CN101671958A - Polysiloxane crease resistant finishing agent composition for natural fiber and preparation method thereof - Google Patents
Polysiloxane crease resistant finishing agent composition for natural fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a polysiloxane crease resistant finishing agent composition for natural fiber and a preparation method thereof. The composition comprises: (A) a modified polysiloxane emulsionwith linear molecular structure, the two ends of the molecule of the modified polysiloxane emulsion are sealed by hydroxyl or alkoxy, and the molecule at least has one hydroxyl bonding with silicon atom and alkyl substituted by amino; (B) a polysiloxane emulsion containing polyhydroxy; (C) a silane coupling agent containing epoxy group; and (D) an organic acid metal salt catalyst. The crease resistant finishing agent has softening function for fabric, and also has the characteristics of no aldehyde, low yellowing, strong capability of preventing the fabric from being damaged, etc.
Description
Technical field
That the present invention relates to is polysiloxane crease resistant finishing agent composition and the preparation method that a kind of natural fabric uses.The key component of this finishing agent is the modified polyorganosiloxanes of linearity molecular structure, by being mixed with itself and polyhydroxy polycarboxylic organosiloxane, crosslinking agent and catalyst, can make the natural fabric after the processing have high resilience, thereby improve the wrinkle resistance of fabric.
Background technology
The anti-crease finishing of natural fabric adopts dihydroxymethyl dihydroxy ethyl ethylene-urea resin (2D resin) more at present, but fabric strength seriously descends after its arrangement, and content of formaldehyde exceeds standard.Therefore, the exploitation at low formaldehyde crease-shedding finishing agent or formaldehydeless crease-shedding finishing agent is the research focus of textile industry always.
Prior art discloses some crease-shedding finishing agents and manufacture method, for example, the CN03134276.0 patent disclosure the no aldehyde crease-shedding finishing agent of forming by chitosan solution, acetic acid, sodium acetate, citric acid and glyoxal; The CN200810038996.X patent disclosure a kind of aqueous polyurethane of sodium hydrogensulfite end-blocking do not have the aldehyde crease-shedding finishing agent.Though more than two kinds of crease-shedding finishing agents do not have aldehyde, very easily make the fabric yellowing by the finishing agent of preparations such as shitosan, citric acid, and strength damage is also bigger.Though the aqueous polyurethane crease-shedding finishing agent is fast because of its film forming speed to the fabric strength not damaged, is prone to skinning and roll banding phenomenon in to the textile finishing process, and it is coarse to handle the back fabric feeling, and flexibility is poor.At present, do not see that useful polysiloxane is open as the crease-shedding finishing agent technology of Main Ingredients and Appearance.
Summary of the invention
The purpose of this invention is to provide does not a kind ofly have aldehyde, low yellowing and can improve soft type polysiloxane crease resistant finishing agent composition of fabric tearing brute force and preparation method thereof.
Polysiloxane crease resistant finishing agent composition of the present invention comprises:
(A) non-volatile part of 100 parts of weight is 20%~40% modified polyorganosiloxanes emulsion, and wherein the general structure of polymer is:
In the formula: R is hydroxyl or methyl;
Y is the amino monovalence alkyl that replaces;
x=40~8000,m=1~500,n=1~500。
(B) non-volatile part of 5~10 parts of weight is 20%~30% the polyhydric organic siloxane emulsion that contains.Wherein the general structure of polymer is:
In the formula: a=4~500, b=4~500.
(C) silane coupler that contains epoxy radicals of 1~5 part of weight.
(D) the organic acid zinc salt or the pink salt of 1~5 part of weight.
In the present composition, at first we select emulsion polymerisation process, will contain amino silane coupler and methyl trialkoxysilane and react with silicone intermediate simultaneously, by reasonable controlling reaction time and temperature, make the modified polyorganosiloxanes emulsion of high molecular weight, i.e. (A) component.Owing in the polysiloxane molecule, introduce aminoly, flexibility, smooth property and the tearing brute force of handling the back fabric are improved greatly, by we can make the xanthochromia degree of product reduce to minimum to the control of amino content; The introducing of methyl tri-alkoxy has simultaneously increased the self-crosslinking of product itself, can improve the resilience of handling the back fabric effectively.
Although (A) component has certain contribution to the wrinkle resistance of fabric, because crosslink density is little, the elasticity deficiency does not often reach the level of 2D resin anti creasefinish.Therefore, in order further to improve the wrinkle resistance of product to natural fabric, we have added the polyhydroxy polycarboxylic organosiloxane in composition, i.e. (B) component, a plurality of hydroxyls on its molecule can with hydroxyl on hydroxyl, amino and the fiber on the polysiloxane molecule in (A) component in heating or the three-dimensional netted resin structure of formation under the catalyst condition is arranged, the crosslink density of product is extremely increased, increased the resilience of fiber, thereby the crease recovery ability of fiber is improved greatly.
Epoxy radicals in the component (C) can react with the amino in component (A) molecular structure, promotes softness and the slippery of handling the back fabric.Alkoxyl in the component (C) can be hydrolyzed into Si-OH in water simultaneously, condensation reaction can take place with the Si-OH in component (A) and component (B) molecular structure in it on the one hand, increase the molecular weight and the degree of cross linking of polymer, further improve the elasticity of handling the back fabric; Si-OH also can form hydrogen bond or covalent bond with the hydroxyl on the fabric on the other hand, thereby increases the washability of handling the back fabric.
Component (D) is used as catalyst in system, and it can improve the reaction speed between the Si-OH, makes it to react more fully, thereby the wrinkle resistance of handling the back fabric is demonstrated fully.
In sum, the natural fabric of handling through this crease resistant finishing agent composition removes has splendid elasticity and flexibility, also has advantages such as no aldehyde, low-yellowing and raising fabric tearing brute force.
The preparation method
One, the preparation of component (A)
Raw material:
(1), 200~350 restrains octamethylcy-clotetrasiloxane or α, alpha, omega-dihydroxy polydimethyl siloxane (molecular weight about 3000);
(2), 1~10 gram contains amino silane coupler, it comprises N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, γ-An Bingjisanjiayangjiguiwan, gamma-aminopropyl-triethoxy-silane one or two kinds of mixing are used;
(3), 1~10 the gram methyl trialkoxysilane, it comprises MTMS or MTES one;
(4), 15~25 gram DBSAs;
(5), 2~5 gram lauryl alcohol polyoxyethylene (20) ethers;
(6), 500~900 gram deionized waters;
Preparation technology:
With octamethylcy-clotetrasiloxane or α, alpha, omega-dihydroxy polydimethyl siloxane (molecular weight about 3000), contain amino silane coupler, methyl trialkoxysilane, DBSA, lauryl alcohol polyoxyethylene (20) ether and deionized water stirs and this mixed liquor logical going in the high pressure homogenization machine of 30Mpa made emulsion, join then in the reactor of being furnished with condenser and agitating device, after reacting 12~24 hours under 70~80 ℃ of conditions, be cooled to 5~20 ℃ and continue reaction 5~10 hours again, transfer pH=7 with 10% aqueous sodium carbonate at last, non-volatile part is 20%~40% modified polyorganosiloxanes emulsion;
Two, the preparation of component (B)
Raw material:
(1), 10~15 gram tetramethyl dihydro base disiloxane;
(2), 30~40 gram tetramethyl-ring tetrasiloxanes;
(3), 200~250 gram octamethylcy-clotetrasiloxanes;
(4), 5~8 gram concentrated sulfuric acid (98%) or trifluoromethane sulfonic acids;
(5), 10~30 gram isomerous tridecanol polyoxyethylene (5) ethers (trade names TO-5);
(6), 15~50 gram isomerous tridecanol polyoxyethylene (7) ethers (trade names TO-7);
(7), 700~1000 gram deionized waters.
Preparation technology:
With tetramethyl dihydro base disiloxane, tetramethyl-ring tetrasiloxane, octamethylcy-clotetrasiloxane, the concentrated sulfuric acid (98%) or trifluoromethane sulfonic acid join in the reactor of being furnished with condenser and agitating device and fully mix, balanced reaction is 6~10 hours under 50 ℃~60 ℃ conditions, add small amount of deionized water then, under this temperature, continue to stir 3~5 hours, get polyhydroxy polycarboxylic organosiloxane performed polymer, reduce to and add isomerous tridecanol polyoxyethylene (5) ether behind the normal temperature and isomerous tridecanol polyoxyethylene (7) ether fully stirs, add deionized water then and carry out emulsification, transfer pH=6 with 10% aqueous sodium carbonate at last, non-volatile part is 20%~30% the polyhydric organic siloxane emulsion that contains.
Three, component (C) is to contain epoxy silane coupling, optional γ-glycidol oxygen propyl trimethoxy silicane, γ-glycidol oxygen propyl-triethoxysilicane, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, β-(3, the 4-epoxycyclohexyl) ethyl triethoxysilane one.
Four, component (D) is organic acid zinc salt or pink salt, optional zinc acetate, dibutyltin diacetate, dibutyl tin laurate one.If the use zinc acetate then can directly join it in treatment fluid,, then it can be emulsified into 20% stable emulsion use with emulsifying agent if use dibutyltin diacetate or dibutyl tin laurate.
During use in (A): (B): (C): (D)=100: 5~10: 1~5: 1~5 ratio is mixed.
The specific embodiment
Component (A) preparation embodiment 1:
With 230.0 gram octamethylcy-clotetrasiloxanes, 3.5 gram gamma-aminopropyl-triethoxy-silane, 4.5 gram MTMS, 17.5 gram DBSA, 2.5 gram lauryl alcohol polyoxyethylene (20) ether and 742 gram deionized waters stir and this mixed liquor logical going in the high pressure homogenization machine of 30Mpa are made emulsion, join then in the reactor of being furnished with condenser and agitating device, after reacting 12 hours under 70~72 ℃ of conditions, be cooled to 20 ℃ and continue reaction 5 hours again, transfer pH=7 with 10% aqueous sodium carbonate at last, non-volatile part be 23.7% emulsion, this emulsion called after A1.
Component (A) preparation embodiment 2:
With 330.0 gram α, the alpha, omega-dihydroxy dimethyl polysiloxane, 2.0 gram gamma-aminopropyl-triethoxy-silane, 6.0 gram MTMS, 20.0 gram DBSA, 3.0 gram lauryl alcohol polyoxyethylene (20) ether and 639 gram deionized waters stir and this mixed liquor logical going in the high pressure homogenization machine of 30Mpa are made emulsion, join then in the reactor of being furnished with condenser and agitating device, after reacting 12 hours under 70~72 ℃ of conditions, be cooled to 20 ℃ and continue reaction 5 hours again, transfer pH=7 with 10% aqueous sodium carbonate at last, non-volatile part is 33.9% emulsion, this emulsion called after A2.
Component (A) preparation embodiment 3:
With 230.0 gram octamethylcy-clotetrasiloxanes, 3.5 gram gamma-aminopropyl-triethoxy-silane, 4.5 gram MTMS, 17.5 gram DBSA, 2.5 gram lauryl alcohol polyoxyethylene (20) ether, and 742 the gram deionized waters stir and this mixed liquor logical going in the high pressure homogenization machine of 30Mpa made emulsion, join then in the reactor of being furnished with condenser and agitating device, after reacting 12 hours under 70~72 ℃ of conditions, be cooled under 5 ℃ of conditions and reacted 10 hours, transfer pH=7 with 10% aqueous sodium carbonate at last, non-volatile part is 24.1% emulsion, this emulsion called after A3.
Component (A) preparation embodiment 4:
With 230.0 gram octamethylcy-clotetrasiloxanes, 6.5 gram N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, 1.5 gram MTES, 15.0 gram DBSA, 5.0 gram lauryl alcohol polyoxyethylene (20) ether and 742 gram deionized waters stir and this mixed liquor logical going in the high pressure homogenization machine of 30Mpa are made emulsion, join then in the reactor of being furnished with condenser and agitating device, after reacting 20 hours under 70~72 ℃ of conditions, be cooled to 5 ℃ and continue reaction 10 hours again, transfer pH=7 with 10% aqueous sodium carbonate at last, non-volatile part be 23.9% emulsion, this emulsion called after A4.
Component (B) preparation embodiment 1:
With 13.4 gram tetramethyl dihydro base disiloxane, 35.8 gram tetramethyl-ring tetrasiloxane, the 222 gram octamethylcy-clotetrasiloxanes and the 8.0 gram concentrated sulfuric acids (98%) stir under 50 ℃ of conditions and carried out equilibration reaction in 10 hours, add 5.0 gram deionized waters then, under this temperature, continue to stir 3 hours, get polyhydroxy polycarboxylic siloxanes performed polymer, add 10.6 gram isomerous tridecanol polyoxyethylene (5) ethers after reducing to normal temperature, 48.0 gram isomerous tridecanol polyoxyethylene (7) fully stirs, add 850 gram deionized waters then with it emulsification, and transfer pH=6 with 10% aqueous sodium carbonate, non-volatile part be 27.5% emulsion, this emulsion called after B1.
Component (B) preparation embodiment 2:
With 13.4 gram tetramethyl dihydro base disiloxane, 30.0 gram tetramethyl-ring tetrasiloxane, 250.0 gram octamethylcy-clotetrasiloxane and 5.0 gram trifluoromethane sulfonic acids stir under 60 ℃ of conditions and carried out equilibration reaction in 6 hours, add 4.4 gram deionized waters then, under this temperature, continue to stir 3 hours, get polyhydroxy polycarboxylic siloxanes performed polymer, add 25.0 gram isomerous tridecanol polyoxyethylene (5) ethers after reducing to normal temperature, 16.0 gram isomerous tridecanol polyoxyethylene (7) fully stirs, add 900 gram deionized waters then with it emulsification, and transfer pH=6 with 10% aqueous sodium carbonate, non-volatile part be 25.7% emulsion, this emulsion called after B2.
Component (B) preparation embodiment 3:
With 10.0 gram tetramethyl dihydro base disiloxane, 40.0 gram tetramethyl-ring tetrasiloxane, 210.0 gram octamethylcy-clotetrasiloxane and 5.0 gram trifluoromethane sulfonic acids stir under 60 ℃ of conditions and carried out equilibration reaction in 8 hours, add 5.2 gram deionized waters then, under this temperature, continue to stir 3 hours, get polyhydroxy polycarboxylic siloxanes performed polymer, add 15.0 gram isomerous tridecanol polyoxyethylene (5) ethers after reducing to normal temperature, 30.0 gram isomerous tridecanol polyoxyethylene (7) fully stirs, add 1050 gram deionized waters then with it emulsification, and transfer pH=6 with 10% aqueous sodium carbonate, non-volatile part be 21.8% emulsion, this emulsion called after B3.
Crease resistant finishing agent composition of the present invention can be put in order fabric with dipping or padding method.
Experimental example 1 (weight ratio):
With 100 parts of A1,10 parts of B1,5 parts of γ-glycidol oxygen propyl trimethoxy silicanes, 5 parts of zinc acetates mix crease resistant finishing agent composition, adding 880 parts of demineralized waters and mix and be made into fabric treating liquid, is that 40 * 40,133 * 72 textile calico is put in order with the method for padding to specification, and pick-up is 75%, dry under 100 ℃ of conditions, bake 2min at 160 ℃ then.Every index testing result of handling the back calico sees Table 1.
Experimental example 2 (weight ratio):
With 100 parts of A1,8 parts of B2,3 parts of γ-glycidol oxygen propyl-triethoxysilicanes, 3 parts of zinc acetates mix crease resistant finishing agent composition, add 886 parts of demineralized waters and mix and be made into fabric treating liquid, according to the finishing technique identical with experimental example 1 fabric is put in order and estimated, testing result sees Table 1.
Experimental example 3 (weight ratio):
With 100 parts of A2,5 parts of B2,2 parts of γ-glycidol oxygen propyl trimethoxy silicanes, 4 parts of zinc acetates mix crease resistant finishing agent composition, add 889 parts of demineralized waters and mix and be made into fabric treating liquid, according to the finishing technique identical with experimental example 1 fabric is put in order and estimated, testing result sees Table 1.
Experimental example 4 (weight ratio):
With 100 parts of A2,5 parts of B2,2 parts of β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, the dibutyl tin laurate emulsion of 1 part of 20% content mix crease resistant finishing agent composition, add 892 parts of demineralized waters and mix and be made into fabric treating liquid, according to the finishing technique identical with experimental example 1 fabric is put in order and estimated, testing result sees Table 1.
Experimental example 5 (weight ratio):
With 100 parts of A3,10 parts of B3,5 parts of γ-glycidol oxygen propyl trimethoxy silicanes, 5 parts of zinc acetates mix crease resistant finishing agent composition, add 880 parts of demineralized waters and mix and be made into fabric treating liquid, according to the finishing technique identical with experimental example 1 fabric is put in order and estimated, testing result sees Table 1.
Experimental example 6 (weight ratio):
With 100 parts of A4,10 parts of B3,5 parts of γ-glycidol oxygen propyl trimethoxy silicanes, the dibutyl tin laurate emulsion of 2 part of 20% content mix crease resistant finishing agent composition, add 883 parts of demineralized waters mixing and be made into fabric treating liquid, to textile finishing and evaluation, testing result sees Table 1 according to the finishing technique identical with experimental example 1.
Comparative Examples 1 (weight ratio):
Low urea formaldehyde Arkofix NDF liq.conc. with 100 parts of Clariants, 30 parts of softener Solusoft MCT liq, 30 parts of catalyst n KS and 840 parts of demineralized waters mix and are made into fabric treating liquid, and to textile finishing and evaluation, testing result sees Table 1 according to the finishing technique identical with experimental example 1.
Comparative Examples 2 (weight ratio):
With 100 parts of polyurethane crease-shedding finishing agent RUCO PUR SLK (German Rudoiph), 900 parts of demineralized waters mix and are made into fabric treating liquid, and to textile finishing and evaluation, testing result sees Table 1 according to the finishing technique identical with experimental example 1.
Table 1
Evaluation criterion to the every performance of fabric is as follows:
1, content of formaldehyde is pressed the GB18401-2001 test;
2, creasy recovery angle is pressed the GB/T3819-1997 test;
3, tearing brute force is pressed the GB/T3917.2-1997 test;
4, the test of xanthochromia degree is that the fiber after handling with crease-shedding finishing agent was baked 5 minutes under 180 ℃ of conditions, represents not have yellow by following standard evaluation: *, and * * represents not have substantially yellow, and * * * represents light yellow, and * * * * represents yellow;
5, the evaluation of pliability is as the criterion to the comprehensive evaluation result of feel with 6 people, ++ ++ for best ,+for the poorest.
Claims (3)
1, polysiloxane crease resistant finishing agent composition for natural fiber is characterized in that comprising:
(A) non-volatile part of 100 parts of weight is 20%~40% modified polyorganosiloxanes emulsion, and wherein the general structure of polymer is:
In the formula: R is hydroxyl or methyl;
Y is the amino monovalence alkyl that replaces;
x=40~8000,m=1~500,n=1~500;
(B) non-volatile part of 5~10 parts of weight is 20%~30% the polyhydric organic siloxane emulsion that contains, and wherein the general structure of polymer is:
In the formula: a=4~500, b=4~500;
(C) silane coupler that contains epoxy radicals of 1~5 part of weight;
(D) the organic acid zinc salt or the pink salt of 1~5 part of weight.
2, polysiloxane crease resistant finishing agent composition for natural fiber according to claim 1 is characterized in that:
The optional γ of the silane coupler-glycidol oxygen propyl trimethoxy silicane that contains epoxy radicals, γ-glycidol oxygen propyl-triethoxysilicane, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, β-(3, the 4-epoxycyclohexyl) ethyl triethoxysilane one or two kinds of mixing are used;
Organic acid zinc salt or pink salt, optional zinc acetate, dibutyltin diacetate, dibutyl tin laurate one.
3, polysiloxane crease resistant finishing agent composition for natural fiber preparation method is characterized in that:
One, the preparation of component (A)
Raw material:
(1), 200~350 restrains octamethylcy-clotetrasiloxane or α, alpha, omega-dihydroxy polydimethyl siloxane (molecular weight about 3000);
(2), 1~10 gram contains amino silane coupler, it comprises N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, γ-An Bingjisanjiayangjiguiwan, gamma-aminopropyl-triethoxy-silane one or two kinds of mixing are used;
(3), 1~10 the gram methyl trialkoxysilane, it comprises MTMS or MTES one;
(4), 15~25 gram DBSAs;
(5), 2~5 gram lauryl alcohol polyoxyethylene (20) ethers;
(6), 500~900 gram deionized waters;
Preparation technology:
With octamethylcy-clotetrasiloxane or α, alpha, omega-dihydroxy polydimethyl siloxane (molecular weight about 3000), contain amino silane coupler, methyl trialkoxysilane, DBSA, lauryl alcohol polyoxyethylene (20) ether and deionized water stirs and this mixed liquor logical going in the high pressure homogenization machine of 30Mpa made emulsion, join then in the reactor of being furnished with condenser and agitating device, after reacting 12~24 hours under 70~80 ℃ of conditions, be cooled to 5~20 ℃ and continue reaction 5~10 hours again, transfer pH=7 with 10% aqueous sodium carbonate at last, getting non-volatile part is 20%~40% modified polyorganosiloxanes emulsion;
Two, the preparation of component (B)
Raw material:
(1), 10~15 gram tetramethyl dihydro base disiloxane;
(2), 30~40 gram tetramethyl-ring tetrasiloxanes;
(3), 200~250 gram octamethylcy-clotetrasiloxanes;
(4), 5~8 gram concentrated sulfuric acid (98%) or trifluoromethane sulfonic acids;
(5), 10~30 gram isomerous tridecanol polyoxyethylene (5) ethers;
(6), 15~50 gram isomerous tridecanol polyoxyethylene (7) ethers;
(7), 700~1000 gram deionized waters;
Preparation technology:
With tetramethyl dihydro base disiloxane, tetramethyl-ring tetrasiloxane, octamethylcy-clotetrasiloxane, the concentrated sulfuric acid (98%) or trifluoromethane sulfonic acid join in the reactor of being furnished with condenser and agitating device and fully mix, balanced reaction is 6~10 hours under 50 ℃~60 ℃ conditions, add small amount of deionized water then, under this temperature, continue to stir 3~5 hours, get polyhydroxy polycarboxylic organosiloxane performed polymer, add isomerous tridecanol polyoxyethylene (5) ether and isomerous tridecanol polyoxyethylene (7) ether and fully stirring after reducing to normal temperature, add deionized water then and carry out emulsification, transfer pH=6 with 10% aqueous sodium carbonate at last, non-volatile part is 20%~30% the polyhydric organic siloxane emulsion that contains;
Three, component (C) is to contain epoxy silane coupling, optional γ-glycidol oxygen propyl trimethoxy silicane, γ-glycidol oxygen propyl-triethoxysilicane, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, β-(3, the 4-epoxycyclohexyl) ethyl triethoxysilane one;
Four, component (D) is organic acid zinc salt or pink salt, optional zinc acetate, dibutyltin diacetate, dibutyl tin laurate one;
During use in (A): (B): (C): (D)=100: 5~10: 1~5: 1~5 ratio is mixed.
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