CN101302268A - Non-formaldehyde organosilicon color fixing agent - Google Patents

Non-formaldehyde organosilicon color fixing agent Download PDF

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CN101302268A
CN101302268A CNA2008100401675A CN200810040167A CN101302268A CN 101302268 A CN101302268 A CN 101302268A CN A2008100401675 A CNA2008100401675 A CN A2008100401675A CN 200810040167 A CN200810040167 A CN 200810040167A CN 101302268 A CN101302268 A CN 101302268A
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laking agent
ammonium chloride
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organosilicon
hydroxyl
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CN101302268B (en
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王利民
徐助成
赵成英
胡小文
田禾
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East China University of Science and Technology
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East China University of Science and Technology
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Abstract

The invention relates to organosilicon coloring stabilizer not containing aldehyde compounds. The coloring stabilizer is a macromolecular compound which takes quaternary ammonium salt as main chain segment and introduces organosilicon chain segment and water soluble reactive groups (such as hydroxyl or/and halogen and so on) at the same time, wherein the oxygen ion group in the macromolecular compound can be reacted with the anion group in dyes so as to generate lake (fixation); the organosilicon chain segment can improve the softness and the smoothness of fabrics, and can also increase wet rubbing fastness; while groups containing hydroxyl and chloro-, etc. can be reacted with fabric fiber to form a crosslinking structure, thereby greatly increasing the washing fastness and the wet rubbing fastness of fabrics. Therefore, the organosilicon coloring stabilizer is environment-friendly (not containing aldehyde compounds) and also has excellent dyefastness.

Description

Non-formaldehyde organosilicon color fixing agent
Technical field
The present invention relates to a kind of laking agent that is used for dyeing, specifically, relate to a kind of organosilicon color fixing agent of not aldehyde-containing type compound.
Background technology
Substantive dyestuff, matching stain and reactive dyestuffs are used in the dyeing of cotton fibre usually.Substantive dyestuff, matching stain and reactive dyestuffs all are anionic dyestuffs, all contain water soluble groups such as sulfonic group, carboxyl in the molecule.Substantive dyestuff and matching stain all mainly are to rely on Van der Waals force and hydrogen bond to anchor on the fiber, and the fastness of set is limited, is easy to hydrolysis and fades in water, so generally all need to improve the coloration of textile materials fastness with laking agent.Contain reactive group in the reactive dyestuff molecule structure, can generate covalent linkage, so dyefastness is higher relatively with fiber-reactive.But reactive dyestuffs are in dyeing course, and dyestuff unreacted reactant and hydrolyzate can not be clean fully, and this part dyestuff will fade, and simultaneously, the covalent linkage that dyes on the thing also can the hydrolysis scission of link.The raising that requires along with the textile dyeing fastness still needs to use laking agent when dying some dark heavy colour fabrics.
Traditional laking agent (as: the resin laking agent of Dyhard RU 100 and formaldehyde condensation) is though can effectively improve the coloration of textile materials fastness, but because its formaldehyde content is higher (after laking agent is handled, free formaldehyde content is generally greater than 200mg/kg), harmful to human and environment.Therefore the development of aldehyde-free colour stabilizer enjoys chemists' concern.
When (even reaching more than the 10%owf) dye strength dyes more than using 5%owf, not quite a lot of with the amount of dye of fibrin reaction set, be very easy to produce hydrolysis, decolouring, cause colour fastness to reduce greatly.Laking agent in the market has apparent in view raising to washing, the soaping fastness of fabric, but the raising of fastness to wet rubbing is not all reached the ideal effect.Because when doing the test of " wet friction " fastness, the white cotton fine cloth that normally will wet rubs mutually with the dyeing cloth specimen of doing.The frictional coefficient that moisture on this moment wet white cotton fine cloth does not only play is lubricated, reduction and dry state painting cloth are mutual and the effect of raising smoothness, a kind of swelling, dissolving and adsorption have been played on the contrary: in friction process, make not participation react dyestuff (the referring generally to staining) swelling of set, dissolve, come off, and be adsorbed on rapidly on the white cotton fine cloth of wet test, so difficulty is very big aspect the fastness to wet rubbing that improves fabric.Thereby the aldehyde-free colour stabilizer of development of new becomes the technical issues that need to address of the present invention.
Existing aldehyde-free colour stabilizer exists deficiency aspect dyefastness.Therefore, the aldehyde-free colour stabilizer cost technical problem to be addressed by invention of development of new.
Summary of the invention
Because dye molecule is generally anionic compound, so we design laking agent is cation compound, both are reacted, produce more firm covalent linkage, the hydrophilic group of dye molecule is closed in and forms precipitation on the fabric, can prevent that like this dyestuff from coming off and hydrolysis from fabric because of ionization, thereby improve colour fastness.Simple table is shown following reaction formula:
DSO 3Na+FX→DSO 3F+NaX
D-is a dye matrix, and F-is a cation group in the laking agent.
In addition, laking agent is designed to superpolymer, makes it, cover caducous right dyestuff in the fabric face film forming; Also according to containing active group or crosslinking structure in the structure of cotton fiber design laking agent, make with toner and anchor at fabric face firmly simultaneously together with dyestuff; Thereby effectively improve the dyefastness of each side.
The said laking agent of the present invention, it is 1 by compound shown in compound shown in vinylsiloxane (vinyl silicone oil), the formula I and the formula II by mass ratio mainly: (2~10): 10, under 30 ℃~80 ℃ conditions, make initiator with Potassium Persulphate, copolymerization obtained in 5~20 hours;
Figure A20081004016700041
Wherein: R 1And R 2Independently be selected from C respectively 1~C 6A kind of in the alkyl, R 3Be C 1~C 16The C of alkyl or replacement 1~C 16Alkyl, X are halogen (F, Cl, Br or I);
The C of said replacement 1~C 16Substituting group in the alkyl is selected from: halogen (F, Cl, Br or I), a kind of in hydroxyl or the phenyl, two or more.
In optimal technical scheme of the present invention, selected vinylsiloxane is that molecular weight is 950~1200, the content of vinyl is the vinylsiloxane of 5wt%~10wt%;
In another optimal technical scheme of the present invention, 60 ℃~80 ℃ of polymeric reaction temperatures, polymerization reaction time is 10-15 hour;
In another optimal technical scheme of the present invention, R 1And R 2Independently be selected from C respectively 1~C 3A kind of in the alkyl;
In another optimal technical scheme of the present invention, R 3Be benzyl, hexadecyl or 2-hydroxyl, 3-chloro-propyl group.
The method for preparing the said laking agent of the present invention (random copolymers) comprises the steps:
(1) preparation of partial monosomy (compound shown in formula I and the formula II):
With corresponding secondary amine is starting raw material, makes corresponding quaternary amine (compound shown in formula I and the formula II) with corresponding haloalkane reaction;
(2) being principal monomer by prepared quaternary amine of step (1) and vinylsiloxane (commercially available product), and satisfying feeds in raw material is: compound is 1 by mass ratio shown in compound shown in vinylsiloxane, the formula I and the formula II: (2~10): 10, under 30 ℃~80 ℃ conditions, make initiator with Potassium Persulphate, copolymerization obtained target compound (laking agent) in 5~20 hours.
Monomeric synthetic route is as follows:
Figure A20081004016700051
Wherein: R 1, R 2, R 3Described identical with the implication of X with preamble.
Embodiment
Prepare the method for laking agent of the present invention, comprise the steps:
(1) preparation of partial monosomy:
Compound (1) and compound (2) were placed reactor in 1: 1 in molar ratio,, react 3-10 hour (preferred 5-8 hour) and get compound (3) in 0 ℃~60 ℃ (preferred 5 ℃~10 ℃);
Compound (3) can make compound shown in the formula II with compound (2) by above-mentioned similar approach again;
In like manner, compound (3) makes compound shown in the formula I with compound (4) reaction.
(2) preparation of laking agent:
Be 1 by mass ratio mainly: (2~10) with compound shown in compound shown in vinylsiloxane, the formula I and the formula II: 10, under 60 ℃~80 ℃ conditions, make initiator with Potassium Persulphate, copolymer-1 obtained target compound in 0~15 hour.
The organosilicon macromolecule aldehyde-free colour stabilizer of the present invention's preparation is compared with traditional laking agent, has safer, environmental protection, makes fabric possess more firm dyefastness, is not easy jaundice simultaneously.
Laking agent of the present invention, be a kind of be main segmental macromolecular compound with quaternary ammonium salt, introduced organosilicon segment and water-soluble reaction group (as hydroxyl or/and halogen etc.) simultaneously.In the described macromolecular compound, the oxonium ion group can generate color lake (fixation) with the anionic group reaction in the dyestuff; Its organosilicon segment can improve the flexibility of fabric, and smooth property has improved fastness to wet rubbing; And hydroxyl, groups such as chloro can form crosslinking structure with the fabric fibre reaction, have improved the washing fastness of fabric, fastness to wet rubbing greatly.Therefore, not only environmental protection of laking agent of the present invention (not aldehyde-containing type compound), and have good dye fastness and dye.
The invention will be further elaborated below by embodiment, and its purpose only is better to understand content of the present invention, and unrestricted protection scope of the present invention.
Embodiment 1
Synthesizing of DMAA:
In the 100ml flask, add 45 gram dimethylamine solutions (33%), under 5 ℃ of conditions, alternately drip the propenyl chloride and the aqueous sodium hydroxide solution of same molar, react after 6 hours, product is divided into three layers of oil reservoir, water layer and solid layers, filter, get the upper strata oil reservoir behind the separatory, with obtaining faint yellow pungency liquid after the sodium hydrate solid drying.
Synthesizing of dimethyl diallyl ammonium chloride:
Add the 10ml DMAA and with the propenyl chloride of molar weight, add the 50ml acetone solvent again in the 100ml flask, carry out quaterisation under 60 ℃, react after 3-4 hour, layering appears in product, and separatory takes off a layer dimethyl diallyl ammonium chloride liquid.
Synthesizing of hexadecyldimethyl benzyl ammonium allyl ammonium chloride:
Get Virahol 100ml and place flask to make solvent, get hexadecyldimethyl benzyl ammonium tertiary amine 20ml and propenyl chloride 25ml, logical nitrogen protection, reaction is after 6-8 hour down at 60 ℃, and behind activated carbon decolorizing, the choosing steaming obtains weak yellow liquid after removing and desolvating.Synthesizing of laking agent:
Get dimethyl diallyl ammonium chloride 10 grams, 1 gram, vinyl silicone oil (molecular weight 950-1050, contents of ethylene are 5wt%) hexadecyldimethyl benzyl ammonium allyl ammonium chloride 2 grams, Hydroxyethyl acrylate 2 grams, K 2S 2O 8Get 0.040 gram as initiator, logical nitrogen protection was reacted 10-15 hour down at 60 ℃, and obtaining thickness village liquid is laking agent, and its performance (dyefastness) sees Table 1.
Embodiment 2
Synthesizing of DMAA:
In the 100ml flask, add 45 gram dimethylamine solutions (33%), under 5 ℃ of conditions, alternately drip the propenyl chloride and the aqueous sodium hydroxide solution of same molar, react after 6 hours, product is divided into three layers of oil reservoir, water layer and solid layers, filter, get the upper strata oil reservoir behind the separatory, with obtaining faint yellow pungency liquid after the sodium hydrate solid drying.
Synthesizing of dimethyl diallyl ammonium chloride:
Add the 10ml DMAA and with the propenyl chloride of molar weight, add the 50ml acetone solvent again in the 100ml flask, carry out quaterisation under 60 ℃, react after 34 hours, layering appears in product, and separatory takes off a layer dimethyl diallyl ammonium chloride liquid.
Synthesizing of dimethyl-allyl benzyl ammonium chloride:
Get Benzyl Chloride 9.633g (0.0761mol) in the 50ml there-necked flask, add the 10ml dehydrated alcohol again, get 7.128g DMAA (0.0837mol), be dissolved in the 5ml dehydrated alcohol, add in the constant pressure funnel, one side mouth is loaded onto reflux condensing tube and upper end dress monochlor(in)ate calcium drying tube, live (lucifuge) reaction system with black paper bag then, 60 ℃ of temperature of reaction, DMAA solution dripped off in 8 minutes, 60 ℃ of holding temperatures continue reaction 3 hours, and decompression steams the solvent dehydrated alcohol then, use 10ml anhydrous diethyl ether washing reaction thing 3 times again, make product be solid state, normal pressure steams the small amount of residual anhydrous diethyl ether, obtains the dimethyl-allyl benzyl ammonium chloride after the vacuum-drying.
Synthesizing of laking agent:
Get dimethyl diallyl ammonium chloride 10 grams, 1 gram vinyl silicone oil (molecular weight 950-1050, contents of ethylene are 5wt%), methacrylic benzyl ammonium chloride 2 grams, Hydroxyethyl acrylate 2 grams, K 2S 2O 8Get 0.040 gram as initiator, logical nitrogen protection was reacted 10-15 hour down at 60 ℃, and obtaining thickness village liquid is laking agent, and its performance (dyefastness) sees Table 1.
Embodiment 3
Synthesizing of DMAA:
In the 100ml flask, add 45 gram dimethylamine solutions (33%), under 5 ℃ of conditions, alternately drip the propenyl chloride and the aqueous sodium hydroxide solution of same molar, react after 6 hours, product is divided into three layers of oil reservoir, water layer and solid layers, filter, get the upper strata oil reservoir behind the separatory, with obtaining faint yellow pungency liquid after the sodium hydrate solid drying.
Synthesizing of dimethyl diallyl ammonium chloride:
Add the 10ml DMAA and with the propenyl chloride of molar weight, add the 50ml acetone solvent again in the 100ml flask, carry out quaterisation under 60 ℃, react after 3-4 hour, layering appears in product, and separatory takes off a layer dimethyl diallyl ammonium chloride liquid.
Synthesizing of dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride:
In the 100ml there-necked flask, add the 9ml DMAA, add 50ml acetone and make solvent, the 9ml epoxy chloropropane is added in the dropping funnel, control reaction temperature is at 60 ℃, epoxy chloropropane dripped off in 30 minutes, after reacting 6 hours, layering appears in product, obtains lower floor's viscous liquid product with decantation.
Synthesizing of laking agent
Get dimethyl diallyl ammonium chloride 10 grams, 1 gram vinyl silicone oil (molecular weight 950-1050, contents of ethylene are 5wt%), dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride 2 grams, Hydroxyethyl acrylate 2 grams, K 2S 2O 8Get 0.040 gram as initiator, logical nitrogen protection was reacted 10-15 hour down at 60 ℃, and obtaining thickness village liquid is laking agent, and its performance (dyefastness) sees Table 1.
Embodiment 4
Synthesizing of DMAA:
In the 100ml flask, add 45 gram dimethylamine solutions (33%), under 5 ℃ of conditions, alternately drip the propenyl chloride and the aqueous sodium hydroxide solution of same molar, react after 6 hours, product is divided into three layers of oil reservoir, water layer and solid layers, filter, get the upper strata oil reservoir behind the separatory, with obtaining faint yellow pungency liquid after the sodium hydrate solid drying.
Synthesizing of dimethyl diallyl ammonium chloride
Add the 10ml DMAA and with the propenyl chloride of molar weight, add the 50ml acetone solvent again in the 100ml flask, carry out quaterisation under 60 ℃, react after 3-4 hour, layering appears in product, and separatory takes off a layer dimethyl diallyl ammonium chloride liquid.
Synthesizing of dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride
In the 100ml there-necked flask, add the 9ml DMAA, add 50ml acetone and make solvent, the 9ml epoxy chloropropane is added in the dropping funnel, control reaction temperature is at 60 ℃, epoxy chloropropane dripped off in 30 minutes, after reacting 6 hours, layering appears in product, obtains lower floor's viscous liquid product with decantation.
Synthesizing of methacrylic benzyl ammonium chloride:
Get Benzyl Chloride 9.633g (0.0761mol) in the 50ml there-necked flask, add the 10ml dehydrated alcohol again, get 7.128g DMAA (0.0837mol), be dissolved in the 5ml dehydrated alcohol, add in the constant pressure funnel, one side mouth is loaded onto reflux condensing tube and upper end dress monochlor(in)ate calcium drying tube, live (lucifuge) reaction system with black paper bag then, 60 ℃ of temperature of reaction, DMAA solution dripped off in 8 minutes, 60 ℃ of holding temperatures continue reaction 3 hours, and decompression steams the solvent dehydrated alcohol then, use 10ml anhydrous diethyl ether washing reaction thing 3 times again, make product be solid state, normal pressure steams the small amount of residual anhydrous diethyl ether, obtains the dimethyl-allyl benzyl ammonium chloride after the vacuum-drying.
Synthesizing of laking agent:
Get dimethyl diallyl ammonium chloride 10 grams, 1 gram vinyl silicone oil (molecular weight 950-1050, contents of ethylene are 5wt%), dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride 2 grams, methacrylic benzyl ammonium chloride 2 grams, K 2S 2O 8Get 0.040 gram as initiator, logical nitrogen protection was reacted 10-15 hour down at 60 ℃, and obtaining thickness village liquid is laking agent, and its performance (dyefastness) sees Table 1.
Embodiment 5
Synthesizing of DMAA:
In the 100ml flask, add 45 gram dimethylamine solutions (33%), under 5 ℃ of conditions, alternately drip the propenyl chloride and the aqueous sodium hydroxide solution of same molar, react after 6 hours, product is divided into three layers of oil reservoir, water layer and solid layers, filter, get the upper strata oil reservoir behind the separatory, with obtaining faint yellow pungency liquid after the sodium hydrate solid drying.
Synthesizing of dimethyl diallyl alkyl ammomium chloride:
Add the 10ml DMAA and with the propenyl chloride of molar weight, add the 50ml acetone solvent again in the 100ml flask, carry out quaterisation under 60 ℃, react after 3-4 hour, layering appears in product, and separatory takes off a layer dimethyl diallyl ammonium chloride liquid.
Synthesizing of dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride:
In the 100ml there-necked flask, add the 9ml DMAA, add 50ml acetone and make solvent, the 9ml epoxy chloropropane is added in the dropping funnel, control reaction temperature is at 60 ℃, epoxy chloropropane dripped off in 30 minutes, after reacting 6 hours, layering appears in product, obtains lower floor's viscous liquid product with decantation.
Synthesizing of hexadecyldimethyl benzyl ammonium allyl ammonium chloride:
Get Virahol 100ml and place flask to make solvent, get hexadecyldimethyl benzyl ammonium tertiary amine 20ml and propenyl chloride 25ml, logical nitrogen protection, reaction is after 6-8 hour down at 60 ℃, and behind activated carbon decolorizing, the choosing steaming obtains weak yellow liquid after removing and desolvating.
Synthesizing of laking agent:
Get dimethyl diallyl ammonium chloride 10 grams, 1 gram vinyl silicone oil (molecular weight 950-1050, contents of ethylene are 5wt%), dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride 2 grams, hexadecyldimethyl benzyl ammonium allyl ammonium chloride 2 grams, K 2S 2O 8Get 0.040 gram as initiator, logical nitrogen protection was reacted 10-15 hour down at 60 ℃, and obtaining thickness village liquid is laking agent, and its performance (dyefastness) sees Table 1.
Embodiment 6
Synthesizing of DMAA:
In the 100ml flask, add 45 gram dimethylamine solutions (33%), under 5 ℃ of conditions, alternately drip the propenyl chloride and the aqueous sodium hydroxide solution of same molar, react after 6 hours, product is divided into three layers of oil reservoir, water layer and solid layers, filter, get the upper strata oil reservoir behind the separatory, with obtaining faint yellow pungency liquid after the sodium hydrate solid drying.
Synthesizing of dimethyl diallyl alkyl ammomium chloride
Add the 10ml DMAA and with the propenyl chloride of molar weight, add the 50ml acetone solvent again in the 100ml flask, carry out quaterisation under 60 ℃, react after 3-4 hour, layering appears in product, and separatory takes off a layer dimethyl diallyl ammonium chloride liquid.
Synthesizing of dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride:
In the 100ml there-necked flask, add the 9ml DMAA, add 50ml acetone and make solvent, the 9ml epoxy chloropropane is added in the dropping funnel, control reaction temperature is at 60 ℃, epoxy chloropropane dripped off in 30 minutes, after reacting 6 hours, layering appears in product, obtains lower floor's viscous liquid product with decantation.
Synthesizing of methacrylic benzyl ammonium chloride:
Get Benzyl Chloride 9.633g (0.0761mol) in the 50ml there-necked flask, add the 10ml dehydrated alcohol again, get 7.128g DMAA (0.0837mol), be dissolved in the 5ml dehydrated alcohol, add in the constant pressure funnel, one side mouth is loaded onto reflux condensing tube and upper end dress monochlor(in)ate calcium drying tube, live (lucifuge) reaction system with black paper bag then, 60 ℃ of temperature of reaction, DMAA solution dripped off in 8 minutes, 60 ℃ of holding temperatures continue reaction 3 hours, and decompression steams the solvent dehydrated alcohol then, use 10ml anhydrous diethyl ether washing reaction thing 3 times again, make product be solid state, normal pressure steams the small amount of residual anhydrous diethyl ether, obtains the dimethyl-allyl benzyl ammonium chloride after the vacuum-drying.
Synthesizing of laking agent:
Get dimethyl diallyl ammonium chloride 10 grams, 1 gram vinyl silicone oil (molecular weight 950-1050, contents of ethylene are 5wt%), dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride 2 grams, methacrylic benzyl ammonium chloride 2 grams, Hydroxyethyl acrylate 2 grams, K 2S 2O 8Get 0.040 gram as initiator, logical nitrogen protection was reacted 10-15 hour down at 60 ℃, and obtaining thickness village liquid is laking agent, and its performance (dyefastness) sees Table 1.
Embodiment 7
Synthesizing of methacrylic amine:
In the 100ml flask, add 45 gram dimethylamine solutions (33%), under 5 ℃ of conditions, alternately drip the propenyl chloride and the aqueous sodium hydroxide solution of same molar, react after 6 hours, product is divided into three layers of oil reservoir, water layer and solid layers, filter, get the upper strata oil reservoir behind the separatory, with obtaining faint yellow pungency liquid after the sodium hydrate solid drying.
Synthesizing of dimethyl diallyl alkyl ammomium chloride:
Add the 10ml DMAA and with the propenyl chloride of molar weight, add the 50ml acetone solvent again in the 100ml flask, carry out quaterisation under 60 ℃, react after 3-4 hour, layering appears in product, and separatory takes off a layer dimethyl diallyl ammonium chloride liquid.
Synthesizing of hexadecyldimethyl benzyl ammonium allyl ammonium chloride:
Get Virahol 100ml and place flask to make solvent, get hexadecyldimethyl benzyl ammonium tertiary amine 20ml and propenyl chloride 25ml, logical nitrogen protection, reaction is after 6-8 hour down at 60 ℃, and behind activated carbon decolorizing, the choosing steaming obtains weak yellow liquid after removing and desolvating.
Synthesizing of dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride:
In the 100ml there-necked flask, add the 9ml DMAA, add 50ml acetone and make solvent, the 9ml epoxy chloropropane is added in the dropping funnel, control reaction temperature is at 60 ℃, epoxy chloropropane dripped off in 30 minutes, after reacting 6 hours, layering appears in product, obtains lower floor's viscous liquid product with decantation.
Synthesizing of laking agent:
Get dimethyl diallyl ammonium chloride 10 grams, 1 gram vinyl silicone oil (molecular weight 950-1050, contents of ethylene are 5wt%), dimethyl-allyl (2-hydroxyl-3-chlorine) propyl ammonium chloride 2 grams, hexadecyldimethyl benzyl ammonium allyl ammonium chloride 2 grams, Hydroxyethyl acrylate 2 grams, K 2S 2O 8Get 0.040 gram as initiator, logical nitrogen protection was reacted 10-15 hour down at 60 ℃, and obtaining thickness village liquid is laking agent, and its performance (dyefastness) sees Table 1.
Table 1:
Figure A20081004016700111
Annotate:
1. multiple, the Shi Lixin of Cui Lian. the production of color fixing agent Y and application [J]. Shenyang chemical industry .1991,2:37-39.
2. positively charged ion, Organosilicon dye fixing agent of reaction type and its preparation method (CN1583763).

Claims (5)

1, a kind of laking agent, it is characterized in that said laking agent is 1 by compound shown in compound shown in vinylsiloxane, the formula I and the formula II by mass ratio mainly: (2~10): 10, under 30 ℃~80 ℃ conditions, make initiator with Potassium Persulphate, copolymerization obtained in 5~20 hours;
Figure A2008100401670002C1
Wherein: R 1And R 2Independently be selected from C respectively 1~C 6A kind of in the alkyl, R 3Be C 1~C 16The C of alkyl or replacement 1~C 16Alkyl, X are halogen;
The C of said replacement 1~C 16Substituting group in the alkyl is selected from: halogen, a kind of in hydroxyl or the phenyl, two or more.
2, laking agent as claimed in claim 1 is characterized in that, wherein the molecular weight of said vinylsiloxane is 950~1200, the content of vinyl is 5wt%~10wt%.
3, laking agent as claimed in claim 1 is characterized in that, wherein polymeric reaction temperature is 60 ℃~80 ℃, and polymerization reaction time is 10-15 hour.
4, as any described laking agent in the claim 1~3, it is characterized in that, wherein R 1And R 2Independently be selected from C respectively 1~C 3A kind of in the alkyl.
5, laking agent as claimed in claim 4 is characterized in that, wherein R 3Be benzyl, hexadecyl or 2-hydroxyl, 3-chloro-propyl group.
CN2008100401675A 2008-07-03 2008-07-03 Non-formaldehyde organosilicon color fixing agent Expired - Fee Related CN101302268B (en)

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