1~0.2: 0.1~0.2: 0.5~ 1;By whole neopelexes, Polyethylene Octylphenol Ether emulsifier and account for the acrylic acid of total amount 1/3, allyl Glycidol ether, butyl acrylate and ammonium persulfate initiator are dissolved in suitable deionized water, uniform stirring, control temperature It is 75~85 DEG C, stirs 1~2h;Then by acrylic acid, allyl glycidyl ether, butyl acrylate and the over cure of residue 2/3 Sour ammonium initiator is added drop-wise in the mixed solution just stirred after being dissolved in appropriate amount of deionized water, and time for adding control is in 2~3h, drop After adding, 2~3h is kept the temperature, polyacrylate emulsion coating agent is obtained, this lotion places January, and lamination does not occur ;
(4) mixing of lotion: the lotion of the hollow porous fiber element microballoon of step (2) preparation and step (3) preparation is mixed It closes, wherein the mass volume ratio of the lotion (mL) of the hollow porous fiber element microballoon (g) and step (3) preparation of step (2) preparation For 1 ︰ 10~20, mixed solution is stirred into 1~2h on high speed dispersion homogenizer, whipping temp is 50~60 DEG C Hollow porous fiber element microballoon/polyacrylate multiple emulsion is obtained, this lotion is Waterproof Breathable type cotton fabric coating;
Another object of the present invention is to provide a kind of application of Waterproof Breathable type cotton fabric coating obtained above, tools Body scheme are as follows: it is on taut frame that cotton fabric is tight, coating agent scraper is uniformly applied and is scraped on cotton fabric, coating weight dry weight is 20 ~25g/m2, dry 2 minutes, baked in 140~170 DEG C 3 minutes in 90 DEG C.
The present invention has following distinguishing feature:
(1) present invention is prepared for a kind of hollow porous fiber element microballoon, and internal hollow aperture can be sweat to outlet Except offer channel;The present invention is successfully prepared for stable hollow porous fiber element microballoon/polyacrylate multiple emulsion, this Lotion places January, and lamination does not occur.Preparation method of the invention is simple, no pollution to the environment, has very strong market Promotion prospect.
(2) the film forming gloss of coating agent prepared by the present invention is in less scalelike mark or the coating without scalelike mark, with buying Agent is close;Its tensile strength is slightly below the coating agent purchased;Its elongation at break is higher than the coating agent of buying;Glue film water absorption rate ratio The coating agent of buying is slightly lower, it is thus regarded that, the performance indicator of the coating agent of coating agent prepared by the present invention and buying is close.
(3) after coating agent top finish prepared by the present invention, the resistance to hydrostatic pressure of coated cotton fibers reaches cotton fabric 6400~7250Pa, hence it is evident that higher than the coated fabric of buying;Its surface moisture resistance illustrates its tool also superior to the coated fabric of buying There is very strong water-proof function;Its vapor transfer rate reaches 250~270g/ (m2For 24 hours), hence it is evident that higher than the coated fabric of buying, explanation It has the function of very strong moisture-inhibiting.Coated cotton fibers are after 10 washings, and indices are not decreased obviously, especially hand Sense is not also hardened, and illustrates that the stability of coated fabric and durability are fine.
Detailed description of the invention
Fig. 1 hollow porous fiber element microballoon schematic diagram
Specific embodiment
The present invention is described in detail in embodiment described below.
Embodiment 1
In the present embodiment, a kind of Waterproof Breathable type cotton fabric coating is prepared with the following method, including as follows Step:
(1) preparation of oil-in-water emulsion: 5g cellulose is swollen 2h in glacial acetic acid, is then dissolved in 30mL acetic anhydride In the mixed solution of 30mL acetic acid, sulfuric acid is added dropwise into system, wherein the dosage of sulfuric acid is acetic anhydride and acetic acid total volume 1.0%, 2h is reacted at 55 DEG C, is 7.6 with the sulfuric acid in sodium hydroxide and in system to pH after reaction, it then will be upper It states reactant and pours into and be settled out cellulose acetate in distilled water, finally by the multiple centrifugal elutriation of gained cellulose acetate to neutrality, It is dried in vacuo again;The dry cellulose acetate of resulting 5g is dissolved in 50mL methylene chloride, obtains the solution of clear, Xiang Shangshu 0.5g sorbester p17 is added in solution, is uniformly mixed, above-mentioned mixed liquor is added to the 250mL ten that mass fraction is 0.75% It in dialkyl sulfonates aqueous solution, is stirred continuously, obtains oil-in-water emulsion;
(2) preparation of hollow porous fiber element microballoon: the methylene chloride in control condition slow evaporation oil-in-water emulsion steams 4~6h is sent out, is centrifuged evaporation residue to obtain cellulose microsphere, the cellulose microsphere obtained by distilled water flushing is to remove Dodecyl sodium sulfate therein is removed, is then cleaned multiple times with ethyl alcohol again to remove sorbester p17, is finally dried in vacuo, obtained pure Hollow porous fiber element microballoon;
(3) neopelex 0.5g, Polyethylene Octylphenol Ether the preparation of polyacrylate emulsion: are weighed Emulsifier 1g, acrylic acid 0.1mol, allyl glycidyl ether 0.1mol, butyl acrylate 0.1mol and ammonium persulfate 0.5g; By whole neopelexes, Polyethylene Octylphenol Ether emulsifier and account for the acrylic acid of total amount 1/3, dimethyl two Allyl ammonium chloride, butyl acrylate and ammonium persulfate initiator are dissolved in the deionized water of 200mL, uniform stirring, control Temperature is 75 DEG C, stirs 1h;Then by acrylic acid, allyl glycidyl ether, butyl acrylate and the ammonium persulfate of residue 2/3 Initiator monomer and ammonium persulfate initiator are dissolved in 20mL deionized water, are added dropwise in the mixed solution just stirred, drip Control is in 2h between added-time, after being added dropwise, keeps the temperature 2.5h, obtains multiple emulsion, this lotion places January, and it is existing that layering does not occur As can be prepared by polyacrylate emulsion coating agent;
(4) mixing of lotion: the lotion of the hollow porous fiber element microballoon of step (2) preparation and step (3) preparation is mixed It closing, wherein the mass volume ratio of the lotion of the hollow porous fiber element microballoon and step (3) preparation of step (2) preparation is 1 ︰ 10, Mixed solution is stirred into 1h on high speed dispersion homogenizer, whipping temp is 50 DEG C, and hollow porous fiber element can be obtained Microballoon/polyacrylate multiple emulsion, this lotion are Waterproof Breathable type cotton fabric coating a;
Another object of the present invention is to provide the application of Waterproof Breathable type cotton fabric coating a obtained above a kind of, The specific scheme is that on taut frame that cotton fabric is tight, coating agent scraper is uniformly applied and is scraped on cotton fabric, coating weight dry weight is 20g/m2, dry 2 minutes, baked in 150 DEG C 3 minutes in 90 DEG C.
Embodiment 2
In the present embodiment, a kind of Waterproof Breathable type cotton fabric coating is prepared with the following method, including as follows Step:
(1) preparation of oil-in-water emulsion: 5g cellulose is swollen 3h in glacial acetic acid, is then dissolved in 40mL acetic anhydride In the mixed solution of 45mL acetic acid, sulfuric acid is added dropwise into system, wherein the dosage of sulfuric acid is acetic anhydride and acetic acid total volume 1.2%, 2h is reacted at 55 DEG C, is 7.6 with the sulfuric acid in sodium hydroxide and in system to pH after reaction, it then will be upper It states reactant and pours into and be settled out cellulose acetate in distilled water, finally by the multiple centrifugal elutriation of gained cellulose acetate to neutrality, It is dried in vacuo again;The dry cellulose acetate of resulting 5g is dissolved in 50mL methylene chloride, obtains the solution of clear, Xiang Shangshu 0.6g sorbester p17 is added in solution, is uniformly mixed, above-mentioned mixed liquor is added to the 250mL ten that mass fraction is 0.85% It in dialkyl sulfonates aqueous solution, is stirred continuously, obtains oil-in-water emulsion;
(2) preparation of hollow porous fiber element microballoon: the methylene chloride in control condition slow evaporation oil-in-water emulsion steams 4~6h is sent out, is centrifuged evaporation residue to obtain cellulose microsphere, the cellulose microsphere obtained by distilled water flushing is to remove Dodecyl sodium sulfate therein is removed, is then cleaned multiple times with ethyl alcohol again to remove sorbester p17, is finally dried in vacuo, obtained pure Hollow porous fiber element microballoon;
(3) neopelex 0.6g, Polyethylene Octylphenol Ether the preparation of polyacrylate emulsion: are weighed Emulsifier 1.2g, acrylic acid 0.12mol, allyl glycidyl ether 0.12mol, butyl acrylate 0.12mol and ammonium persulfate 0.6g;By whole neopelexes, Polyethylene Octylphenol Ether emulsifier and account for the acrylic acid of total amount 1/3, two Methyl diallyl ammonium chloride, butyl acrylate and ammonium persulfate initiator are dissolved in the deionized water of 200mL, are uniformly stirred It mixes, controlled at 75 DEG C, stirs 1h;Then by residue 2/3 acrylic acid, allyl glycidyl ether, butyl acrylate and Ammonium persulfate initiator monomer and ammonium persulfate initiator are dissolved in 20mL deionized water, and it is molten to be added dropwise to the mixing just stirred In liquid, time for adding is controlled in 2h, after being added dropwise, is kept the temperature 2.5h, is obtained multiple emulsion, this lotion places January, does not send out Raw lamination can be prepared by polyacrylate emulsion coating agent;
(4) mixing of lotion: the lotion of the hollow porous fiber element microballoon of step (2) preparation and step (3) preparation is mixed It closing, wherein the mass volume ratio of the lotion of the hollow porous fiber element microballoon and step (3) preparation of step (2) preparation is 1 ︰ 15, Mixed solution is stirred into 1h on high speed dispersion homogenizer, whipping temp is 50 DEG C, and hollow porous fiber element can be obtained Microballoon/polyacrylate multiple emulsion, this lotion are Waterproof Breathable type cotton fabric coating b;
Another object of the present invention is to provide the application of Waterproof Breathable type cotton fabric coating b obtained above a kind of, The specific scheme is that on taut frame that cotton fabric is tight, coating agent scraper is uniformly applied and is scraped on cotton fabric, coating weight dry weight is 23g/m2, dry 2 minutes, baked in 160 DEG C 3 minutes in 90 DEG C.
Embodiment 3
In the present embodiment, a kind of Waterproof Breathable type cotton fabric coating is prepared with the following method, including as follows Step:
(1) preparation of oil-in-water emulsion: 5g cellulose is swollen 4h in glacial acetic acid, is then dissolved in 30mL acetic anhydride In the mixed solution of 30mL acetic acid, sulfuric acid is added dropwise into system, wherein the dosage of sulfuric acid is acetic anhydride and acetic acid total volume 1.5%, 2h is reacted at 55 DEG C, is 7.6 with the sulfuric acid in sodium hydroxide and in system to pH after reaction, it then will be upper It states reactant and pours into and be settled out cellulose acetate in distilled water, finally by the multiple centrifugal elutriation of gained cellulose acetate to neutrality, It is dried in vacuo again;The dry cellulose acetate of resulting 5g is dissolved in 50mL methylene chloride, obtains the solution of clear, Xiang Shangshu 0.7g sorbester p17 is added in solution, is uniformly mixed, above-mentioned mixed liquor is added to the 250mL ten that mass fraction is 1.0% It in dialkyl sulfonates aqueous solution, is stirred continuously, obtains oil-in-water emulsion;
(2) preparation of hollow porous fiber element microballoon: the methylene chloride in control condition slow evaporation oil-in-water emulsion steams 4~6h is sent out, is centrifuged evaporation residue to obtain cellulose microsphere, the cellulose microsphere obtained by distilled water flushing is to remove Dodecyl sodium sulfate therein is removed, is then cleaned multiple times with ethyl alcohol again to remove sorbester p17, is finally dried in vacuo, obtained pure Hollow porous fiber element microballoon;
(3) neopelex 0.7g, Polyethylene Octylphenol Ether the preparation of polyacrylate emulsion: are weighed Emulsifier 1.4g, acrylic acid 0.14mol, allyl glycidyl ether 0.14mol, butyl acrylate 0.14mol and ammonium persulfate 0.7g;By whole neopelexes, Polyethylene Octylphenol Ether emulsifier and account for the acrylic acid of total amount 1/3, two Methyl diallyl ammonium chloride, butyl acrylate and ammonium persulfate initiator are dissolved in the deionized water of 200mL, are uniformly stirred It mixes, controlled at 75 DEG C, stirs 1h;Then by residue 2/3 acrylic acid, allyl glycidyl ether, butyl acrylate and Ammonium persulfate initiator monomer and ammonium persulfate initiator are dissolved in 20mL deionized water, and it is molten to be added dropwise to the mixing just stirred In liquid, time for adding is controlled in 2h, after being added dropwise, is kept the temperature 2.5h, is obtained multiple emulsion, this lotion places January, does not send out Raw lamination can be prepared by polyacrylate emulsion coating agent;
(4) mixing of lotion: the lotion of the hollow porous fiber element microballoon of step (2) preparation and step (3) preparation is mixed It closing, wherein the mass volume ratio of the lotion of the hollow porous fiber element microballoon and step (3) preparation of step (2) preparation is 1 ︰ 20, Mixed solution is stirred into 1h on high speed dispersion homogenizer, whipping temp is 50 DEG C, and hollow porous fiber element can be obtained Microballoon/polyacrylate multiple emulsion, this lotion are Waterproof Breathable type cotton fabric coating c;
Another object of the present invention is to provide the application of Waterproof Breathable type cotton fabric coating c obtained above a kind of, The specific scheme is that on taut frame that cotton fabric is tight, coating agent scraper is uniformly applied and is scraped on cotton fabric, coating weight dry weight is 25g/m2, dry 2 minutes, baked in 170 DEG C 3 minutes in 90 DEG C.
PERFORMANCE EXAMPLES:
(1) film forming finish, glue coating agent performance evaluation: are carried out to coating agent a, b, c of Examples 1 to 3 preparation respectively Performance and glue film water absorption rate test are stretched in film drawing, and test method is as follows: the finish that (a) forms a film test: lotion being uniformly applied to On clean glass plate, then 30 DEG C of constant temperature film forming bake 3min under the conditions of 160 DEG C, observe the bright flatness of film forming, and With hand inspection pliability.(b) performance test is stretched in glue film drawing: the glue film after baking is cut into the slice of about (30 × 3 × 1) mm, It is stretched on strength tester.(c) glue film water absorption rate test: the glue film after baking is claimed to constant weight, immerses 25 DEG C of water In for 24 hours, blot film surface droplet, claim quality.Glue film water absorption rate (%)=(film quality-drying film quality after water suction)/desciccator diaphragm Quality × 100.For the coating agent of buying from Lu Ke chemical industry Co., Ltd, Shandong Province, test result is as shown in table 1:
The coating agent prepared by the present invention of table 1 is compared with the coating agent performance of buying
Project Coating agent a Coating agent b Coating agent c The coating agent of buying
Form a film gloss Without scalelike mark Without scalelike mark Scalelike mark is less Scalelike mark is less
Tensile strength/MPa 14.875 15.267 14.276 17.337
Elongation at break/% 523.5 519.6 571.8 727.8
Glue film water absorption rate/% 33.6 33.8 34.5 29.8
Seen from table 1, the film forming gloss of coating agent a, b, c prepared by the present invention is in less scalelike mark or without scalelike mark, Slightly better than the coating agent of buying;Its tensile strength is slightly below the coating agent purchased;Its elongation at break is slightly below the coating purchased Agent;Glue film water absorption rate is more slightly higher than the coating agent of buying.Comprehensive analysis thinks, the coating agent of coating agent prepared by the present invention and buying Performance indicator it is close.
(2) coated fabric performance evaluation: the cotton fabric arranged to the coating agent of Examples 1 to 3 preparation carries out gloss respectively Degree, vapor transfer rate, resistance to hydrostatic pressure and the test of surface moisture resistance.Glossiness presses FZ/T 01097-2006 " fabric sheen test method " Standard testing;Method for washing washes 10 by GB/T 8629-2001 " Textile Test with home washings and drying program " 5A program It is secondary;Surface moisture resistance is by GB/T4745-2012 " detection and evaluation of textile water proof performance get wet method " standard testing;Resistance to hydrostatic FZ/T1004-9l regulation is pressed to carry out;Vapor transfer rate presses GB/T12704-91 " fabric moisture transmission quantity measuring method " standard testing;It adopts For the coated cotton fibers of purchase from Lu Ke chemical industry Co., Ltd, Shandong Province, test result is as shown in table 2:
The performance test results of the coated cotton fibers prepared by the present invention of table 2 and the coated cotton fibers of buying
As can be seen from Table 2, cotton fabric is after coating agent top finish prepared by the present invention, the glossiness of coated fabric reaches 11 or more, it is almost approached with the coated fabric of buying;Resistance to hydrostatic pressure reaches 6400~7250Pa, hence it is evident that the coating higher than buying is knitted Object;Its surface moisture resistance illustrates it with very strong water-proof function also superior to the coated cotton fibers of buying;Its vapor transfer rate reaches 250~270g/ (m2For 24 hours), hence it is evident that higher than the coated cotton fibers of buying, illustrate that it has the function of very strong moisture-inhibiting.Its coating After 10 washings, indices are not decreased obviously fabric, and especially feel is not also hardened, and illustrate coated cotton fibers Stability and durability are fine.Comprehensive analysis thinks: coating agent prepared by the present invention is a kind of Waterproof Breathable type cotton of qualification Textile coating agent.

Claims (2)

1. a kind of preparation method of Waterproof Breathable type cotton fabric coating, which is characterized in that described method includes following steps:
(1) preparation of oil-in-water emulsion: cellulose is swollen 2~4h in glacial acetic acid, is then dissolved in acetic anhydride and acetic acid Mixed solution in, sulfuric acid is added dropwise into system, 2~5h is reacted at 55 DEG C, after reaction, in sodium hydroxide and system In sulfuric acid to pH be 7~8, then above-mentioned reactant is poured into and is settled out cellulose acetate in distilled water, finally by gained vinegar The multiple centrifugal elutriation of acid cellulose is to neutrality, then is dried in vacuo;Resulting dry cellulose acetate is dissolved in methylene chloride, is obtained The solution of clear is added sorbester p17 in Xiang Shangshu solution, is uniformly mixed, above-mentioned mixed liquor is added to dodecyl It in the aqueous solution of sodium sulfonate, is stirred continuously, obtains oil-in-water emulsion;The volume ratio of the acetic anhydride and acetic acid is 1: (1~ 1.5);The dosage of sulfuric acid is the 1.0~1.5% of acetic anhydride and acetic acid total volume;Methylene chloride and sodium dodecyl sulfate aqueous solution Volume ratio be 1: (5~7);The weight ratio of cellulose acetate and sorbester p17 is 1: (0.10~0.15);Dodecyl sodium sulfate The mass fraction of aqueous solution is 0.75~1.0%;
(2) preparation of hollow porous fiber element microballoon: the methylene chloride in control condition slow evaporation oil-in-water emulsion, evaporation Time is 4~6h;It is centrifuged evaporation residue to obtain cellulose microsphere, the cellulose microsphere obtained by distilled water flushing To remove dodecyl sodium sulfate therein, then it is cleaned multiple times with ethyl alcohol again to remove sorbester p17, is finally dried in vacuo, obtains Pure hollow porous fiber element microballoon;
(3) preparation of polyacrylate emulsion: weigh neopelex, Polyethylene Octylphenol Ether emulsifier, Acrylic acid, allyl glycidyl ether, butyl acrylate and ammonium persulfate;The neopelex, sim alkylphenol are poly- Ethylene oxide ether emulsifier, acrylic acid, allyl glycidyl ether, butyl acrylate and ammonium persulfate ratio are as follows: (0.5~1) g : (1~2) g: (0.1~0.2) mol: (0.1~0.2) mol: (0.1~0.2) mol: (0.5~1) g;By whole dodecyls Benzene sulfonic acid sodium salt, Polyethylene Octylphenol Ether emulsifier and the acrylic acid, allyl glycidyl ether, acrylic acid that account for total amount 1/3 Butyl ester and ammonium persulfate initiator are dissolved in deionized water, uniform stirring, controlled at 75~85 DEG C, stir 1~2h;So After acrylic acid, allyl glycidyl ether, butyl acrylate and the ammonium persulfate initiator of residue 2/3 are dissolved in deionized water afterwards It is added drop-wise in the mixed solution just stirred, time for adding is controlled in 2~3h, after being added dropwise, is kept the temperature 2~3h, is obtained poly- Acrylic emulsion coating agent, this lotion place January, lamination do not occur;
(4) mixing of lotion: hollow porous fiber element microballoon prepared by step (2) is mixed with lotion prepared by step (3), The mass volume ratio of the lotion of the hollow porous fiber element microballoon and step (3) preparation of the step (2) preparation be 1g ︰ (10~ 20) mL;Mixed solution is stirred into 1~2h on high speed dispersion homogenizer, whipping temp is 50~60 DEG C, be can be obtained Empty porous cellulose microballoon/polyacrylate multiple emulsion, this lotion are Waterproof Breathable type cotton fabric coating.
2. a kind of application using Waterproof Breathable type cotton fabric coating described in claim 1, which is characterized in that the application Method are as follows: it is on taut frame that cotton fabric is tight, coating agent scraper is uniformly applied and is scraped on fabric, is dried 2 minutes in 90 DEG C, in 140~170 DEG C bake 3 minutes, and coating weight dry weight is 20~25g/m2
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