CN110042661A - Finishing agent composition, finishing agent and its preparation method and application - Google Patents
Finishing agent composition, finishing agent and its preparation method and application Download PDFInfo
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- CN110042661A CN110042661A CN201910222468.8A CN201910222468A CN110042661A CN 110042661 A CN110042661 A CN 110042661A CN 201910222468 A CN201910222468 A CN 201910222468A CN 110042661 A CN110042661 A CN 110042661A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
- D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
- D06M15/29—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides containing a N-methylol group or an etherified N-methylol group; containing a N-aminomethylene group; containing a N-sulfidomethylene group
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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- D06M2200/10—Repellency against liquids
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Abstract
The present invention relates to fabric functional finishing agent technical field, a kind of finishing agent composition, finishing agent and its preparation method and application are provided.In terms of mass parts, the finishing agent composition includes 40~60 parts of three-proof finishing agents, 20~40 parts of acrylate containing silicone copolymer emulsions, 20~25 parts of tripropylene glycols, 2~5 parts of water-soluble silicon oils, 1~3 part of hydroxymethyl cellulose and 1~10 part of blocked isocyanate, the blocked isocyanate plays a significant role in balance waterproof and easy dirt-removing functions, the method for preparing the finishing agent are as follows: first dissolve hydroxymethyl cellulose, then water-soluble silicon oil and tripropylene glycol are sequentially added, three-proof finishing agent and acrylate containing silicone copolymer emulsion are added after stirring 15~25min at 50~55 DEG C, 15~25min of blocked isocyanate stirring is added after continuing 5~20min of stirring.The finishing agent compatibility is good, which is applied to textile finishing processes, the baking temperature needed is low, reduces production cost, and obtained fabric is washable and is provided simultaneously with excellent waterproof and easy dirt-removing functions.
Description
Technical field
The present invention relates to fabric functional finishing agent technical fields, more specifically, be related to it is a kind of efficiently washable waterproof easily go
Dirty finishing agent composition, the preparation method and application comprising the finishing agent of the composition and the finishing agent.
Background technique
Existing fabric functional finishing agent still has following problems and needs to solve: first is that existing easy detergent makes fabric
With certain hydrophily, to make water-proof finish and soil-releasing finiss, there are certain paradoxes, meet one of condition
While necessarily sacrifice another condition, so there are water repellent, easy clean effect are poor, the low problem of grade causes to be difficult to meet
The demand of high-end market；Second is that excellent waterproof and easy clean effect can not be possessed simultaneously in existing technical solution, one
As be all have extraordinary soil release performance can and general waterproof performance, meanwhile, washable effect is also not outstanding enough.Third is that existing
The baking temperature of waterproof soil-releasing finishing agent is 160~180 DEG C in some technical solutions, and the too high fabric of temperature, which can turn to be yellow, to be hardened,
Power consumption is big simultaneously, shortens the service life of equipment, increases production cost.
Summary of the invention
The present invention provides a kind of efficiently washable waterproof soil-releasing finishing agent composition and include the finishing agent of the composition
And preparation method thereof, while the finishing agent is used for fabric, washable waterproof easy-to-remove-dirt fabric is prepared, to solve existing finishing agent
After handling fabric, fabric cannot keep excellent soil release performance energy, waterproof performance and washing fastness problem and existing whole simultaneously
Reason agent is required to higher baking temperature problem.
In order to solve the above-mentioned technical problem, first aspect present invention provides a kind of efficiently washable waterproof soil-releasing finishing agent
Composition, in terms of mass parts, the composition includes: 40~60 parts of three-proof finishing agents, 20~25 parts of acrylate containing silicone copolymerization
Lotion, 20~40 parts of tripropylene glycols, 2~5 parts of water-soluble silicon oils, 1~3 part of hydroxymethyl cellulose and 1~10 part of enclosed type isocyanide
Acid esters.
Preferably, the synthetic method of the blocked isocyanate includes the following steps:
SA1 dissolves hydrophilic modifier to obtain the solution one that the mass fraction of hydrophilic modifier is 15~25%；
The solution one is added and contains in annular aliphatic or aromatic diisocyanate under a shielding gas by SA2,
65~75 DEG C of reaction 110~130min are continuously heating to after reacting 30~50min at 40~50 DEG C, it is pre- to obtain isocyanates
Aggressiveness.
SA3 blocks the Isocyanate prepolymers body using end-capping reagent, to obtain the blocked isocyanate.
It is highly preferred that annular aliphatic or the aromatic diisocyanate of containing is isoflurane chalcone diisocyanate, first
The combination of any one or more in phenylene diisocyanate, '-diphenylmethane diisocyanate or naphthalene diisocyanate；And/or
The end-capping reagent is selected from sodium hydrogensulfite, methyl ethyl ketone oxime, sodium pyrosulfate, sodium peroxydisulfate, phenol, cresols, second
The combination of any one or more in acyl acetone, malonic acid diethyl vinegar, isopropyl alcohol or Malaysia acid imide；And/or
The hydrophilic modifier is selected from polyethylene glycol, poly glycol monomethyl ether, polyoxypropyleneglycol, polypropylene oxide three
Alcohol, orthoformic acid, ethylene glycol, propylene glycol, butanediol category, pentanediol class, hexylene glycol class, glycerol, pentaerythrite, sorbierite,
The combination of any one or more in neopentyl glycol, bisphenol-A or Xylene glycol；And/or
The mass fraction of free NCO is 5~10% in the Isocyanate prepolymers body.
Preferably, the preparation method of the three-proof finishing agent includes the following steps:
SB1 weighs 50~60 parts of perfluoro hexyl ethyl methyl acrylates, 25~35 parts of long-chain acrylic acid in terms of mass parts
Ester monomer, 20~30 parts containing cricoid acrylate monomer, the acrylate cross linked monomer of 3~7 parts of hydroxyls, 15~20 parts partially
Dichloroethylene, 1~3 part of cetyl trimethylammonium bromide, 4~10 parts of alcohol ethers emulsifiers, 2~5 parts of Tween 80s, 30~40 parts
Polyethylene glycol 400,0.1~0.5 part of lauryl mercaptan and 200~250 parts of deionized waters, obtain mixture one after mixing；
The temperature of the mixture one is risen to 50~60 DEG C and is stirred, after mixing evenly in 30~50MPa by SB2
Pressure under 5~10min of homogeneous, be warming up to 65~67 DEG C again after homogeneous, 0.5~1 part of initiator one be then added, continues to heat up
To 70~72 DEG C of 4~6h of reaction, to obtain the three-proof finishing agent.
It is highly preferred that the long chain acrylic ester monomer is selected from dodecyl acrylate, octadecyl acrylate, acrylic acid 20
The combination of any one or more in diester or isodecyl methacrylate；And/or
It is described to be selected from cyclohexyl methacrylate, benzyl methacrylate or methyl-prop containing cricoid acrylate monomer
The combination of any one or more in olefin(e) acid isobornyl thiocyanoacetate；And/or
The acrylate cross linked monomer of the hydroxyl is selected from N hydroxymethyl acrylamide, hydroxyethyl methacrylate or first
The combination of any one or more in base hydroxypropyl acrylate；And/or
The initiator one is selected from V-50, benzoyl peroxide, lauroyl peroxide, tert-butyl peroxide, hydrogen peroxide
Change cumene, tert-butyl hydroperoxide neopentanoic acid, diisopropyl peroxydicarbonate, t-butyl perbenzoate, 1- hydroxy cyclohexylphenyl
Any one in base hydroperoxides, 3- carbonyl propiony peroxide or acetyl peroxide.
Preferably, the preparation method of the acrylate containing silicone copolymer emulsion includes the following steps:
SC1 weighs 20~30 parts of methacrylic acids, 5~15 parts of hydroxy-ethyl acrylates, 25~35 parts of first in terms of mass parts
Base butyl acrylate, 3~7 parts of vinyl-functional dimethyl silicone polymers, 15~25 parts of polyethylene glycol 400s, 60~140 parts go
Ionized water, 2~5 parts of cetyl trimethylammonium bromides, 2~5 parts of Tween 80s and 2~5 parts of fatty alcohol polyoxyethylene ether AEO-9,
Mixture two is obtained after mixing；
The temperature of the mixture two is risen to 50~60 DEG C and is stirred, after mixing evenly in 30~50MPa by SC2
Pressure under 5~10min of homogeneous, be warming up to 65~67 DEG C again after homogeneous, 0.3~0.8 part of initiator two be then added, after of continuing rising
Temperature is to 70~72 DEG C of 4~6h of reaction, to obtain the acrylate containing silicone copolymer emulsion；Wherein, the initiator two is selected from V-
50, benzoyl peroxide, lauroyl peroxide, tert-butyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide neopentanoic acid,
Diisopropyl peroxydicarbonate, t-butyl perbenzoate, 1- hydroxy-cyclohexyl hydroperoxides, 3- carbonyl propiono mistake
Any one in oxide or acetyl peroxide.
Second aspect of the present invention provides a kind of efficiently washable waterproof soil-releasing finishing agent, and the efficiently washable waterproof is easily gone
Dirty finishing agent includes above-mentioned efficient washable waterproof soil-releasing finishing agent composition and solvent.
Third aspect present invention provides a kind of method for preparing above-mentioned efficiently washable waterproof soil-releasing finishing agent, the side
Method includes the following steps:
SD1 dissolves the hydroxymethyl cellulose with solvent, then sequentially adds water into dissolved hydroxymethyl cellulose
Dissolubility silicone oil and tripropylene glycol obtain mixture three after being warming up to 50~55 DEG C of 15~25min of stirring；
The three-proof finishing agent and the acrylate containing silicone copolymer emulsion are added in SD2, Xiang Suoshu mixture three, continues
Mixture four is obtained after stirring 5~20min at 50~55 DEG C；
Blocked isocyanate is added in SD3, Xiang Suoshu mixture four, continues to stir 15~25min at 50~55 DEG C
After obtain it is described efficiently washable waterproof soil-releasing finishing agent.
Fourth aspect present invention provides a kind of preparation method of washable waterproof easy-to-remove-dirt fabric, and the method includes as follows
Step:
Fabric to be processed is immersed in above-mentioned efficient washable waterproof soil-releasing finishing agent by SE1, and two leaching two bundles are rolled
Remaining rate is 70~75%；
SE2, by the fabric after two leaching two bundles at a temperature of 80~100 DEG C 15~20min of preliminary drying, then in 110~120 DEG C of temperature
Degree is lower to bake 10~15min, and washable waterproof easy-to-remove-dirt fabric can be obtained.
Fifth aspect present invention provides a kind of washable waterproof easy-to-remove-dirt fabric, and the fabric uses above-mentioned preparation method system
?.
Compared with prior art, the invention has the advantages that and effect:
1, in finishing agent composition provided by the invention and finishing agent comprising the composition, used enclosed type is different
Cyanate has lower deblocking temperature, can hand over the effective component of three-proof finishing agent and acrylate containing silicone copolymer emulsion
Connection gets up, and promotes the combination of these effective components and face liber molecule at 80~100 DEG C, to form sky in fabric surface
Between network structure, so that the contradiction between waterproof and soil release performance energy is balanced, so that waterproof, soil release performance can be good at opening up
Reveal and, and the flexibility of fabric can be increased, economic value with higher.
2, the finishing agent composition provided by the invention comprising above-mentioned crosslinking agent and the finishing agent application comprising the composition
In textile finishing processes, one layer of protective film can be formed on the surface of fabric, significantly reduce its surface tension, can significantly mention
The hydrophily of high fabric in water, so that dirt can be removed easily from fiber surface in washing process, to show
The easy dirt-removing functions of excellent waterproof out.
3, efficiently washable waterproof soil-releasing finishing agent provided by the invention, compatibility is good, can be with softening agent, bleeding agent and anti-
The textile auxiliaries such as electrostatic agent are used cooperatively, and without influencing original performance, and preparation method is simple, and the process conditions needed are easy
It realizes, is conducive to industrialized production, there is high economic benefit.
4, it is further provided the present invention is based on above-mentioned efficiently washable waterproof soil-releasing finishing agent and prepares washable waterproof and easily go
The method of dirty fabric can toast under cryogenic when handling fabric, it will be able to keep fabric that there is efficient washable waterproof to go
Dirty performance avoids fabric xanthochromia due to high-temperature baking, while extending the service life of equipment, reduces production cost.This
Invention further provides the washable waterproof easy-to-remove-dirt fabric obtained based on the preparation method, the washable waterproof easy-to-remove-dirt fabric
Washing fastness can be promoted to 50 times or more, and the fabric still has more excellent Water-proof and oil-proof after 50 times are washed repeatedly
With easy dirt-removing functions and flexibility is good, white coefficient is high effect.
Specific embodiment
In order to keep the narration of this disclosure more detailed with it is complete, below for embodiments of the present invention and specific real
It applies example and proposes illustrative description；But this not implements or uses the unique forms of the specific embodiment of the invention.Embodiment
In cover multiple specific embodiments feature and to construction with operate these specific embodiments method and step it is suitable with it
Sequence.However, can also reach identical or impartial function and sequence of steps using other specific embodiments.
Existing finishing agent cannot possess excellent waterproof performance and soil release performance energy, therefore, first party of the present invention simultaneously
Face provides a kind of blocked isocyanate, to balance the contradiction in finishing agent between waterproof performance and soil release performance energy, the envelope
The synthetic method of closed form isocyanates includes: first using hydrophilic modifier and the diisocyanate containing annular aliphatic or containing fragrance
Then the diisocyanate synthesizing isocyanate performed polymer of race blocks the Isocyanate prepolymers body using end-capping reagent, with
Obtain the blocked isocyanate.In some embodiments of the invention, the method for synthesizing isocyanate performed polymer specifically includes:
Hydrophilic modifier first is dissolved with solvent, to obtain the solution one that the mass fraction of hydrophilic modifier is 15~25%, is then being protected
It protects under gas, according to solution one: containing annular aliphatic or contain aromatic diisocyanate=(10~15): 1 ratio will be molten
Liquid one is added containing annular aliphatic or containing in aromatic diisocyanate, after completion of dropwise addition at 40~50 DEG C reaction 30~
50min, preferably 35~45min are continuously heating to 65~75 DEG C of reactions 110~130min, preferably 115~125min, finally drop
It discharges when temperature is to 45 DEG C and following temperature, to obtain Isocyanate prepolymers body, in this step, needs through hydrophilic modifier control
The mass fraction of the free NCO group of system so that system keeps homogeneous, will not be layered, viscosity is suitable 5~10% after standing
In, gel will not occur.
The process for preparing Isocyanate prepolymers body needs to carry out under agitation, according to some embodiments of the present invention,
It is first put into there-necked flask by a certain amount of containing annular aliphatic or containing aromatic diisocyanate, and starts blender, then
Solution one is slowly instilled by dropping funel while stirring containing annular aliphatic or containing in aromatic diisocyanate, is being dripped
It fills protective gas while solubilization liquid one to be protected, in the present invention it is possible to select any suitable protection gas in this field
Body, such as nitrogen after completion of dropwise addition, continue to stir, and carry out heating and polymerization reaction.In other embodiments of the invention
In, the solvent for dissolving the hydrophilic modifier is dehydrated alcohol；It prepares needed for Isocyanate prepolymers body containing annular aliphatic
Or containing aromatic diisocyanate is isoflurane chalcone diisocyanate, toluene di-isocyanate(TDI), '-diphenylmethane diisocyanate
Or the combination of any one or more in naphthalene diisocyanate；And the hydrophilic modifier used can be polyalcohol, polyalcohols
It is polyethylene glycol, poly glycol monomethyl ether, polyoxypropyleneglycol, polypropylene oxide with polyethers alcohols, such as hydrophilic modifier
Triol, orthoformic acid, ethylene glycol, propylene glycol, butanediol category, pentanediol class, hexylene glycol class, glycerol, pentaerythrite, sorb
The combination of any one or more in alcohol, neopentyl glycol, bisphenol-A or Xylene glycol uses in some preferred embodiments
Hydrophilic modifier be polyethylene glycol or orthoformic acid.
In other embodiments of the invention, the step of Isocyanate prepolymers body is blocked using end-capping reagent tool
Body includes: first to dissolve end-capping reagent with solvent, to obtain the solution two that the mass fraction of end-capping reagent is 25~35%；According still further to quality
Than for (1~3): 1 ratio respectively puts into Isocyanate prepolymers body and ethyl alcohol in there-necked flask, starts blender, then side is stirred
Side is mixed slowly to instill solution two in there-necked flask by dropping funel, according to some embodiments of the present invention, the addition of solution two
Amount is the 25~45% of the mixture quality formed after above-mentioned Isocyanate prepolymers body and ethyl alcohol mixing, reacts 2 after completion of dropwise addition
~3h, can be obtained blocked isocyanate.According to some embodiments of the present invention, the end-capping reagent used is selected from bisulfite
Sodium, methyl ethyl ketone oxime, sodium pyrosulfate, sodium peroxydisulfate, phenol, cresols, acetylacetone,2,4-pentanedione, malonic acid diethyl vinegar, isopropyl alcohol
Or the combination of any one or more in the acid imide of Malaysia, the solvent for dissolving end-capping reagent are deionized water or anhydrous second
Alcohol；In some preferred embodiments, the end-capping reagent used be the inorganic acids with lower dissociation temperature, as sodium hydrogensulfite,
Sodium peroxydisulfate etc., using the inorganic acids end-capping reagent prepare blocked isocyanate at a lower temperature, such as 80 DEG C of energy
Enough promote the combination of the effective component and fabric fibre molecule in finishing agent so that fabric have excellent washable, waterproof,
Easy dirt-removing functions.And the solvent for dissolving the inorganic acids end-capping reagent is deionized water, being compared to dehydrated alcohol can save
About preparation cost.
Based on the blocked isocyanate of above-mentioned synthesis, second aspect of the present invention provide it is a kind of efficiently washable waterproof easily go
Dirty finishing agent composition, in terms of mass parts, the composition includes: 40~60 parts of three-proof finishing agents, 20~40 parts of silyl acrylates
Ester copolymer emulsion, 20~25 parts of tripropylene glycols, 2~5 parts of water-soluble silicon oils, 1~3 part of hydroxymethyl cellulose and 1~10 part are above-mentioned
Blocked isocyanate.In the composition, three-proof finishing agent and acrylate containing silicone can be total to by blocked isocyanate
The effective component crosslinking of poly- lotion is got up, and promotes the combination of these effective components and face liber molecule at 80~100 DEG C,
To form spacial framework in fabric surface, to balance the contradiction between waterproof and soil release performance energy, so that waterproof, easily going
Dirt can be good at showing, and the crosslinking agent can also increase the flexibility of fabric, therefore warp with higher
Ji value.
According to some embodiments of the present invention, the three-proof finishing agent in the composition is prepared by the following procedure method and is made: with
Mass parts meter first weighs 50~60 parts of perfluoro hexyl ethyl methyl acrylates, 25~35 parts of long chain acrylic ester monomers, 20~30
Part containing cricoid acrylate monomer, the acrylate cross linked monomer of 3~7 parts of hydroxyls, 15~20 parts of vinylidene chlorides, 1~3
Part cetyl trimethylammonium bromide, 4~10 parts of alcohol ethers emulsifiers, 2~5 parts of Tween 80s, 30~40 parts of polyethylene glycol 400s,
0.1~0.5 part of lauryl mercaptan and 200~250 parts of deionized waters, obtain mixture one after mixing；Then by the mixture
One temperature rises to 50~60 DEG C and is stirred, after mixing evenly 5~10min of homogeneous, homogeneous under the pressure of 30~50MPa
It is warming up to 65~67 DEG C again afterwards, adds 0.5~1 part of initiator one, be continuously heating to 70~72 DEG C of 4~6h of reaction, can obtain
To the three-proof finishing agent.
In the preferred embodiment of the present invention, the three-proof finishing agent used is made by following methods: in terms of mass parts,
Successively weigh that 55 parts of perfluoro hexyl ethyl methyl acrylates, 30 parts of long chain acrylic ester monomers, 25 parts containing cricoid acrylate
Acrylate cross linked monomer, 18 parts of vinylidene chlorides, the 2 parts of cetyl trimethylammonium bromides, 3 parts of monomer, 5 parts of hydroxyls
Genifol 04L, 3 parts of Genifol, 307,3 parts of Tween 80s, 35 parts of polyethylene glycol 400s, 0.2 part of lauryl mercaptan and 220 parts
Deionized water is mixed in four-hole boiling flask；It then heats to 50~60 DEG C to stir evenly, then the homogeneous under the pressure of 40MPa
6min is warming up to 67 DEG C after homogeneous again, and 0.8 part of initiator one is added dropwise into the lotion after homogeneous by dropping funel, knot is added dropwise
Shu Hou is continuously heating to 70 DEG C of 4~6h of reaction, and the polymerized emulsion obtained after being cooled to room temperature is three-proof finishing agent.
Other embodiments according to the present invention, long chain acrylic ester monomer used in above-mentioned preparation method are selected from third
In alkene dodecyl gallate, octadecyl acrylate, Behenyl acrylate or isodecyl methacrylate any one or more
Combination；And cyclohexyl methacrylate, methyl are selected from containing cricoid acrylate monomer used in above-mentioned preparation method
The combination of any one or more in benzyl acrylate or isobornyl methacrylate；And institute in above-mentioned preparation method
The acrylate cross linked monomer of the hydroxyl used is selected from N hydroxymethyl acrylamide, hydroxyethyl methacrylate or metering system
The combination of any one or more in sour hydroxypropyl acrylate；And initiator one used in above-mentioned preparation method be selected from V-50,
It is benzoyl peroxide, lauroyl peroxide, tert-butyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide neopentanoic acid, two different
Peroxydicarbonate, t-butyl perbenzoate, 1- hydroxy-cyclohexyl hydroperoxides, 3- carbonyl propiono peroxidating
Any one in object or acetyl peroxide.In some preferred embodiments, long-chain third used in above-mentioned preparation method
Olefin(e) acid ester monomer is preferably octadecyl acrylate；It is preferably containing cricoid acrylate monomer used in above-mentioned preparation method
Benzyl methacrylate；The acrylate cross linked monomer N- methylol acryloyl of hydroxyl used in above-mentioned preparation method
Amine；Initiator one used in above-mentioned preparation method is V-50.
In some preferred embodiments, used three-proof finishing agent is HEC TA-5635F, is 6 carbon fluoropolymers
Lotion, solid content 30% are main to provide the waterproof performance of fabric；It is a kind of weak cation type three-proof finishing agent simultaneously, tool
There is very excellent compatibility, can be used cooperatively with textile auxiliaries such as softening agent, bleeding agent and antistatic agents, without influencing it
Waterproof performance.
According to some embodiments of the present invention, the acrylate containing silicone copolymer emulsion side of being prepared by the following procedure in the composition
Method is made: in terms of mass parts, successively weighing 20~30 parts of methacrylic acids, 5~15 parts of hydroxy-ethyl acrylates, 25~35 parts of methyl
Butyl acrylate, 3~7 parts of vinyl-functional dimethyl silicone polymers, 15~25 parts of polyethylene glycol 400s, 60~140 parts go from
Sub- water, 2~5 parts of cetyl trimethylammonium bromides, 2~5 parts of Tween 80s and 2~5 parts of fatty alcohol polyoxyethylene ether AEO-9 are mixed
Mixture two is obtained after conjunction；Then the temperature of the mixture two is risen to 50~60 DEG C and be stirred, after mixing evenly 30
5~10min of homogeneous under the pressure of~50MPa is warming up to 65~67 DEG C after homogeneous again, and 0.3~0.8 part of initiator is then added
Two, 70~72 DEG C of 4~6h of reaction are continuously heating to, after being cooled to room temperature, obtained polymerized emulsion is that acrylate containing silicone is total
Poly- lotion, Si-O-Si key, Si-C key and Si-O key are contained in the acrylate containing silicone copolymer emulsion, their bond energy is much larger than
The bond energy of C-O key, with the flexibility of height, excellent high and low temperature resistance, weatherability, water resistance and good ventilative
Property, substantially increase solvent resistance, resistant of high or low temperature and the durability in oxidative degradation energy of esters of acrylic acid.
In the preferred embodiment of the present invention, acrylate containing silicone copolymer emulsion is prepared by the following procedure method and is made: with
Mass parts meter successively weighs 25 parts of methacrylic acids, 10 parts of hydroxy-ethyl acrylates, 30 parts of butyl methacrylates, 5 parts of vinyl
Functionalized poly dimethyl siloxane, 20 parts of polyethylene glycol 400s, 70 parts of deionized waters, 3 parts of cetyl trimethylammonium bromides, 3 parts
Tween 80 and 3 parts of fatty alcohol polyoxyethylene ether AEO-9, mixing；It then heats to 50~60 DEG C to stir evenly, then 40MPa's
Homogeneous 6min under pressure is warming up to 67 DEG C after homogeneous again, and 0.5 part of initiator two is then added, be continuously heating to 70 DEG C of reactions 4~
6h, after being cooled to room temperature, obtained polymerized emulsion is acrylate containing silicone copolymer emulsion.
Other embodiments according to the present invention, initiator two used in above-mentioned preparation method are selected from V-50, peroxide
Change benzoyl, lauroyl peroxide, tert-butyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide neopentanoic acid, diisopropyl
Peroxy dicarbonate, t-butyl perbenzoate, 1- hydroxy-cyclohexyl hydroperoxides, 3- carbonyl propiony peroxide or
Any one in acetyl peroxide, preferably V-50.
Based on above-mentioned efficiently washable waterproof soil-releasing finishing agent composition, third aspect present invention provides a kind of efficiently resistance to
Waterproof soil-releasing finishing agent is washed, which contains the composition and solvent of above-mentioned introduction, some implementations according to the present invention
Mode, the solvent are deionized water, the solids or powder being mainly used in first dissolved composition or the certain ingredients of dilution it is dense
Degree, in order to mix with other compositions, the concentration for the finishing agent that dosage configures as needed is determined, in some embodiments,
In terms of mass parts, 30~40 parts of water have been used during preparing above-mentioned finishing agent.The finishing agent is applied to textile finishing
Process can form one layer of protective film on the surface of fabric, significantly reduce its surface tension, can significantly improve fabric and exist
Hydrophily in water, so that dirt can be removed easily from fiber surface in washing process, so that it is easy to show waterproof
Dirt-removing functions.
Further, fourth aspect present invention provides a kind of side for preparing above-mentioned efficiently washable waterproof soil-releasing finishing agent
Method, this method comprises: in terms of mass parts, successively weigh 40~60 parts of three-proof finishing agents prepared, 20~40 parts prepare
Acrylate containing silicone copolymer emulsion, 20~25 parts of tripropylene glycols, 2~5 parts of water-soluble silicon oils, 1~3 part of hydroxymethyl cellulose and 1
~10 parts of synthetic blocked isocyanates；Hydroxymethyl cellulose first is dissolved with solvent, after its dissolution, then to dissolved
Water-soluble silicon oil and tripropylene glycol are sequentially added in hydroxymethyl cellulose, are warming up to 50~55 DEG C of 15~25min of stirring, are preferably stirred
Mixture three is obtained after mixing 20min；Continue that three-proof finishing agent and acrylate containing silicone copolymer emulsion are added into the mixture three,
And 5~20min is stirred still at 50~55 DEG C, mixture four is obtained after preferably stirring 10min；It is further continued for into the mixture four
Blocked isocyanate is added, and stirs 15~25min still at 50~55 DEG C, preferably stirring 20min, is then cooled down to it,
Efficient washable waterproof soil-releasing finishing agent can be obtained.
Other embodiments according to the present invention, blocked isocyanate before addition, are first diluted it with solvent,
Such as 5 parts of blocked isocyanates are diluted using 10 parts of deionized waters.
Above-mentioned preparation method is simple, and the process conditions needed are easily realized, is conducive to industrialized production, has high economy
Benefit.Efficiently washable waterproof soil-releasing finishing agent obtained, compatibility is good, can spin with softening agent, bleeding agent and antistatic agent etc.
It knits auxiliary agent to be used cooperatively, without influencing original performance.
Efficient washable waterproof soil-releasing finishing agent based on above-mentioned offer is easily gone by the efficient washable waterproof of offer
The finishing agent that dirty finishing agent preparation method is prepared, fifth aspect present invention, which provides, a kind of to be prepared the easy decontamination of washable waterproof and knits
The method of object, this method are as follows: using technique is dipped, fabric to be processed is immersed in above-mentioned efficiently washable waterproof soil-releasing finiss
In agent, pick-up is 70~75%；Then by the fabric after dipping at a temperature of 80~100 DEG C 15~20min of preliminary drying, then
10~15min is baked at a temperature of 110~120 DEG C, and washable waterproof easy-to-remove-dirt fabric can be obtained.According to an embodiment of the invention,
The fabric that finishing agent provided by the invention can act on include pure cotton fabric, polyester-cotton fabric and other containing cotton blended fabric, pass through
Fabric after the finishing agent arranges all has excellent washable, waterproof, easy dirt-removing functions.In some currently preferred embodiments of the present invention
In, first weigh 10~20g this efficiently washable waterproof soil-releasing finishing agent is diluted in 1L water, then fabric to be processed is impregnated
Wherein, two leaching two bundles, pick-up 70%, then by the fabric after two leaching two bundles at a temperature of 80~100 DEG C preliminary drying 20min,
10~15min is finally baked at a temperature of 120 DEG C.The above method is to toast under cryogenic, fabric can not only be kept to have
There is efficient washable waterproof detergency ability, it is thus also avoided that fabric xanthochromia due to high-temperature baking, while the service life of equipment is extended,
Production cost is reduced, the washing fastness of fabric obtained can be promoted to 50 times or more, and should after 50 times are washed repeatedly
Fabric still has the effect of more excellent Water-proof and oil-proof and easy dirt-removing functions and flexibility is good, white coefficient is high.
Finally, sixth aspect present invention additionally provide it is a kind of using above-mentioned preparation method preparation the easy decontamination of washable waterproof knit
Object, the fabric are provided simultaneously with excellent washable, waterproof, easy dirt-removing functions.
In order to make the objectives, technical solutions, and advantages of the present invention clearer, combined with specific embodiments below to this
Invention is described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
It is of the invention in limiting.
Prepare aqueous silicon-acrylate copolymer emulsion
According to quality proportioning, by 25 parts of methacrylic acids, 10 parts of hydroxy-ethyl acrylates, 30 parts of butyl methacrylates, 5 parts
Vinyl-functional dimethyl silicone polymer, 20 parts of polyethylene glycol 400s, 135 parts of deionized waters, 3 parts of cetyl trimethyl bromines
Change ammonium, 3 parts of fatty alcohol polyoxyethylene ether AEO-9 and 3 parts of Tween 80s to be mixed in four-hole boiling flask, it is equal to be warming up to 50~60 DEG C of stirrings
Even, then the high-pressure homogeneous 6min of 40MPa, is warming up to 70 DEG C, and 0.5 part of initiator V-50 is added dropwise, and reacts 4~6h, is cooled to room temperature,
Obtain aqueous silicon-acrylate copolymer emulsion.
Prepare three-proof finishing agent HEC TA-5635F
According to mass ratio, by 55 parts of perfluoro hexyl ethyl methyl acrylates, 30 parts of octadecyl acrylates, 25 parts of metering systems
Sour benzyl ester, 5 parts of N hydroxymethyl acrylamides, 18 parts of vinylidene chlorides, 2 parts of cetyl trimethylammonium bromides, 3 parts
Genifol 04L (purchase is in Nanjing Lian Zhi Science and Technology Ltd.), 3 parts of Tween 80s, (purchase joins 3 parts of Genifol 307 in Nanjing
Intelligence Science and Technology Ltd.), 35 parts of polyethylene glycol 400s, 0.2 part of lauryl mercaptan and 220 parts of deionized waters be mixed in four mouthfuls of burnings
In bottle, it is warming up to 50-60 DEG C and stirs evenly, then the high-pressure homogeneous 6min of 40MPa, be warming up to 67 DEG C, it is water-soluble with 20 parts of deionizations
0.8 part of V-50 is solved, is then added dropwise by dropping funel into the lotion after homogeneous, after dripping, is warming up to 70 DEG C of reaction 4-6h,
It is cooled to room temperature, obtains polymerized emulsion.
Synthesize blocked isocyanate
Synthesis example 1
(1) ethanol solution that polyethylene glycol mass fraction is 20% is respectively configured and methyl ethyl ketone oxime mass fraction is
30% ethanol solution；
(2) 22.2g isoflurane chalcone diisocyanate is put into there-necked flask, blender is started, under nitrogen protection, while stirring
Mix side and overflow the ethanol solution for instilling 300g polyethylene glycol slowly by dropping funel, after dripping, stir and oil bath be warming up to 40~
50 DEG C of reaction 40min；It is warming up to 70 DEG C of reaction 120min again, obtains performed polymer, controlling its free NCO mass fraction is 8% left
It is right；
(3) by 20g performed polymer and 20g ethyl alcohol investment there-necked flask, blender is started, 11.6g methyl ethyl ketone oxime is molten
Liquid slowly instills wherein, and after reacting 3h, vacuum distillation removes ethyl alcohol, obtains blocked isocyanate A.
Synthesis example 2
(1) it is 30% that ethanol solution that polyethylene glycol mass fraction is 20% and sodium hydrogensulfite mass fraction, which is respectively configured,
Aqueous solution；
(2) 22.2g isoflurane chalcone diisocyanate is put into there-necked flask, blender is started, under nitrogen protection, while stirring
Mix side and overflow the ethanol solution for instilling 300g polyethylene glycol slowly by dropping funel, after dripping, stir and oil bath be warming up to 40~
50 DEG C of reaction 40min；It is warming up to 70 DEG C of reaction 120min again, obtains performed polymer, controlling its free NCO mass fraction is 8% left
It is right；
(3) by 20g performed polymer and 20g ethyl alcohol investment there-necked flask, blender is started, by 16g aqueous solution of sodium bisulfite
It slowly instills wherein, after reacting 3h, vacuum distillation removes ethyl alcohol, obtains blocked isocyanate B.
Synthesis example 3
(1) ethanol solution and methyl ethyl ketone oxime mass fraction that trimethylolpropane mass fraction is 20% is respectively configured
For 30% ethanol solution；
(2) 22.2g isoflurane chalcone diisocyanate is put into there-necked flask, blender is started, under nitrogen protection, while stirring
It mixes side and overflows the ethanol solution for instilling 300g trimethylolpropane slowly by dropping funel, after dripping, stir and oil bath is warming up to
40~50 DEG C of reaction 40min；It is warming up to 70 DEG C of reaction 120min again, obtains performed polymer, controlling its free NCO mass fraction is
8% or so；
(3) by 20g performed polymer and 20g ethyl alcohol investment there-necked flask, blender is started, 11.6g methyl ethyl ketone oxime is molten
Liquid slowly instills wherein, and after reacting 3h, vacuum distillation removes ethyl alcohol, obtains blocked isocyanate C.
Synthesis example 4
(1) ethanol solution that trimethylolpropane mass fraction is 20% is respectively configured and sodium hydrogensulfite mass fraction is
30% aqueous solution；
(2) 22.2g isoflurane chalcone diisocyanate is put into there-necked flask, blender is started, under nitrogen protection, while stirring
It mixes side and overflows the ethanol solution for instilling 300g trimethylolpropane slowly by dropping funel, after dripping, stir and oil bath is warming up to
40~50 DEG C of reaction 40min；It is warming up to 70 DEG C of reaction 120min again, obtains performed polymer, controlling its free NCO mass fraction is
8% or so；
(3) by 20g performed polymer and 20g ethyl alcohol investment there-necked flask, blender is started, by 16g aqueous solution of sodium bisulfite
It slowly instills wherein, after reacting 3h, vacuum distillation removes ethyl alcohol, obtains blocked isocyanate D.
Embodiment 1
2 parts of carboxymethyl celluloses are added in 22 parts of water, are stirred evenly, after sequentially add 5 parts of water-soluble silicon oils and 20 parts
Tripropylene glycol is warming up to 50~55 DEG C of stirring 20min, and 50 parts of HEC TA-5635F are added and 30 parts of aqueous silicon-acrylates are total
Poly- lotion, continues to stir 10min, dilutes 5 parts of blocked isocyanate A with 10 parts of deionized waters, the lotion before being then added
In, 20min is stirred, it is cooling to solution, efficient durable waterproof soil-releasing finishing agent can be obtained.
The above-mentioned finishing agent of 20g is diluted in the water of 1L, then wherein by pure cotton blended fabric dipping, second dipping and rolling,
Pick-up is 70%, then by fabric at a temperature of 100 DEG C preliminary drying 20min, then at a temperature of 120 DEG C bake 10~15min after
To product one.
Embodiment 2
2 parts of carboxymethyl celluloses are added in 22 parts of water, are stirred evenly, after sequentially add 5 parts of water-soluble silicon oils and 20 parts
Tripropylene glycol is warming up to 50~55 DEG C of stirring 20min, and 50 parts of HEC TA-5635F are added and 30 parts of aqueous silicon-acrylates are total
Poly- lotion, continues to stir 10min, dilutes 5 parts of blocked isocyanate B with 10 parts of deionized waters, the lotion before being then added
In, 20min is stirred, it is cooling to solution, efficient durable waterproof soil-releasing finishing agent can be obtained.
The above-mentioned finishing agent of 20g is diluted in the water of 1L, then wherein by pure cotton blended fabric dipping, second dipping and rolling,
Pick-up is 70%, then by fabric at a temperature of 80 DEG C preliminary drying 20min, then at a temperature of 120 DEG C bake 10~15min after obtain
Product two.
Embodiment 3
2 parts of carboxymethyl celluloses are added in 22 parts of water, are stirred evenly, after sequentially add 5 parts of water-soluble silicon oils and 20 parts
Tripropylene glycol is warming up to 50~55 DEG C of stirring 20min, and 50 parts of HEC TA-5635F are added and 30 parts of aqueous silicon-acrylates are total
Poly- lotion, continues to stir 10min, dilutes 5 parts of blocked isocyanate C with 10 parts of deionized waters, the lotion before being then added
In, 20min is stirred, it is cooling to solution, efficient durable waterproof soil-releasing finishing agent can be obtained.
The above-mentioned finishing agent of 20g is diluted in the water of 1L, then wherein by pure cotton blended fabric dipping, second dipping and rolling,
Pick-up is 70%, then by fabric at a temperature of 100 DEG C preliminary drying 20min, then at a temperature of 120 DEG C bake 10~15min after
To product three.
Embodiment 4
2 parts of carboxymethyl celluloses are added in 22 parts of water, are stirred evenly, after sequentially add 5 parts of water-soluble silicon oils and 20 parts
Tripropylene glycol is warming up to 50-55 DEG C of stirring 20min, and 50 parts of HEC TA-5635F are added and 30 parts of aqueous silicon-acrylates are total
Poly- lotion, continues to stir 10min, dilutes 5 parts of blocked isocyanate D with 10 parts of deionized waters, the lotion before being then added
In, 20min is stirred, it is cooling to solution, efficient durable waterproof soil-releasing finishing agent can be obtained.
The above-mentioned finishing agent of 20g is diluted in the water of 1L, then wherein by pure cotton blended fabric dipping, second dipping and rolling,
Pick-up is 70%, then by fabric at a temperature of 80 DEG C preliminary drying 20min, then at a temperature of 120 DEG C bake 10~15min after obtain
Product four.
Comparative example 1
2 parts of carboxymethyl celluloses are added in 17 parts of water, are stirred evenly, after sequentially add 5 parts of water-soluble silicon oils and 20 parts
Tripropylene glycol is warming up to 50-55 DEG C of stirring 20min, and 55 parts of HEC TA-5635F and 25 parts of water-and acrylate copolymerization creams are added
Liquid continues to stir 30min, cooling to solution, and efficient durable waterproof soil-releasing finishing agent can be obtained.
The above-mentioned finishing agent of 20g is diluted in the water of 1L, then wherein by pure cotton blended fabric dipping, second dipping and rolling,
Pick-up is 70%, then obtains product five after baking 10~15min at a temperature of 120 DEG C.
Comparative example 2
2 parts of carboxymethyl celluloses are added in 22 parts of water, are stirred evenly, after sequentially add 5 parts of water-soluble silicon oils and 20 parts
Tripropylene glycol is warming up to 50~55 DEG C of stirring 20min, and 50 parts of HEC TA-5635F are added and 30 parts of aqueous silicon-acrylates are total
Poly- lotion, continues to stir 10min, dilutes 5 parts of blocked isocyanate A with 10 parts of deionized waters, the lotion before being then added
In, 20min is stirred, it is cooling to solution, efficient durable waterproof soil-releasing finishing agent can be obtained.
The above-mentioned finishing agent of 20g is diluted in the water of 1L, then wherein by pure cotton blended fabric dipping, second dipping and rolling,
Pick-up is 70%, then by fabric at a temperature of 80 DEG C preliminary drying 20min, then at a temperature of 120 DEG C bake 10~15min after obtain
Product six.
Comparative example 3
2 parts of carboxymethyl celluloses are added in 22 parts of water, are stirred evenly, after sequentially add 5 parts of water-soluble silicon oils and 20 parts
Tripropylene glycol is warming up to 50~55 DEG C of stirring 20min, and 50 parts of HEC TA-5635F are added and 30 parts of aqueous silicon-acrylates are total
Poly- lotion, continues to stir 10min, dilutes 5 parts of blocked isocyanate C with 10 parts of deionized waters, the lotion before being then added
In, 20min is stirred, it is cooling to solution, efficient durable waterproof soil-releasing finishing agent can be obtained.
The above-mentioned finishing agent of 20g is diluted in the water of 1L, then wherein by pure cotton blended fabric dipping, second dipping and rolling,
Pick-up is 70%, then by fabric at a temperature of 80 DEG C preliminary drying 20min, then at a temperature of 120 DEG C bake 10~15min after obtain
Product seven.
Performance test
Test the performance of above-mentioned seven products: Water-proof and oil-proof, soil release performance energy including fabric, and to its sense of touch and remove
Dirty degree is evaluated, wherein waterproof test is referring to AATCC22, and referring to AATCC130-2000, control group is not for easy decontamination test
With the processed pure cotton blended fabric of finishing agent, test method is as follows:
Soil release performance energy test method:
AATCC Stain Release Management Performance Test of the easy detergency test based on the U.S.
Method is carried out.Test uses corn oil, mineral oil or artificial oil with dirt.
On the blotting paper of place mat in the horizontal direction, the test cloth that side length is 20cm square is sprawled, on the test cloth
Artificial oily 5 drop (about 0.2cc) dripped as dirt.Glassine paper is spread on it, then loads the counterweight of 2268g, is placed 60 seconds
Clock.After 60 seconds, counterweight and glassine paper are taken away, at room temperature, standing state is kept to place 15 minutes.After 15 minutes, to
It tests and adds ballast cloth on cloth, make its 1.8kg, using lotion (the WOB lotion of AATCC standard) 100g, washed with AATCC standard
Clothing machine washs 12 minutes under conditions of 64 liters of water, 38 DEG C of water temperature, after washing, with AATCC normal drum drying machine to test
Cloth is dried.The state of remaining dirt on test cloth after drying is compared with judgement with standard photographs plate, with right
The decision level (referring to table 1) answered indicates detergency ability.Determine to use AATCC-TM 130-2000 with standard photographs plate
(American Association of Textile Chemists and Colorists Test Method 130-2000)
Standard photographs plate.
The decision level of one soil release performance of table
| Decision level | Determinating reference |
| 1.0 | Remaining has obvious dirt |
| 2.0 | Remaining has considerable dirt |
| 3.0 | Remaining has a little dirt |
| 4.0 | Dirt is unobvious |
| 5.0 | Not remaining dirt |
Waterproof performance test method:
Water repellency test is carried out according to JIS L1092 benchmark.It indicates to prevent with waterproofing grade shower resistance.Water repellent is between two etc.
5 points can be added on the basis of lower waterproofing grade between grade.Evaluation criteria is shown in Table 2.
Two water repellency criterion of table
| Waterproofing grade | Evaluation criteria |
| 100 | Surface does not soak or water droplet attachment |
| 90 | Surface shows a small amount of water droplet attachment |
| 80 | Surface shows the wet of a few place parts |
| 70 | The half on surface shows wet |
| 50 | Surface is all wet |
| 0 | Two sides shows completely wet in table |
Oil preventing performance test method:
The evaluation criteria of oil repellent is the regulation according to AATCC-TM118, and a drop examination is added dropwise on the cloth through refusing oil processing
Liquid is tested, the state after 30 seconds is observed, when the experimental liquid of dropwise addition is held on cloth, further uses the test of greater number
Liquid is tested, and then with the marginal test liquid on cloth is able to maintain, the oil repellent based on following table is evaluated (should
Illustrate, be not able to maintain in the case of 100% atoleine (Nujol) and be denoted as 0).Evaluation criteria is shown in Table 3.
Three oil repellent criterion of table
| Rank | Test fluid |
| 8 | Normal heptane |
| 7 | Normal octane |
| 6 | N-decane |
| 5 | N-dodecane |
| 4 | N-tetradecane |
| 3 | Hexadecane |
| 2 | 35/ medical liquid paraffin 65 of hexadecane |
| 1 | Medical liquid paraffin |
Washing resistance test method:
According to JIS L-0217-103 method, washs ten times, 30 times or 50 times repeatedly, then evaluate water and oil repellant
Property (HL10 or HL30 or HL50).HLO refers to do not wash after the evaluation that carries out.
Sense of touch test:
According to following standard, the sense of touch of processed fabric is determined by being touched with hand.
It is good: more significantly than untreated fabric more soft
It is good: with untreated fabric flexibility having the same or compared with more soft
Difference: harder than untreated fabric
Decontamination degree evaluates (white coefficient):
Test cloth of the washing used in Performance evaluation in initial stage (initial stage) and washability evaluation (washing) after dry is used
Spectral photometric colour measuring agent measures reflectivity, calculates white coefficient (W.I%), the removing degree of spot is evaluated according to the size of its numerical value
(white coefficient is smaller, and the deciding degree of spot is bigger).
Test effect see the table below four and table five:
The performance test results of each product of table four after not washing and washing 10 times repeatedly
The performance test results of each product of table five after washing 30 times and 50 times repeatedly
Following result is obtained from table four and table five:
(1) properties of the processed fabric of unused finishing agent are very poor；
(2) comparative example 1 and Examples 1 to 4 are compared it is found that being arranged through the finishing agent without blocked isocyanate
The washing fastness of fabric afterwards is poor, and after washing 30 times repeatedly, properties are destroyed；And through finishing agent provided by the invention
The washing fastness of fabric after arrangement can be promoted to 50 times or more, and by 50 times repeatedly wash after the fabric still have it is more excellent
Different Water-proof and oil-proof and easy dirt-removing functions and the effect that flexibility is good, white coefficient is high；
(3) embodiment 1, embodiment 2 and comparative example 2 are compared respectively, embodiment 3, embodiment 4 and comparative example 3 into
Row comparison is it is found that comprising acting on fabric by the finishing agent that methyl ethyl ketone oxime is the blocked isocyanate that end-capping reagent synthesizes
When, the preliminary drying temperature needed is higher than the finishing agent of the blocked isocyanate synthesized by sodium hydrogensulfite for end-capping reagent, and
When its preliminary drying temperature is reduced to 80 DEG C, obtained fabric product washing fastness is substantially reduced, therefore, provided by the invention to include
When handling fabric by the finishing agent that sodium hydrogensulfite is the blocked isocyanate that end-capping reagent synthesizes, it can dry under cryogenic
The roasting fabric that is just able to maintain has efficient washable waterproof detergency ability, avoids fabric xanthochromia due to high-temperature baking, extends simultaneously
The service life of equipment reduces production cost.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of efficiently washable waterproof soil-releasing finishing agent composition, which is characterized in that in terms of mass parts, the composition packet
It includes: 40~60 parts of three-proof finishing agents, 20~40 parts of acrylate containing silicone copolymer emulsions, 20~25 parts of tripropylene glycols, 2~5 parts of water
Dissolubility silicone oil, 1~3 part of hydroxymethyl cellulose and 1~10 part of blocked isocyanate.
2. efficiently washable waterproof soil-releasing finishing agent composition as described in claim 1, which is characterized in that the enclosed type is different
The synthetic method of cyanate includes the following steps:
SA1 dissolves hydrophilic modifier to obtain the solution one that the mass fraction of hydrophilic modifier is 15~25%；
The solution one is added containing annular aliphatic or contains in aromatic diisocyanate under a shielding gas by SA2,
65~75 DEG C of 110~130min of reaction are continuously heating to after reacting 30~50min at 40~50 DEG C, to obtain Isocyanate prepolymers
Body.
SA3 blocks the Isocyanate prepolymers body using end-capping reagent, to obtain the blocked isocyanate.
3. efficiently washable waterproof soil-releasing finishing agent composition as claimed in claim 2, which is characterized in that described containing cyclic annular rouge
Fat race is isoflurane chalcone diisocyanate, toluene di-isocyanate(TDI), two isocyanide of diphenyl-methane containing aromatic diisocyanate
The combination of any one or more in acid esters or naphthalene diisocyanate；And/or
The end-capping reagent is selected from sodium hydrogensulfite, methyl ethyl ketone oxime, sodium pyrosulfate, sodium peroxydisulfate, phenol, cresols, levulinic
The combination of any one or more in ketone, malonic acid diethyl vinegar, isopropyl alcohol or Malaysia acid imide；And/or
The hydrophilic modifier be selected from polyethylene glycol, poly glycol monomethyl ether, polyoxypropyleneglycol, polypropylene oxide triol,
Orthoformic acid, ethylene glycol, propylene glycol, butanediol category, pentanediol class, hexylene glycol class, glycerol, pentaerythrite, sorbierite, new penta
The combination of any one or more in glycol, bisphenol-A or Xylene glycol；And/or
The mass fraction of free NCO is 5~10% in the Isocyanate prepolymers body.
4. efficiently washable waterproof soil-releasing finishing agent composition as described in claim 1, which is characterized in that the three-prevention finishing
The preparation method of agent includes the following steps:
SB1 weighs 50~60 parts of perfluoro hexyl ethyl methyl acrylates, 25~35 parts of long chain acrylate lists in terms of mass parts
Body, 20~30 parts of acrylate cross linked monomer, 15~20 parts of inclined dichloros containing cricoid acrylate monomer, 3~7 parts of hydroxyls
Ethylene, 1~3 part of cetyl trimethylammonium bromide, 4~10 parts of alcohol ethers emulsifiers, 2~5 parts of Tween 80s, 30~40 parts of poly- second
400,0.1~0.5 parts of lauryl mercaptans of glycol and 200~250 parts of deionized waters, obtain mixture one after mixing；
The temperature of the mixture one is risen to 50~60 DEG C and is stirred, after mixing evenly in the pressure of 30~50MPa by SB2
5~10min of homogeneous under power is warming up to 65~67 DEG C after homogeneous again, and 0.5~1 part of initiator one is then added, is continuously heating to 70
~72 DEG C of 4~6h of reaction, can be obtained the three-proof finishing agent.
5. efficiently washable waterproof soil-releasing finishing agent composition as claimed in claim 4, which is characterized in that the long-chain propylene
Acid ester monomer appointing in dodecyl acrylate, octadecyl acrylate, Behenyl acrylate or isodecyl methacrylate
It anticipates one or more combinations；And/or
It is described to be selected from cyclohexyl methacrylate, benzyl methacrylate or methacrylic acid containing cricoid acrylate monomer
The combination of any one or more in isobornyl thiocyanoacetate；And/or
The acrylate cross linked monomer of the hydroxyl is selected from N hydroxymethyl acrylamide, hydroxyethyl methacrylate or methyl-prop
The combination of any one or more in olefin(e) acid hydroxypropyl acrylate；And/or
It is withered that the initiator one is selected from V-50, benzoyl peroxide, lauroyl peroxide, tert-butyl peroxide, hydroperoxidation
Alkene, tert-butyl hydroperoxide neopentanoic acid, diisopropyl peroxydicarbonate, t-butyl perbenzoate, 1- hydroxy-cyclohexyl hydrogen
Any one in peroxide, 3- carbonyl propiony peroxide or acetyl peroxide.
6. efficiently washable waterproof soil-releasing finishing agent composition as described in claim 1, which is characterized in that the siliceous propylene
The preparation method of acid esters copolymer emulsion includes the following steps:
SC1 weighs 20~30 parts of methacrylic acids, 5~15 parts of hydroxy-ethyl acrylates, 25~35 parts of methyl-props in terms of mass parts
Olefin(e) acid butyl ester, 3~7 parts of vinyl-functional dimethyl silicone polymers, 15~25 parts of polyethylene glycol 400s, 60~140 parts of deionizations
Water, 2~5 parts of cetyl trimethylammonium bromides, 2~5 parts of Tween 80s and 2~5 parts of fatty alcohol polyoxyethylene ether AEO-9, mixing
After obtain mixture two；
The temperature of the mixture two is risen to 50~60 DEG C and is stirred, after mixing evenly in the pressure of 30~50MPa by SC2
5~10min of homogeneous under power is warming up to 65~67 DEG C after homogeneous again, and 0.3~0.8 part of initiator two is then added, is continuously heating to
70~72 DEG C of 4~6h of reaction, to obtain the acrylate containing silicone copolymer emulsion；Wherein, the initiator two is selected from V-50, mistake
Benzoyl Oxide, lauroyl peroxide, tert-butyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide neopentanoic acid, diisopropyl
Base peroxy dicarbonate, t-butyl perbenzoate, 1- hydroxy-cyclohexyl hydroperoxides, 3- carbonyl propiony peroxide
Or any one in acetyl peroxide.
7. a kind of efficiently washable waterproof soil-releasing finishing agent, which is characterized in that the efficiently washable waterproof soil-releasing finishing agent packet
Containing efficient washable waterproof soil-releasing finishing agent composition and solvent described in any one of claim 1~6.
8. a kind of preparation method of washable waterproof soil-releasing finishing agent efficient as claimed in claim 7, which is characterized in that the side
Method includes the following steps:
SD1 dissolves the hydroxymethyl cellulose with solvent, then sequentially adds water solubility into dissolved hydroxymethyl cellulose
Silicone oil and tripropylene glycol obtain mixture three after being warming up to 50~55 DEG C of 15~25min of stirring；
The three-proof finishing agent and the acrylate containing silicone copolymer emulsion are added in SD2, Xiang Suoshu mixture three, continues 50
Mixture four is obtained after stirring 5~20min at~55 DEG C；
Blocked isocyanate is added in SD3, Xiang Suoshu mixture four, continues to obtain after stirring 15~25min at 50~55 DEG C
To the efficiently washable waterproof soil-releasing finishing agent.
9. a kind of preparation method of washable waterproof easy-to-remove-dirt fabric, which is characterized in that described method includes following steps:
Fabric to be processed is immersed in the efficient washable easy decontamination of waterproof made from preparation method according to claim 8 by SE1
Finishing agent is as claimed in claim 7 efficiently in washable waterproof soil-releasing finishing agent, two leaching two bundles, and pick-up is 70~
75%；
SE2, by the fabric after two leaching two bundles at a temperature of 80~100 DEG C 15~20min of preliminary drying, then at a temperature of 110~120 DEG C
10~15min is baked, washable waterproof easy-to-remove-dirt fabric can be obtained.
10. a kind of using washable waterproof easy-to-remove-dirt fabric made from preparation method described in claim 9.
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| CN114673000A (en) * | 2022-03-31 | 2022-06-28 | 中国第一汽车股份有限公司 | Three-proofing negative oxygen ion finishing agent for automotive interior, preparation method and application |
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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 |
| CN112391839A (en) * | 2020-11-18 | 2021-02-23 | 湖南派意特服饰有限公司 | Western-style clothes finishing agent and preparation method thereof |
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| CN114575156A (en) * | 2022-03-23 | 2022-06-03 | 中国第一汽车股份有限公司 | Three-proofing composite finishing agent for automotive interior suede fabric, preparation and application |
| CN114575156B (en) * | 2022-03-23 | 2024-04-16 | 中国第一汽车股份有限公司 | Three-proofing composite finishing agent for automotive interior suede-like fabric, preparation and application |
| CN114673000A (en) * | 2022-03-31 | 2022-06-28 | 中国第一汽车股份有限公司 | Three-proofing negative oxygen ion finishing agent for automotive interior, preparation method and application |
| CN114673000B (en) * | 2022-03-31 | 2024-04-16 | 中国第一汽车股份有限公司 | Three-proofing negative oxygen ion finishing agent for automotive interiors, preparation method and application |
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