CN110409183A - A kind of free-floride water-proof aagent and its methods for making and using same - Google Patents

A kind of free-floride water-proof aagent and its methods for making and using same Download PDF

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CN110409183A
CN110409183A CN201910819968.XA CN201910819968A CN110409183A CN 110409183 A CN110409183 A CN 110409183A CN 201910819968 A CN201910819968 A CN 201910819968A CN 110409183 A CN110409183 A CN 110409183A
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parts
floride
agent
free
water
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熊贤银
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Sanyeng Household Products (heyuan) Co Ltd
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Sanyeng Household Products (heyuan) Co Ltd
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    • 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
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224Esters of carboxylic acids; Esters of carbonic acid
    • 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/236Esters of carboxylic acids; Esters of carbonic acid containing halogen atoms
    • 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46Compounds containing quaternary nitrogen atoms
    • 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
    • D06M15/53Polyethers
    • 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
    • D06M15/564Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • 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
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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

Abstract

The invention discloses a kind of floride-free water-proof aagent and its methods for making and using sames, it is related to textile finishing technical field, its key points of the technical solution are that a kind of free-floride water-proof aagent, a kind of free-floride water-proof aagent, based on parts by weight, including following component: 2-4 parts of floride-free spill resistant agent, 0.1-0.3 parts of crosslinking agent, 1-2 parts of bleeding agent, 1-2 parts of defoaming agent and 45-55 parts of water;The free-floride spill resistant agent includes fatty alcohol polyoxyethylene ether.The present invention passes through the characteristic of the low surface property of floride-free spill resistant agent, with excellent water repellency, cooperate floride-free spill resistant agent obtained that can quickly sprawl film forming in fiber surface with crosslinking agent, bleeding agent and defoaming agent it, the coefficient of friction of fiber surface is effectively reduced, improves the waterproof performance of fabric.

Description

A kind of free-floride water-proof aagent and its methods for making and using same
Technical field
The present invention relates to textile finishing technical fields, more specifically, it is related to a kind of floride-free water-proof aagent and its system Standby and methods for using them.
Background technique
Textile finishing refers to that all process for improving fabric quality are whole except scouringing and bleaching, dyeing, in addition to stamp Reason content generally comprise make fabric door width is neat, size modes stablize, improve fabric feeling, promote appearance of fabrics and it is fire-retardant, Water repellent, other arrangements such as refuse oily, hygienic, antistatic, easy decontamination;It is different for the field of employment of fabric, it is arranged selected from corresponding Content.For the shower curtain in bathroom, material is mainly textile fabric and plastic material, and textile fabric comes compared to plastic material It says, ageing-resistant performance and tear-resistant ability are stronger, therefore the service life is longer for the shower curtain of textile fabric, textile fabric Shower curtain is more widely applied;Existing shower curtain is usually terylene material with textile fabric, since the humidity in bathroom is higher, is got wet Polyester fabric afterwards is not easy drying, leads to its bacterium easy to breed, generates peculiar smell, therefore the polyester fabric of shower curtain usually requires Carry out water-proof finish.
Common fabric waterproof finishing agent includes fluorocarbon polymer, organosilicon, long chain alkane polymer knot currently on the market The water-proof aagent of structure.Fluorine-containing water repellent with preferable crystallinity, bulk density, thus with excellent waterproof due to imitating Fruit;But organic fluorine chemistry product PFOS (perfluorooctane sulfonate) and PFOA (perfluoro caprylic acid), to human body there is bioaccumulation, Different degrees of toxicity, persistence and potentially hazardous, therefore to receive some countries different degrees of for fluorine-contained finishing agent at present Limitation, thus the research that people put on floride-free water-proof aagent is more and more, current floride-free water-proof aagent is mainly Long chain alkane class waterproofing agent and waterproofing agent of organosilicon, although floride-free water-proof aagent is not easy to accumulate in vivo, endanger to human body Evil is small, is the product of comparatively safe environmental protection.But the waterproofness and washability of floride-free spill resistant agent traditional at present can't reach To the requirement of people.
Summary of the invention
One of the objects of the present invention is to provide a kind of floride-free water-proof aagents, pass through the low surface of floride-free spill resistant agent The characteristic of performance has excellent water repellency, cooperates free-floride obtained is anti-to sprinkle with crosslinking agent, bleeding agent and defoaming agent it Aqua can quickly sprawl film forming in fiber surface, and the coefficient of friction of fiber surface is effectively reduced, and improve the waterproof of fabric Performance.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of free-floride water-proof aagent, based on parts by weight, including following component: 2-4 parts of floride-free spill resistant agent, crosslinking agent 0.1- 0.3 part, 1-2 parts of bleeding agent, 1-2 parts of defoaming agent and 45-55 parts of water;The free-floride spill resistant agent includes aliphatic alcohol polyethenoxy Ether.
By using above-mentioned technical proposal, floride-free spill resistant agent has the characteristic of low surface property, has excellent water repellent It is cooperated floride-free spill resistant agent obtained that can quickly spread in fiber surface by performance with crosslinking agent, bleeding agent and defoaming agent Film is transformed into, the coefficient of friction of fiber surface is effectively reduced, improves the waterproof performance of fabric.
Further, α-isotridecyl-ω-hydroxyl-is poly- (oxygen -1,2- ethylidene).
By using above-mentioned technical proposal, α-isotridecyl-ω-hydroxyl-poly- (oxygen -1,2- ethylidene) is used as a kind of table Face activating agent can reduce the surface energy of water, cooperate with floride-free water-sprinkling agent, water repellent ability can be improved.
Further, the defoaming agent is oleic acid polyethylene glycol dibasic acid esters.
By using above-mentioned technical proposal, oleic acid polyethylene glycol dibasic acid esters is nonionic surfactant, is that a kind of yellow is solid Body, it is soluble easily in water, there is good smooth, emulsification, the flexibility of fabric can be improved, and reduce surface tension, it is right Floride-free water-proof aagent plays the role of defoaming, foam inhibition.
Further, the crosslinking agent is prepared with the following method: based on parts by weight, take 4-6 parts of dihydromethyl propionic acids, 4-6 parts of ethylene glycol and 30-40 parts of isophorone diisocyanate, are warming up to 60-80 DEG C, are stirred with the speed of 100-400r/min Mix 1-2h;Then 6-7 part diacetylmonoximes are added, 65-75 DEG C at a temperature of keep the temperature 2-3h, after 1-3 parts of ethylenediamines of addition, with The speed of 6000-7000r/min stirs 20-40min, obtains crosslinking agent.
By using above-mentioned technical proposal, the addition of crosslinking agent can not only add floride-free spill resistant agent and bleeding agent effective In conjunction with the permeance property of the floride-free water-proof aagent of raising allows it quickly to sprawl film forming in fiber surface, fiber is effectively reduced The coefficient of friction on surface, improves the waterproof performance of fabric, while crosslinking agent can also be with the hydroxyl that contains in dacron Reaction, keeps the combination of floride-free water-proof aagent and fiber stronger, to improve the washing fastness of floride-free water-proof aagent.
It further, further include 1-2 parts of waterproof synergistic agents, the waterproof synergistic agent is prepared with the following method: with weight Number meter, by 0-20 parts of silica 1,3-5 parts of surfactant, 2-4 parts of methacrylic acid octadecane alcohol ester, the poly- second two of oleic acid 50-60 parts of emulsion dispersion 5-10min under conditions of supersonic frequency is 20-30KHz of 2-4 parts of alcohol dibasic acid esters and ethylene glycol, obtain Pre-emulsion;After 2-4 parts of silane coupling agent, 30-40 parts of hydroxy silicon oil mixing, pre-emulsion is added, is heated to 80-90 DEG C, After being dispersed with stirring 30-40min under the speed of 1000-2000r/min;After being cooled to 70-75 DEG C, after keeping the temperature 50-60min, obtain To waterproof synergistic agent.
By using above-mentioned technical proposal, after the waterproof synergistic agent and floride-free spill resistant agent cooperation of silicon-containing compound, It can be effectively reduced the surface tension of fabric, improve the waterproof performance of fabric.
Further, the surfactant is living by the nonionic surfactant and cationic surface that weight ratio is 3:1 Property agent mixes.
Further, the nonionic surfactant is fatty alcohol polyoxyethylene ether, ethoxylated dodecyl alcohol, dehydration One of sorbitan monostearate or theirs is compound;The cationic surfactant is hexadecyldimethyl benzyl ammonium chlorine Change ammonium, one of dodecyldimethyl ammonium oxide or theirs is compound.
By using above-mentioned technical proposal, fatty alcohol polyoxyethylene ether, ethoxylated dodecyl alcohol, anhydrosorbitol list Stearate has emulsification well, dispersion and permeance property, hexadecyldimethyl benzyl ammonium ammonium chloride, dodecyl dimethyl oxidation Ammonium has sterilization well, soft and certain emulsification and wettability, when the two is used cooperatively, is conducive to the emulsification of raw material And dispersion, the permeance property of waterproof synergistic agent can be improved, and make it have certain anti-microbial property, to improve fabric Antibacterial and mouldproof performance.
The second object of the present invention is to provide a kind of preparation method of floride-free water-proof aagent.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation method of free-floride water-proof aagent, includes the following steps:
Based on parts by weight, take 2-4 parts of floride-free spill resistant agent, 0.1-0.3 parts of crosslinking agent, 1-2 parts of bleeding agent, 1-2 parts of defoaming agent, 1-2 parts of waterproof synergistic agent and 45-55 parts of water are stirred 10-20min, it is whole to be obtained floride-free waterproof with the speed of 50-200r/min Manage agent.
The second object of the present invention is to provide a kind of application method of floride-free water-proof aagent.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of application method of free-floride water-proof aagent, includes the following steps:
(1) fabric is impregnated in floride-free water-proof aagent and carries out water-proof finish;Dipping temperature is 60-80 DEG C, and dip time is 1-2min;
(2) fabric after dipping is subjected to padding machine roll compacting;Padding machine pressure is 3-4kg/cm2
(3) it repeats step (1) and step (2), carrying out second dipping and rolling to pick-up is 70-80%;Then by fabric carry out preliminary drying, It bakes and washing is dried.
Further, preliminary drying temperature is 75-95 DEG C in step (3), dry 10-20min;Stoving temperature is 160-180 DEG C At a temperature of, dry 5-10min;Washing drying refers to by fabric after washing, places it at a temperature of 60-70 DEG C, dry 5-15min。
By using above-mentioned technical proposal, fabric is first passed through into low temperature preliminary drying, can prevent finishing agent quickly to fabric table Face migration and influence the washing fastness arranged, under conditions of 160-180 DEG C, floride-free water-proof aagent and fiber can be made to send out Raw cross-linking reaction, to improve the waterproofness and washability of fabric.
In conclusion the present invention has the advantages that compared with the prior art
1. floride-free spill resistant agent has the characteristic of low surface property, there is excellent water repellency, by itself and crosslinking agent, bleeding agent And defoaming agent cooperation floride-free spill resistant agent obtained can quickly sprawl film forming in fiber surface, and fiber surface is effectively reduced Coefficient of friction improves the waterproof performance of fabric;
2. the addition of crosslinking agent can not only add floride-free spill resistant agent to be effectively combined with bleeding agent, floride-free water-proof aagent is improved Permeance property, so that it is quickly sprawled film forming in fiber surface, be effectively reduced the coefficient of friction of fiber surface, improve fiber The waterproof performance of fabric, while crosslinking agent can also be reacted with the hydroxyl contained in dacron, make floride-free water-proof aagent with The combination of fiber is stronger, to improve the washing fastness of floride-free water-proof aagent;
3. the surface of fabric can be effectively reduced after the waterproof synergistic agent and floride-free spill resistant agent cooperation of silicon-containing compound Tension improves the waterproof performance of fabric;Fatty alcohol polyoxyethylene ether, ethoxylated dodecyl alcohol, anhydrosorbitol list are stearic Acid esters has emulsification well, dispersion and permeance property, hexadecyldimethyl benzyl ammonium ammonium chloride, dodecyldimethyl ammonium oxide tool There are sterilization well, soft and certain emulsification and wettability, when the two is used cooperatively, is conducive to the emulsification of raw material and divides It dissipates, the permeance property of floride-free spill resistant agent can be improved, and make it have certain anti-microbial property, to improve the anti-of fabric Bacterium fungicidal properties.
Specific embodiment
Invention is further described in detail below.
One, 4kg dihydromethyl propionic acid, 4kg ethylene glycol and 30kg the preparation example 1 of the preparation example crosslinking agent of crosslinking agent: are taken Isophorone diisocyanate is warming up to 60 DEG C, stirs 1h with the speed of 100r/min;Then 6kg diacetylmonoxime is added, at 65 DEG C At a temperature of keep the temperature 2h, after 1kg ethylenediamine is added, 20min is stirred with the speed of 6000r/min, obtains crosslinking agent.
The preparation example 2 of crosslinking agent: 5kg dihydromethyl propionic acid, 5kg ethylene glycol and 35kg isophorone diisocyanate are taken Ester is warming up to 70 DEG C, stirs 1.5h with the speed of 200r/min;Then be added 6.5kg diacetylmonoxime, 70 DEG C at a temperature of keep the temperature 2.5h after 2kg ethylenediamine is added, stirs 30min with the speed of 6500r/min, obtains crosslinking agent.
The preparation example 3 of crosslinking agent: 6kg dihydromethyl propionic acid, 6kg ethylene glycol and 40kg isophorone diisocyanate are taken Ester is warming up to 80 DEG C, stirs 2h with the speed of 400r/min;Then be added 7kg diacetylmonoxime, 75 DEG C at a temperature of keep the temperature 3h, After 3kg ethylenediamine is added, 40min is stirred with the speed of 7000r/min, obtains crosslinking agent.
Two, the hydroxy silicon oil in the following preparation example of the preparation example of waterproof synergistic agent is selected from the model PMX- that DOW CORNING provides 0156 hydroxy silicon oil.
The preparation example 1 of waterproof synergistic agent: by silica 1 0kg, fatty alcohol polyoxyethylene ether 2.25kg, cetyl two Ammonio methacrylate 0.75kg, methacrylic acid octadecane alcohol ester 2kg, oleic acid polyethylene glycol dibasic acid esters 2kg and ethylene glycol 50kg exist Supersonic frequency is emulsion dispersion 5min under conditions of 20KHz, obtains pre-emulsion;By silane coupling agent KH560 2kg, hydroxyl silicon After oily 30kg mixing, pre-emulsion is added, 80 DEG C are heated to, after being dispersed with stirring 30min under the speed of 1000r/min;Cooling To after 70 DEG C, after keeping the temperature 50min, waterproof synergistic agent is obtained.
The preparation example 2 of waterproof synergistic agent: by silica 1 5kg, ethoxylated dodecyl alcohol 3kg, dodecyl dimethyl Amine-oxides 1kg, methacrylic acid octadecane alcohol ester 3g, oleic acid polyethylene glycol dibasic acid esters 3kg and ethylene glycol 55kg are in supersonic frequency For emulsion dispersion 8min under conditions of 25KHz, pre-emulsion is obtained;Silane coupling agent KH560 3kg, hydroxy silicon oil 35kg are mixed After conjunction, pre-emulsion is added, 85 DEG C are heated to, after being dispersed with stirring 35min under the speed of 1500r/min;After being cooled to 73 DEG C, After keeping the temperature 55min, waterproof synergistic agent is obtained.
The preparation example 3 of waterproof synergistic agent: by silica 20kg, sorbitan monosterate 3.75kg, 12 Alkyl dimethylamine oxides ammonium 1.25kg, methacrylic acid octadecane alcohol ester 4kg, oleic acid polyethylene glycol dibasic acid esters 4kg and ethylene glycol 60kg emulsion dispersion 10min under conditions of supersonic frequency is 30KHz, obtains pre-emulsion;By silane coupling agent KH560 After 4kg, hydroxy silicon oil 40kg mixing, pre-emulsion is added, is heated to 90 DEG C, is dispersed with stirring under the speed of 2000r/min After 40min;After being cooled to 75 DEG C, after keeping the temperature 60min, waterproof synergistic agent is obtained.
Three, the floride-free spill resistant agent in embodiment following embodiment includes fatty alcohol polyoxyethylene ether, CAS 68002- 97-1, the product of the model KW-802B provided selected from Guangzhou liberal-mindedness and vigorous endurance Science and Technology Ltd.;Bleeding agent is α-isotridecyl- ω-hydroxyl-is poly- (oxygen -1,2- ethylidene), CAS 9043305;Defoaming agent is oleic acid polyethylene glycol dibasic acid esters, CAS 9005-07- 6。
Embodiment 1: it is a kind of free-floride water-proof aagent be prepared with the following method:
Floride-free spill resistant agent 2kg, crosslinking agent 0.1kg, bleeding agent 1kg, defoaming agent 1kg and water 45kg are taken, with the speed of 50r/min Degree stirs 10min, obtains floride-free water-proof aagent;The preparation example 1 that wherein crosslinking agent is selected from crosslinking agent is prepared.
Embodiment 2: it is a kind of free-floride water-proof aagent be prepared with the following method:
Floride-free spill resistant agent 3kg, crosslinking agent 0.2kg, bleeding agent 1.5kg, defoaming agent 1.5kg and water 50kg are taken, with 100r/ The speed of min stirs 15min, obtains floride-free water-proof aagent;The preparation example 2 that wherein crosslinking agent is selected from crosslinking agent is prepared.
Embodiment 3: it is a kind of free-floride water-proof aagent be prepared with the following method:
Floride-free spill resistant agent 4kg, crosslinking agent 0.3kg, bleeding agent 2kg, defoaming agent 2kg and water 55kg are taken, with 200r/min's Speed stirs 20min, obtains floride-free water-proof aagent;The preparation example 3 that wherein crosslinking agent is selected from crosslinking agent is prepared.
Embodiment 4: the present embodiment difference from example 1 is that, further include 1kg in raw material by waterproof synergistic agent Waterproof synergistic agent prepared by preparation example 1.
Embodiment 5: the present embodiment difference from example 1 is that, further include 1.5kg in raw material by waterproof synergistic agent Preparation example 2 prepare waterproof synergistic agent.
Embodiment 6: the present embodiment difference from example 1 is that, further include 2kg in raw material by waterproof synergistic agent Waterproof synergistic agent prepared by preparation example 3.
Four, application examples application examples 1: a kind of application method of free-floride water-proof aagent includes the following steps:
(1) fabric being impregnated in floride-free water-proof aagent (selected from embodiment 1) and carries out water-proof finish, dipping temperature is 60 DEG C, Dip time is 1min;
(2) fabric after dipping is subjected to padding machine roll compacting, padding machine pressure is 3kg/cm2
(3) it repeats step (1) and step (2), carrying out second dipping and rolling to pick-up is 70%;Then fabric is subjected to preliminary drying, dried Roasting and washing drying, preliminary drying temperature are 75 DEG C, dry 10min;At a temperature of stoving temperature is 160 DEG C, dry 5min;Washing Drying refers to by fabric after washing, places it at a temperature of 60 DEG C, dry 5min.
Application examples 2: a kind of application method of free-floride water-proof aagent includes the following steps:
(1) fabric being impregnated in floride-free water-proof aagent (selected from embodiment 2) and carries out water-proof finish, dipping temperature is 70 DEG C, Dip time is 1.5min;
(2) fabric after dipping is subjected to padding machine roll compacting, padding machine pressure is 3.5kg/cm2
(3) it repeats step (1) and step (2), carrying out second dipping and rolling to pick-up is 75%;Then fabric is subjected to preliminary drying, dried Roasting and washing drying, preliminary drying temperature are 80 DEG C, dry 15min;At a temperature of stoving temperature is 170 DEG C, dry 8min;Washing Drying refers to by fabric after washing, places it at a temperature of 65 DEG C, dry 10min.
Application examples 3: a kind of application method of free-floride water-proof aagent includes the following steps:
(1) fabric being impregnated in floride-free water-proof aagent (selected from embodiment 3) and carries out water-proof finish, dipping temperature is 80 DEG C, Dip time is 2min;
(2) fabric after dipping is subjected to padding machine roll compacting, padding machine pressure is 4kg/cm2
(3) it repeats step (1) and step (2), carrying out second dipping and rolling to pick-up is 80%;Then fabric is subjected to preliminary drying, dried Roasting and washing drying, preliminary drying temperature are 95 DEG C, dry 20min;At a temperature of stoving temperature is 180 DEG C, dry -10min;Water It washes drying to refer to by fabric after washing, place it at a temperature of 70 DEG C, dry 5-15min.
Application examples 4: the application example and application examples 1 the difference is that, floride-free water-proof aagent is selected from the preparation of embodiment 4 And it obtains.
Application examples 5: the application example and application examples 1 the difference is that, floride-free water-proof aagent is selected from the preparation of embodiment 5 And it obtains.
Application examples 6: the application example and application examples 1 the difference is that, floride-free water-proof aagent is selected from the preparation of embodiment 6 And it obtains.
Five, comparative example comparative example 1: this comparative example difference from example 1 is that, crosslinking agent in raw material is selected from wide The bridging agent DM-3918 that U.S. fine chemistry industry Group Plc, East Germany provides.
Comparative example 2: this comparative example difference from example 1 is that, in raw material do not include bleeding agent α-different tridecane Base-ω-hydroxyl-is poly- (oxygen -1,2- ethylidene).
Comparative example 3: this comparative example and embodiment 4 the difference is that, the crosslinking agent in raw material is selected from Guangdong dolantin essence Refine the bridging agent DM-3918 that work Group Plc provides.
Six, reference examples reference examples 1: this reference examples and application examples 1 the difference is that, floride-free water-proof aagent using pair Ratio 1 is made.
Reference examples 2: this reference examples and application examples 1 the difference is that, floride-free water-proof aagent is using the system of comparative example 2 .
Reference examples 3: this reference examples and application examples 4 the difference is that, floride-free water-proof aagent is using the system of comparative example 3 .
Seven, the method that performance test is respectively adopted in application examples 1-6 and reference examples 1-3 processes fabric, obtains Sample as follows tests the performance of fabric, and test result is shown in table 1.
Waterproof performance: it is tested according to AATCC 22-2017 " refusing performance test-spray process ", grade 0-100,0 is Two sides is completely wet in table, and 100 be that surface does not soak or water droplet adheres to;After fabric washing 20 times, according to the method described above, then Secondary its water repellency of test, washing procedure: 27 DEG C, conventional wash, hang airing.
Table 1
According to 1 data of table, knitting for the floride-free water-proof aagent processing prepared using embodiment 1-3 can be seen that from application examples 1-3 Object has good waterproof performance, there is preferable water-fastness secured performance after washing 20 times;The nothing prepared using embodiment 4-6 The processing of fluorine water-proof aagent has excellent waterproof performance, and waterproof performance only has reduction more by a small margin after washing 20 times, Illustrate that the addition of the waterproof synergistic agent in embodiment 4-5 not only facilitates raising waterproof performance, also contributes to improve water-fast Wash secured performance.
The crosslinking agent in floride-free water-proof aagent in reference examples 1 is conventional cross-linking agent, compared to application examples 1, fabric Waterproof performance after waterproof performance and washing is declined, and illustrates that crosslinking agent prepared by the present invention can be obviously improved fabric Waterproof performance, be particularly useful to improve water-fastness secured performance.
Poly- (the Asia the oxygen -1,2- second of α-isotridecyl-ω-hydroxyl-is not included in floride-free water-proof aagent in reference examples 2 Base), compared to application examples 1, the waterproof performance and the waterproof performance after washing of fabric are declined slightly, and illustrate the different tridecane of α- The addition of base-ω-hydroxyl-poly- (oxygen -1,2- ethylidene) helps to improve the waterproof performance of floride-free water-proof aagent.
The crosslinking agent in floride-free water-proof aagent in reference examples 3 is conventional cross-linking agent, compared to application examples 4, fabric The waterproof performance and the waterproof performance after washing of waterproof fabric are declined, and illustrate crosslinking agent prepared by the present invention and waterproof It can be obviously improved the waterproof performance of fabric after synergist cooperation, be particularly useful to improve water-fastness secured performance.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this All by the protection of Patent Law in the scope of the claims of invention.

Claims (10)

1. a kind of free-floride water-proof aagent, it is characterised in that: based on parts by weight, including following component: floride-free spill resistant agent 2-4 Part, 0.1-0.3 parts of crosslinking agent, 1-2 parts of bleeding agent, 1-2 parts of defoaming agent and 45-55 parts of water;
The free-floride spill resistant agent includes fatty alcohol polyoxyethylene ether.
2. a kind of floride-free water-proof aagent according to claim 1, it is characterised in that: the bleeding agent is the different tridecane of α- Base-ω-hydroxyl-is poly- (oxygen -1,2- ethylidene).
3. a kind of floride-free water-proof aagent according to claim 1, it is characterised in that: the defoaming agent is the poly- second two of oleic acid Alcohol dibasic acid esters.
4. a kind of floride-free water-proof aagent according to claim 1, it is characterised in that: the crosslinking agent is with the following method Preparation: based on parts by weight, 4-6 parts of dihydromethyl propionic acids, 4-6 parts of ethylene glycol and 30-40 parts of isophorone diisocyanates are taken Ester is warming up to 60-80 DEG C, stirs 1-2h with the speed of 100-400r/min;Then 6-7 parts of diacetylmonoximes are added, at 65-75 DEG C At a temperature of keep the temperature 2-3h, after 1-3 part ethylenediamines are added, with the speed stirring 20-40min of 6000-7000r/min, be crosslinked Agent.
5. a kind of floride-free water-proof aagent according to claim 1, it is characterised in that: further include 1-2 parts of waterproof synergy Agent, the waterproof synergistic agent are prepared with the following method: based on parts by weight, by 0-20 parts of silica 1, surfactant 3- 5 parts, 2-4 parts of methacrylic acid octadecane alcohol ester and 50-60 parts of ethylene glycol creams under conditions of supersonic frequency is 20-30KHz Change dispersion 5-10min, obtains pre-emulsion;After 2-4 parts of silane coupling agent, 30-40 parts of hydroxy silicon oil mixing, pre-emulsification is added Liquid is heated to 80-90 DEG C, after being dispersed with stirring 30-40min under the speed of 1000-2000r/min;After being cooled to 70-75 DEG C, After keeping the temperature 50-60min, floride-free spill resistant agent is obtained.
6. a kind of floride-free water-proof aagent according to claim 5, it is characterised in that: the surfactant is by weight ratio It is mixed for the nonionic surfactant and cationic surfactant of 3:1.
7. a kind of floride-free water-proof aagent according to claim 6, it is characterised in that: the nonionic surfactant is One of fatty alcohol polyoxyethylene ether, ethoxylated dodecyl alcohol, sorbitan monosterate or theirs is compound; The cationic surfactant be one of hexadecyldimethyl benzyl ammonium ammonium chloride, dodecyldimethyl ammonium oxide or they It is compound.
8. a kind of preparation method of free-floride water-proof aagent, characterized by the following steps: based on parts by weight, take nothing 1-2 parts of 2-4 parts of fluorine spill resistant agent, 0.1-0.3 parts of crosslinking agent, 1-2 parts of bleeding agent, 1-2 parts of defoaming agent and waterproof synergistic agent, with And 45-55 parts of water, with the speed of 50-200r/min, 10-20min is stirred, floride-free water-proof aagent is obtained.
9. a kind of application method of free-floride water-proof aagent, characterized by the following steps:
(1) fabric is impregnated in floride-free water-proof aagent and carries out water-proof finish;Dipping temperature is 60-80 DEG C, and dip time is 1-2min;
(2) fabric after dipping is subjected to padding machine roll compacting;Padding machine pressure is 3-4kg/cm2
(3) it repeats step (1) and step (2), carrying out second dipping and rolling to pick-up is 70-80%;Then by fabric carry out preliminary drying, It bakes and washing is dried.
10. a kind of application method of floride-free water-proof aagent according to claim 9, it is characterised in that: pre- in step (3) Drying temperature is 75-95 DEG C, dry 10-20min;At a temperature of stoving temperature is 160-180 DEG C, dry 5-10min;Washing drying Refer to by fabric after washing, places it at a temperature of 60-70 DEG C, dry 5-15min.
CN201910819968.XA 2019-08-31 2019-08-31 A kind of free-floride water-proof aagent and its methods for making and using same Pending CN110409183A (en)

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CN112281493A (en) * 2020-11-16 2021-01-29 五邑大学 Fluoride-free waterproof finishing agent and preparation method thereof
CN112695525A (en) * 2020-12-28 2021-04-23 京准化工技术(上海)有限公司 Flame-retardant waterproof and oil-proof finishing agent and preparation method thereof
CN113430833A (en) * 2021-07-09 2021-09-24 福可新材料(上海)有限公司 Fluoride-free waterproof finishing liquid for ready-made clothes and application thereof
CN113564930A (en) * 2021-07-09 2021-10-29 福可新材料(上海)有限公司 Aqueous fluoride-free waterproof finishing liquid for all-cotton textiles and application thereof
CN113832716A (en) * 2021-09-24 2021-12-24 厦门海溢针纺织品有限公司 Production method of waterproof cloth, cloth and production method of cloth
CN114808455A (en) * 2022-05-19 2022-07-29 广州大学 Environment-friendly fluorine-free fabric waterproof moisture-permeable agent, preparation method and application
CN114892390A (en) * 2021-06-25 2022-08-12 上海九裕纺织科技有限公司 Water-splashing finishing agent and process applied to C0 water-splashing high index improvement

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CN112281493A (en) * 2020-11-16 2021-01-29 五邑大学 Fluoride-free waterproof finishing agent and preparation method thereof
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CN113564930A (en) * 2021-07-09 2021-10-29 福可新材料(上海)有限公司 Aqueous fluoride-free waterproof finishing liquid for all-cotton textiles and application thereof
CN113832716A (en) * 2021-09-24 2021-12-24 厦门海溢针纺织品有限公司 Production method of waterproof cloth, cloth and production method of cloth
CN114808455A (en) * 2022-05-19 2022-07-29 广州大学 Environment-friendly fluorine-free fabric waterproof moisture-permeable agent, preparation method and application
CN114808455B (en) * 2022-05-19 2023-05-05 广州大学 Environment-friendly fluorine-free fabric waterproof moisture permeable agent, preparation method and application

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