CN109706746B - Water-repellent polyolefin elastic fabric - Google Patents
Water-repellent polyolefin elastic fabric Download PDFInfo
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Abstract
The invention discloses a water-repellent polyolefin polyester fabric, which comprises a polyolefin polyester fabric substrate and an organic silicon water-repellent finishing agent latex film arranged on the surface of the substrate; according to the mass portion, 10 portions of water repellent finishing agent, 4 portions of thickening agent and 86 portions of water are mixed and fully stirred to form coating agent, the viscosity reaches 35000 and 40000CPS, and the viscosity is 70-90 portions/m2Coating the coating agent on a polyolefin polyester fabric substrate, and drying at 70 ℃ for 5min and at 160 ℃ for 2min to prepare the water-repellent polyolefin polyester fabric; the organic silicon water repellent finishing agent is formed by blending organic silicon modified acrylate emulsion and organic silicon modified polyurethane emulsion according to the mass ratio of 1:1.2-1: 2. Due to the modification of the organic silicon, the polyolefin polyester fabric has good waterproof performance and air permeability.
Description
Technical Field
The invention relates to a functional fabric, in particular to a water-repellent polyolefin elastic fabric, and belongs to the field of functional textile fabrics.
Background
In recent years, with the rapid development of social life, the living standard of people is improved, the requirements on clothes, food, live and walk are higher and higher, and the clothes are required to have the functions of comfort, moisture permeability, perspiration, wrinkle resistance, water resistance, oil resistance, easy decontamination, ultraviolet resistance, static resistance and the like. Different industries require different garments for practitioners, for example, those in outdoor sports require outer garments to have water and soil release properties.
The elastic fabric is a fabric woven by a shuttle loom from yarns containing elastic fibers. The fabric with elastic fibers only in the warp yarns is called warp elastic fabric, the fabric with elastic fibers only in the weft yarns is called weft elastic fabric, and the fabric with elastic fibers in both the warp yarns and the weft yarns is called four-side elastic fabric. The yarn of the sports fabric is mainly made of chemical fibers such as terylene and chinlon, and the spandex is a common elastic fiber and is added into the yarn in an air-covered mode. However, spandex is inferior in weather resistance, particularly in resistance to chemicals such as chlorine water.
The waterproof fabric is a fabric which forms a waterproof and airtight continuous film on the surface of a fabric and prevents water and air from passing through by using a physical or chemical method. The waterproof performance of the fabric is obtained mainly by two ways, namely, special fibers or functional fibers are used; the other is to apply the finishing agent to the fabric to improve the surface property of the fabric, so that the surface tension of the fabric is lower than that of water, thereby the water is not easy to permeate on the fabric, and the air permeability of the fabric is not influenced.
At present, the fabric water repellent finishing agent mainly comprises: fluorine-containing finishing agents, silicone finishing agents, and the like.
(1) Fluorine-containing finishing agent
Because fluorine atoms are active in chemical property and high in electronegativity, the intermolecular cohesive force between C-F bonds is small, and the intermolecular acting force of compounds containing C-F bonds is small, so that the surface energy of the fluorine-containing compounds is reduced.
When the fluorine-containing compound is acted on the surface of the fabric for waterproof finishing, hydrophobic groups in the molecules of the fluorine-containing compound extend to the air, namely, the fluorine-containing groups are arranged on the outer layer, and hydrophilic groups are directed to the fiber substrate, so that the surface of the fabric is full of the hydrophobic groups, the surface energy of the fabric is reduced, and the surface of the fabric has certain waterproofness. The fluorine-containing finishing agent has excellent waterproof performance, oil repellency and anti-fouling performance. But the use of fluorine-containing adjuvants tends to be prudent for environmental reasons.
(2) Silicone materials are widely used because of their excellent properties and water repellency. The polysiloxane is a polymer with a main chain formed by alternately bonding silicon atoms and oxygen atoms, the main chain of the polysiloxane is a repeated Si-O bond, an organic group is directly connected to the polymer on the silicon atoms, the bond spacing of the Si-O bond in the molecule is long, the bonding angle between Si-O-Si is large, the bond energy is also large, and the silicon-oxygen chain has methyl shielding, so that the polysiloxane chain segment is very soft; the polysiloxane has a low surface tension due to the low interaction force between the siloxane chains and the large molar volume. The polysiloxane has a special molecular structure, so that the polysiloxane has excellent performances of good film forming property, high air permeability, high temperature resistance, water repellency and the like. However, silicone also has disadvantages such as insufficient mechanical strength and poor adhesion.
The waterborne polyurethane has the advantages of good physical and mechanical properties, excellent cold resistance, elasticity, high gloss and the like, but has poor water resistance and poor mechanical strength. The acrylate emulsion has good water resistance and weather resistance, and the high wear resistance and good mechanical property of the polyurethane can be organically combined with the good weather resistance and water resistance of the acrylate by modifying the polyurethane with the acrylate emulsion, so that the performance of the polyurethane/acrylate is obviously improved.
By combining the advantages of organic silicon and acrylate/polyurethane, and utilizing the water repellent function of environment-friendly organic siloxane, a fluorine-free water repellent finishing agent is formed, and the environment-friendly water repellent fabric is prepared.
Disclosure of Invention
The invention aims to take polyolefin elastic fabric as a substrate, respectively modify acrylate and polyurethane with organic silicon to form organic silicon functional emulsion, then blend the organic silicon functional emulsion to obtain a fluorine-free green environment-friendly organic silicon water repellent finishing agent, and coat the surface of the fabric to obtain the water repellent polyolefin elastic fabric.
In order to achieve the purpose, the invention adopts the following technical scheme.
A water repellent polyolefin elastic fabric comprises a polyolefin elastic fabric substrate and an organic silicon water repellent coating agent adhesive film arranged on the surface of the substrate;
according to the mass portion, 10 portions of organosilicon water-repellent finishing agent, 4 portions of thickening agent and 86 portions of water are mixed and fully stirred to form organosilicon water-repellent coating agent, the viscosity reaches 35000-40000CPS, and 70-90 portions/m2Coating the organic silicon water repellent coating agent on a polyolefin elastic fabric substrate, and then drying at 70 ℃ for 5min and at 160 ℃ for 2min to prepare the water repellent polyolefin elastic fabric;
the organic silicon water repellent finishing agent is formed by blending organic silicon modified acrylate emulsion and organic silicon modified polyurethane emulsion; the mass ratio of the organic silicon modified acrylate emulsion to the organic silicon modified polyurethane emulsion is 1:1.2-1: 2;
the organic silicon modified acrylate emulsion is prepared by adopting an emulsion polymerization method and comprises the following raw materials in parts by weight: 250-350 parts of acrylate mixed monomer, (shown as formula a) 35-52 parts of organosilicon monomer, 16-24 parts of emulsifier, 15-21 parts of diacetone acrylamide, 3-5 parts of initiator and 800 parts of deionized water, wherein the acrylate mixed monomer comprises methyl methacrylate, butyl acrylate and ethyl acrylate in a mass ratio of 1:2: 1; the preparation method of the organic silicon modified acrylate emulsion comprises the following steps:
(1) adding deionized water and an emulsifier into a four-neck flask at normal temperature, stirring for dissolving, slowly dropwise adding an acrylate mixed monomer, an organic silicon monomer and diacetone acrylamide under high-speed stirring (the rotating speed is 1500r/min), and stirring for 30min to obtain a stable milky pre-emulsion; dissolving an initiator and part of deionized water to prepare an initiator aqueous solution;
(2) adding 30% of the pre-emulsion obtained in the step (1) into a reactor, adding 20% of initiator aqueous solution under low-speed stirring at 200r/min in a water bath at 65 ℃, stirring for reaction for 30min, then heating to 70 ℃, supplementing 10% of initiator aqueous solution when blue light appears in the system, preserving heat and continuously reacting for 30min to obtain seed emulsion;
(3) maintaining the temperature at 70-72 ℃, dropwise adding the rest of pre-emulsion and the initiator aqueous solution for 2-3h, continuously stirring for reacting for 2h after dropwise adding, then cooling to room temperature, and filtering to obtain the organic silicon modified acrylate emulsion;
the preparation method of the organic silicon modified polyurethane emulsion comprises the following steps:
a. adding 1400 parts of dehydrated 1200-1400 parts of polyhydric alcohol (molecular weight 2000), 80-120 parts of double-end hydroxyl straight-chain dimethyl silicone oil (molecular weight 3000), 380-450 parts of diisocyanate, 24-46 parts of dihydroxy organic silicon monomer (shown as formula b), 0.3-0.5 part of dibutyltin dilaurate into a reactor provided with a stirrer, a thermometer and a condenser, and stirring and reacting for 5 hours at 90 ℃;
b. cooling to 60 ℃, adding 76-92 parts of dimethylolpropionic acid and 500 parts of acetone, and continuing to react for 3 hours;
c. adding 12-18 parts of 1, 4-butanediol, and carrying out chain extension reaction for 2 hours;
d. adding 14-21 parts of adipic acid dihydrazide, and carrying out end-capping reaction on a double-end NCO group for 2 hours;
e. cooling to 40 ℃ after the reaction is finished, and adding 48-66 parts of triethylamine for neutralization for 30 min;
f. and (2) adding 6800-8000 parts of deionized water by a step-by-step addition method under high-speed stirring for emulsification, and removing acetone under reduced pressure after the emulsification is finished to obtain the organic silicon modified polyurethane emulsion.
The emulsifier is formed by compounding an anionic emulsifier and a nonionic emulsifier according to the mass ratio of 2: 1.
The anionic emulsifier is one or more of sodium dodecyl sulfate, sodium dodecyl diphenyl ether disulfonate and sodium dodecyl benzene sulfonate.
The nonionic emulsifier is as follows: one or more of nonylphenol polyoxyethylene ether TX-10, TX-12, fatty alcohol polyoxyethylene ether AEO-9 and AEO-15.
The initiator is one of sodium persulfate, potassium persulfate and ammonium persulfate.
The polyalcohol is one or more of polypropylene oxide ether dihydric alcohol, polytetrahydrofuran ether dihydric alcohol, adipic acid polyester diol, polycaprolactone polyalcohol and polycarbonate diol.
The diisocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate.
The organosilicon has a unique chemical structure, and oxygen atoms and silicon atoms in a silicon-oxygen chain structure are alternately arranged and form a spiral straight-chain structure in a winding way. Two groups (typically methyl) attached to each silicon atom rotate around the Si — O. The methyl and silicon atoms in the molecular chain have weak hydrophilicity, and the only oxygen atom with better affinity with water is wrapped by the methyl, so the polysiloxane has good hydrophobicity. The siloxane bond has a large bond angle and can rotate freely, so that the organic silicon molecule has good lubricity and flexibility. Meanwhile, the surface energy of the organic silicon is low, and the organic silicon tends to be enriched to the surface of the coating in the film forming process, so that the organic silicon is applied to the fabric after modifying the waterborne polyurethane and the acrylic ester, and the coating with excellent waterproof performance and comprehensive performance can be obtained. In addition, the silica-alumina composite material has small interaction force and large molar volume, so that the silica-alumina composite material has good high air permeability.
Existing organic silicon acrylate emulsion and organic silicon polyurethane emulsionThe organosilicon monomer used in the liquid is usually vinyl silicone oil, hydroxy silicone oil, octamethylcyclotetrasiloxane, tetravinyl octamethylcyclotetrasiloxane, and a silane coupling agent containing a C ═ C bond is an organosilicon modifier. Vinyl silicone oil and hydroxy silicone oil have high viscosity and are difficult to emulsify, D4Silane coupling agents and the like containing hydrolyzable groups Si-O-CH3In the emulsion polymerization process, hydrolysis and condensation occur to a certain extent, so that excessive crosslinking among polymer molecules causes unstable reaction, and a stable organosilicon modified emulsion with high silicon content is difficult to obtain. The invention prepares organosilicon monomer which is difficult to hydrolyze, and Si-OCH in methoxysilane3Replacement of the radical by a more sterically hindered Si (CH)3)3The stable emulsion prepared by emulsifying and copolymerizing the acrylic ester monomer not only solves the problem of containing Si-OCH3The hydrolysis problem of the monomers of the group in the emulsion polymerization process improves the water repellency of the emulsion.
The diacetone acrylamide (DAAM) is introduced into the acrylate emulsion, the Adipic Dihydrazide (ADH) is introduced into the polyurethane emulsion, the crosslinking sites in the system are increased after the two emulsions are blended, and the diacetone acrylamide and the adipic dihydrazide are subjected to crosslinking reaction at a certain temperature, so that the self-crosslinking performance of the emulsion is improved.
The polyolefin elastic fabric has good heat resistance, can restore the elasticity of the fiber after being subjected to heat finishing, has good drapability and hand feeling, has strong stability to most of strongly corrosive chemical substances, and has the characteristics of washability, bleaching, steam ironing resistance, ironing and dry cleaning. The organic silicon water repellent coating agent is arranged on the surface of the fabric to form an adhesive film, so that the fabric has excellent water repellency.
Detailed Description
The unit "part" of the component raw materials related to the invention refers to "part by mass".
The preparation method of the organic silicon monomer and the dihydroxy organic silicon monomer is as follows.
The organic silicon monomer is prepared by reacting 2- (trimethylsiloxy) ethanolamine with ethyl methacrylate, and the method comprises the following steps:
adding dehydrated 2- (trimethylsiloxy) ethanolamine, ethyl methacrylate and dibutyltin dilaurate into a reactor provided with a stirrer, a thermometer and a condenser, and stirring at 100 ℃ for 5 hours to react to obtain a functional organic silicon monomer containing C ═ C bonds; the molar ratio of the 2- (trimethylsiloxy) ethanolamine to the isocyanate ethyl methacrylate is 1:1, and the mass of the dibutyltin dilaurate accounts for 0.4 percent of the total mass of the reaction monomers. The involved reaction process is shown as (1).
The preparation method of the 2- (trimethylsiloxy) ethanolamine comprises the following steps: adding ethanolamine into a reactor with a mechanical stirrer and a thermometer, stirring and dropwise adding hexamethyldisilazane, reacting at 5-50 ℃ for 0.5-2 h, and obtaining 2- (trimethylsiloxy) ethanolamine through decompression and filtration after the reaction is finished. The molar ratio of ethanolamine to hexamethyldisilazane was 2: 1.
The dihydroxy organic silicon monomer is prepared by reacting diethanolamine, NaOH and trimethylchlorosilane, and the preparation method comprises the following steps:
adding diethanolamine and 0.4mol/L NaOH aqueous solution into a three-neck flask with a stirrer and a reflux condenser, slowly adding trimethylchlorosilane into the flask, reacting at 70 ℃ for 80min after the addition is finished, carrying out reduced pressure distillation, removing redundant water and unreacted diethanolamine, and obtaining N-diethanol-trimethyl silicon (dihydroxyorganosilicon monomer); wherein, the molar ratio of the added diethanol amine to the added trimethyl chlorosilane is 1.1:1, and the molar ratio of the trimethyl chlorosilane to the NaOH is 1:1. The reaction process is shown as (2).
The polyolefin elastic fabric comprises the following components: 88% of terylene, 12% of Polyolefin (POE), specification: 75D +70D, gram weight: 100g/m2。
Example 1:
a water repellent polyolefin elastic fabric comprises a polyolefin elastic fabric substrate and an organic silicon water repellent coating agent adhesive film arranged on the surface of the substrate;
according to the mass parts, 10 parts of organosilicon water repellent finishing agent, 4 parts of polyacrylic acid thickening agent and 86 parts of water are mixed and fully stirred to form organosilicon water repellent coating agent, the viscosity reaches 35000-40000CPS, and 70 parts/m2Coating the coating agent on a polyolefin elastic fabric substrate, drying at 70 ℃ for 5min, and baking at 160 ℃ for 2min, wherein the organosilicon water-repellent coating agent forms an adhesive film on the surface of the fabric to prepare the water-repellent polyolefin elastic fabric;
the organic silicon water repellent finishing agent is formed by blending organic silicon modified acrylate emulsion and organic silicon modified polyurethane emulsion; the mass ratio of the organic silicon modified acrylate emulsion to the organic silicon modified polyurethane emulsion is 1: 1.2;
the organic silicon modified acrylate emulsion is prepared by adopting an emulsion polymerization method and comprises the following raw materials in parts by weight: 250 parts of acrylate mixed monomer, 35 parts of organic silicon monomer, 16 parts of emulsifier, 15 parts of diacetone acrylamide, 3 parts of initiator and 600 parts of deionized water, wherein the acrylate mixed monomer consists of methyl methacrylate, butyl acrylate and ethyl acrylate in a mass ratio of 1:2: 1; the emulsifier is composed of anionic emulsifier sodium dodecyl sulfate and nonionic emulsifier nonylphenol polyoxyethylene ether TX-10 in a mass ratio of 2: 1; the initiator is sodium persulfate;
the preparation method of the organic silicon modified acrylate emulsion comprises the following steps:
(1) adding 570 parts of deionized water and an emulsifier into a four-neck flask at normal temperature, stirring for dissolving, slowly dropwise adding an acrylate mixed monomer, an organic silicon monomer (shown as the formula a) and diacetone acrylamide under high-speed stirring (the rotating speed is 1500r/min), and stirring for 30min to obtain a stable milky pre-emulsion; dissolving an initiator and 30 parts of deionized water to prepare an initiator aqueous solution;
(2) adding 30% of the pre-emulsion obtained in the step (1) into a reactor, adding 20% of initiator aqueous solution under low-speed stirring at 200r/min in a water bath at 65 ℃, stirring for reaction for 30min, then heating to 70 ℃, supplementing 10% of initiator aqueous solution when blue light appears in the system, preserving heat and continuously reacting for 30min to obtain seed emulsion;
(3) maintaining the temperature at 70-72 ℃, dropwise adding the rest of pre-emulsion and the initiator aqueous solution for 2-3h, continuously stirring for reacting for 2h after dropwise adding, then cooling to room temperature, and filtering to obtain the organic silicon modified acrylate emulsion;
the preparation method of the organic silicon modified polyurethane emulsion comprises the following steps:
a. 1200 parts of polycaprolactone polyol (molecular weight 2000), 80 parts of double-end hydroxyl straight-chain dimethyl silicone oil (molecular weight 3000), 380 parts of diphenylmethane diisocyanate, 24 parts of dihydroxy organosilicon monomer (shown as formula b) and 0.3 part of dibutyltin dilaurate which are subjected to dehydration treatment are added into a reactor provided with a stirrer, a thermometer and a condenser tube, and are stirred and reacted for 5 hours at 90 ℃;
b. cooling to 60 ℃, adding 76 parts of dimethylolpropionic acid and 500 parts of acetone, and continuing to react for 3 hours;
c. adding 12 parts of 1, 4-butanediol, and carrying out chain extension reaction for 2 hours;
d. adding 14 parts of adipic acid dihydrazide, and carrying out end-capping reaction on a double-end NCO group for 2 hours;
e. after the reaction is finished, cooling to 40 ℃, adding 48 parts of triethylamine to neutralize for 30 min;
f. and (2) adding 6800 parts of deionized water by a step-by-step addition method under high-speed stirring for emulsification, and removing acetone under reduced pressure after the emulsification is finished to obtain the organic silicon modified polyurethane emulsion.
Example 2:
a water repellent polyolefin elastic fabric comprises a polyolefin elastic fabric substrate and an organic silicon water repellent coating agent adhesive film arranged on the surface of the substrate;
according to the mass parts, 10 parts of organosilicon water repellent finishing agent, 4 parts of polyacrylic acid thickening agent and 86 parts of water are mixed and fully stirred to form organosilicon water repellent coating agent, the viscosity reaches 35000-40000CPS, and 80 parts/m2The organic silicon water repellent coating agent is coated on the polyolefin bombDrying the fabric substrate at 70 ℃ for 5min and at 160 ℃ for 2min, and forming an adhesive film on the surface of the fabric by using the organic silicon water-repellent coating agent to prepare the water-repellent polyolefin elastic fabric;
the organic silicon water repellent finishing agent is formed by blending organic silicon modified acrylate emulsion and organic silicon modified polyurethane emulsion; the mass ratio of the organic silicon modified acrylate emulsion to the organic silicon modified polyurethane emulsion is 1: 1.6;
the organic silicon modified acrylate emulsion is prepared by adopting an emulsion polymerization method and comprises the following raw materials in parts by weight: 300 parts of acrylate mixed monomer, 44 parts of organic silicon monomer, 20 parts of emulsifier, 18 parts of diacetone acrylamide, 4 parts of initiator and 700 parts of deionized water, wherein the acrylate mixed monomer consists of methyl methacrylate, butyl acrylate and ethyl acrylate in a mass ratio of 1:2: 1; the emulsifier is formed by compounding anionic emulsifier sodium dodecyl diphenyl ether disulfonate and nonionic emulsifier fatty alcohol polyoxyethylene ether AEO-9 according to the mass ratio of 2: 1; the initiator is potassium persulfate;
the preparation method of the organic silicon modified acrylate emulsion comprises the following steps:
(1) adding 670 parts of deionized water and an emulsifier into a four-neck flask at normal temperature, stirring for dissolving, slowly dropwise adding an acrylate mixed monomer, an organic silicon monomer (shown as the formula a) and diacetone acrylamide under high-speed stirring (the rotating speed is 1500r/min), and stirring for 30min to obtain a stable milky pre-emulsion; dissolving an initiator and 30 parts of deionized water to prepare an initiator aqueous solution;
(2) adding 30% of the pre-emulsion obtained in the step (1) into a reactor, adding 20% of initiator aqueous solution under low-speed stirring at 200r/min in a water bath at 65 ℃, stirring for reaction for 30min, then heating to 70 ℃, supplementing 10% of initiator aqueous solution when blue light appears in the system, preserving heat and continuously reacting for 30min to obtain seed emulsion;
(3) maintaining the temperature at 70-72 ℃, dropwise adding the rest of pre-emulsion and the initiator aqueous solution for 2-3h, continuously stirring for reacting for 2h after dropwise adding, then cooling to room temperature, and filtering to obtain the organic silicon modified acrylate emulsion;
the preparation method of the organic silicon modified polyurethane emulsion comprises the following steps:
a. 1300 parts of polytetrahydrofuran ether glycol (molecular weight 2000), 100 parts of double-end hydroxyl straight chain dimethyl silicone oil (molecular weight 3000), 420 parts of isophorone diisocyanate, 34 parts of dihydroxy organic silicon monomer (shown as formula b) and 0.4 part of dibutyltin dilaurate which are subjected to dehydration treatment are added into a reactor provided with a stirrer, a thermometer and a condenser tube, and are stirred and reacted for 5 hours at the temperature of 90 ℃;
b. cooling to 60 ℃, adding 84 parts of dimethylolpropionic acid and 500 parts of acetone, and continuing to react for 3 hours;
c. adding 15 parts of 1, 4-butanediol, and carrying out chain extension reaction for 2 hours;
d. adding 17 parts of adipic acid dihydrazide, and carrying out end-capping reaction on a double-end NCO group for 2 hours;
e. after the reaction is finished, cooling to 40 ℃, adding 58 parts of triethylamine to neutralize for 30 min;
f. and (2) under high-speed stirring, adding 7400 parts of deionized water by adopting a step-by-step addition method for emulsification, and removing acetone under reduced pressure after the emulsification is finished to obtain the organic silicon modified polyurethane emulsion.
Example 3:
a water repellent polyolefin elastic fabric comprises a polyolefin elastic fabric substrate and an organic silicon water repellent coating agent adhesive film arranged on the surface of the substrate;
according to the mass parts, 10 parts of organosilicon water repellent finishing agent, 4 parts of polyacrylic acid thickening agent and 86 parts of water are mixed and fully stirred to form organosilicon water repellent coating agent, the viscosity reaches 35000-40000CPS, and the viscosity is 90 parts per m2Coating the organic silicon water repellent coating agent on a polyolefin elastic fabric substrate, drying at 70 ℃ for 5min, and baking at 160 ℃ for 2min, wherein the organic silicon water repellent coating agent forms an adhesive film on the surface of the fabric to prepare the water repellent polyolefin elastic fabric;
the organic silicon water repellent finishing agent is formed by blending organic silicon modified acrylate emulsion and organic silicon modified polyurethane emulsion; the mass ratio of the organic silicon modified acrylate emulsion to the organic silicon modified polyurethane emulsion is 1: 2;
the organic silicon modified acrylate emulsion is prepared by adopting an emulsion polymerization method and comprises the following raw materials in parts by weight: 350 parts of acrylate mixed monomer, 52 parts of organic silicon monomer, 24 parts of emulsifier, 21 parts of diacetone acrylamide, 5 parts of initiator and 800 parts of deionized water, wherein the acrylate mixed monomer consists of methyl methacrylate, butyl acrylate and ethyl acrylate in a mass ratio of 1:2: 1; the emulsifier is composed of an anionic emulsifier sodium dodecyl benzene sulfonate and a nonionic emulsifier nonylphenol polyoxyethylene ether TX-12 in a mass ratio of 2: 1; the initiator is ammonium persulfate;
the preparation method of the organic silicon modified acrylate emulsion comprises the following steps:
(1) adding 770 parts of deionized water and an emulsifier into a four-neck flask at normal temperature, stirring for dissolving, slowly dropwise adding an acrylate mixed monomer, an organic silicon monomer (shown as the formula a) and diacetone acrylamide under high-speed stirring (the rotating speed is 1500r/min), and stirring for 30min to obtain a stable milky pre-emulsion; dissolving an initiator and 30 parts of deionized water to prepare an initiator aqueous solution;
(2) adding 30% of the pre-emulsion obtained in the step (1) into a reactor, adding 20% of initiator aqueous solution under low-speed stirring at 200r/min in a water bath at 65 ℃, stirring for reaction for 30min, then heating to 70 ℃, supplementing 10% of initiator aqueous solution when blue light appears in the system, preserving heat and continuously reacting for 30min to obtain seed emulsion;
(3) maintaining the temperature at 70-72 ℃, dropwise adding the rest of pre-emulsion and the initiator aqueous solution for 2-3h, continuously stirring for reacting for 2h after dropwise adding, then cooling to room temperature, and filtering to obtain the organic silicon modified acrylate emulsion;
the preparation method of the organic silicon modified polyurethane emulsion comprises the following steps:
a. 1400 parts of dehydrated polypropylene oxide ether glycol (molecular weight 2000), 120 parts of double-end hydroxyl straight chain dimethyl silicone oil (molecular weight 3000), 450 parts of toluene diisocyanate, 46 parts of dihydroxy organic silicon monomer (shown as the formula b) and 0.5 part of dibutyltin dilaurate are added into a reactor provided with a stirrer, a thermometer and a condenser pipe, and stirred and reacted for 5 hours at 90 ℃;
b. cooling to 60 ℃, adding 92 parts of dimethylolpropionic acid and 500 parts of acetone, and continuing to react for 3 hours;
c. adding 18 parts of 1, 4-butanediol, and carrying out chain extension reaction for 2 hours;
d. adding 21 parts of adipic acid dihydrazide, and carrying out end-capping reaction on a double-end NCO group for 2 hours;
e. after the reaction is finished, cooling to 40 ℃, adding 66 parts of triethylamine to neutralize for 30 min;
f. and (2) under high-speed stirring, adding 8000 parts of deionized water by a step-by-step addition method for emulsification, and after the emulsification is finished, removing acetone under reduced pressure to obtain the organic silicon modified polyurethane emulsion.
Waterproof performance: tested according to the method described in AATCC-22-2017. Spraying method: the water temperature is 27 ℃; washing procedure: and (3) washing at 27 ℃, performing conventional washing, hanging and airing, and washing with water for 20 times.
Chlorine water resistance tensile elastic recovery: the test was carried out according to the method described in FZ/T81021-2014.
The moisture permeability is tested according to the GB/T12704-.
Hydrostatic pressure performance is tested according to the method GB/T4744-2013.
The tearing strength is carried out according to the GB/T3917.1-2009 coating fabric tearing strength test method.
The results of the above performance tests are shown in table 1.
Table 1 water repellent polyolefin elastic fabric each performance test results
The test results in table 1 show that after the water repellent finishing agent is coated, the strength of the fabric is high, the chlorine water resistant stretch elastic recovery rate of the polyolefin elastic fabric is high, and the elasticity of the fabric is basically maintained; the fabric has high hydrostatic pressure and excellent waterproof performance, and can still keep good waterproof performance after being washed; the fabric also has good moisture permeability and does not have a dense and airtight film feeling.
Claims (7)
1. A water repellent polyolefin elastic fabric comprises a polyolefin polyester fabric substrate and an organic silicon water repellent coating agent adhesive film arranged on the surface of the substrate;
according to the mass portion, 10 portions of organosilicon water-repellent finishing agent, 4 portions of thickening agent and 86 portions of water are mixed and fully stirred to form organosilicon water-repellent coating agent, the viscosity reaches 35000-40000cps, and the viscosity is 70-90 portions/m2Coating the organic silicon water repellent coating agent on a polyolefin terylene fabric substrate, and then drying at 70 ℃ for 5min and at 160 ℃ for 2min to prepare the water repellent polyolefin elastic fabric;
the organic silicon water repellent finishing agent is formed by blending organic silicon modified acrylate emulsion and organic silicon modified polyurethane emulsion; the mass ratio of the organic silicon modified acrylate emulsion to the organic silicon modified polyurethane emulsion is 1:1.2-1: 2;
the organic silicon modified acrylate emulsion is prepared by adopting an emulsion polymerization method and comprises the following raw materials in parts by weight: 250-350 parts of acrylate mixed monomer, 35-52 parts of organic silicon monomer shown as formula a, 16-24 parts of emulsifier, 15-21 parts of diacetone acrylamide, 3-5 parts of initiator and 800 parts of deionized water, wherein the acrylate mixed monomer is composed of methyl methacrylate, butyl acrylate and ethyl acrylate in a mass ratio of 1:2: 1; the preparation method of the organic silicon modified acrylate emulsion comprises the following steps:
(1) adding deionized water and an emulsifier into a four-neck flask at normal temperature, stirring for dissolving, slowly dropwise adding an acrylate mixed monomer, an organic silicon monomer and diacetone acrylamide under high-speed stirring at a rotating speed of 1500r/min, and stirring for 30min to obtain a stable milky pre-emulsion; dissolving an initiator and part of deionized water to prepare an initiator aqueous solution;
(2) adding 30% of the pre-emulsion obtained in the step (1) into a reactor, adding 20% of initiator aqueous solution under low-speed stirring at 200r/min in a water bath at 65 ℃, stirring for reaction for 30min, then heating to 70 ℃, supplementing 10% of initiator aqueous solution when blue light appears in the system, preserving heat and continuously reacting for 30min to obtain seed emulsion;
(3) maintaining the temperature at 70-72 ℃, dropwise adding the rest of pre-emulsion and the initiator aqueous solution for 2-3h, continuously stirring for reacting for 2h after dropwise adding, then cooling to room temperature, and filtering to obtain the organic silicon modified acrylate emulsion;
the preparation method of the organic silicon modified polyurethane emulsion comprises the following steps:
a. adding 1400 parts of dehydrated 1200-1400 parts of polyhydric alcohol, 80-120 parts of double-end hydroxyl straight-chain dimethyl silicone oil, 450 parts of diisocyanate, 24-46 parts of dihydroxy organic silicon monomer shown as the formula b and 0.3-0.5 part of dibutyltin dilaurate into a reactor provided with a stirrer, a thermometer and a condensing tube, and stirring and reacting for 5 hours at 90 ℃;
b. cooling to 60 ℃, adding 76-92 parts of dimethylolpropionic acid and 500 parts of acetone, and continuing to react for 3 hours;
c. adding 12-18 parts of 1, 4-butanediol, and carrying out chain extension reaction for 2 hours;
d. adding 14-21 parts of adipic acid dihydrazide, and carrying out end-capping reaction on a double-end NCO group for 2 hours;
e. cooling to 40 ℃ after the reaction is finished, and adding 48-66 parts of triethylamine for neutralization for 30 min;
f. adding 6800-
2. The water-repellent polyolefin elastic fabric according to claim 1, characterized in that: the emulsifier is formed by compounding an anionic emulsifier and a nonionic emulsifier according to the mass ratio of 2: 1.
3. The water-repellent polyolefin elastic fabric according to claim 2, characterized in that: the anionic emulsifier is one or more of sodium dodecyl sulfate, sodium dodecyl diphenyl ether disulfonate and sodium dodecyl benzene sulfonate.
4. The water-repellent polyolefin elastic fabric according to claim 2, characterized in that: the nonionic emulsifier is as follows: one or more of nonylphenol polyoxyethylene ether TX-10, TX-12, fatty alcohol polyoxyethylene ether AEO-9 and AEO-15.
5. The water-repellent polyolefin elastic fabric according to claim 1, characterized in that: the initiator is one of sodium persulfate, potassium persulfate and ammonium persulfate.
6. The water-repellent polyolefin elastic fabric according to claim 1, characterized in that: the polyalcohol is one or more of polypropylene oxide ether dihydric alcohol, polytetrahydrofuran ether dihydric alcohol, adipic acid polyester diol, polycaprolactone polyalcohol and polycarbonate diol.
7. The water-repellent polyolefin elastic fabric according to claim 1, characterized in that: the diisocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate.
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| CN112796110B (en) * | 2020-12-31 | 2023-01-06 | 四川省纺织科学研究院 | Ketone-hydrazine cross-linking type water-based fluorine-free fabric waterproof finishing agent and preparation method and application thereof |
| CN113956783A (en) * | 2021-12-08 | 2022-01-21 | 浙江明丰实业股份有限公司 | Low-thermal-conductivity refrigeration coating and application thereof |
| CN114164663A (en) * | 2021-12-21 | 2022-03-11 | 广东湛丰精细化工有限公司 | High-performance durable polyurethane polyacrylate waterproof agent and preparation method thereof |
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