CN101768883A - Preparation method of formaldehyde-free active dye fixing agent - Google Patents
Preparation method of formaldehyde-free active dye fixing agent Download PDFInfo
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Abstract
The invention relates to a preparation method of a formaldehyde-free active dye fixing agent. The compound prescription of the active dye fixing agent consists of two components, component 1 is chitosan quaternary ammonium salt produced by 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride grafted with chitosan under ultrasonic, and component 2 is reactive fixing agent produced after reaction of one weight part of triethylene tetramine and three weight parts of epoxy chloropropane; the mass ratio of the component 1 and the component 2 is 1:3. The method of the invention can be applied to fixing treatment of cotton fabric dyed by active dye, can improve rubbing fastness, washing fastness and light fastness of the fabric without influence on the chromatic light and the fabric hand feel; the prepared fixing agent which is free from formaldehyde, nontoxic and environment-friendly is a novel printing and dyeing assistant.
Description
Technical field:
The present invention relates to a kind of preparation method of formaldehyde-free active dye fixing agent, belong to novel printing and dyeing assistant technical field.Can be applicable to the fixation treatment of Dyeing of Cotton Fabric with Reactive Dyes fabric.
Background technology:
At present, the COTTON FABRIC used dye species that dyes is more, and kinds such as reducing dye, direct dyes, SULPHUR DYES, REACTIVE DYES are arranged.Fastness was better after reducing dye made cotton dyeing, but cost an arm and a leg, and the used reductant price that dyes is also higher, and the dyeing complexity, and the dyeing cost is than much higher with other dyestuffs; Direct dyes combine with fiber because of only depending on Van der Waals force, hydrogen bond, and the adhesion of dyestuff and fiber is less, and its fastness to wet rubbing is relatively poor; SULPHUR DYES (containing liquid sulfurate dye) is when dying dark color, and fastness to wet rubbing is also undesirable; The REACTIVE DYES chromatogram is complete, bright in colour, with low cost, easy to use, becomes the wider cotton of application and uses dyestuff, and its demand increases year by year.Yet, increase along with REACTIVE DYES is used also exposes following point: (1) causes the decline of cotton dyeing degree of fixation owing to do not anchor at free dye on the cotton fiber and the existence of hydrolysed reactive dye, washing performance is relatively poor, and the consumption of dye well water, electricity, vapour increases; (2) REACTIVE DYES combines with fiber with covalent bond, though fastness is stronger, but in dying, when dark, fastness to wet rubbing is lower, its product dyed thereby is under the influence of factors such as bleaching agent, heat, sour gas and water at daylight, sweat, active chlorine, oxygen, easily causes variable color, fades, discolors and move look and contamination with wash.REACTIVE DYES when particularly dying heavy colour, tends to make a large amount of not REACTIVE DYES of set of existence on the DYED FABRICS because of dye strength is too high in dyeing course, and this part dyestuff will fade in washing process; Simultaneously, formed chemical bond facile hydrolysis fracture causes wet colour fastness lower between some active group and fiber.So, just need use the color-fixing agent fixation in order to prevent fading of dyestuff on the fabric.In the color-fixing agent of REACTIVE DYES, reactive cross-linking type color-fixing agent is the reasonable veriety of effect, and it can form macromolecule polyalcohol with the REACTIVE DYES reaction, reaches the purpose that improves dyefastness.The degree of fixation of general REACTIVE DYES only is 60-70%, for the dyestuff user, in order to guarantee REACTIVE DYES good fastness is arranged, just must be by means of color-fixing agent.Wherein comparatively desirable with dicyandiamide formaldehyde resin and cupric dicyandiamide formaldehyde resin colour fixation, and to form commercialization production gradually be Colourfix Y and Coprantex B (developing into homemade color fixing agent Y and color fixing agent M afterwards).The beginning of the fifties, REACTIVE DYES was come out, and foretold inside door chemical company soon and proposed patent, handled with cationic fixing agent and acidulous material, can improve the wet colour fastness of REACTIVE DYES.From then on, the kind of color-fixing agent is more and more, but since half a century, the chemical constitution of color-fixing agent seldom has improvement.Entered twentieth century since the eighties; enhancing along with environmental protection consciousness; containing the shortcoming that exists in the aldehyde color-fixing agent also comes out gradually; as the look that causes product dyed thereby easily become, feel is coarse, particularly free formaldehyde content is higher, it can stimulate human body skin; make pruitus; even make skin produce canceration, also have the possibility of teratogenesis, therefore controlled use.At present, states such as European Union, the U.S. and Japan have all formulated strict rules in succession, the free formaldehyde concentration on the restriction textiles.World textile market has also proposed new requirement to the fastness of product dyed thereby in recent years, as German Eco-Tex and Oeko-Tex the fastness to washing of fabric is required to reach the 3-4 level.Product dyed thereby after fixation treatment not only will have fastness such as the soaping of certain grade, washing, rub resistance, perspiration resistance, sun-resistant, anti-chlorine float, but also require not contain formaldehyde, nontoxic, do not influence fabric feeling and look change etc.Therefore in order to overcome problems such as wet rubbing fastness of reactive dye is undesirable, and the formaldehyde mass fraction on the restriction textiles, it is necessary to use formaldehyde-free color fixing agent to improve the dyefastness of cotton reactive dye.
At present, patent and document are not reported the compounding method of the new reactive dyes color-fixing agent that the present invention relates to as yet both at home and abroad, and this formaldehydeless novel color-fixing agent is with a wide range of applications and prospect aspect textile finishing.
Summary of the invention:
The objective of the invention is to overcome the defective of prior art, a kind of preparation method of novel formaldehyde-free active dye fixing agent is provided, this method comprises the synthetic method and the compounded formula of two kinds of components in the color-fixing agent, can improve crock fastness, washing fastness and the light fastness of COTTON FABRIC after reactive dyeing, and do not influence coloured light, safe, nontoxic, environmental protection.
The preparation method of formaldehyde-free active dye fixing agent of the present invention, the compounded formula of its active dye fixing agent is that the mass ratio of component 1 and component 2 is 1: 3 by two kinds of composite forming of component; Wherein component 1 is 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride resulting chitosan quaternary ammonium salt of grafted chitosan under the ultrasonic wave effect, and component 2 is response type color-fixing agent that 1 weight portion triethylene tetramine and 3 weight portion epichlorohydrin reactions obtain.
The preparation method of formaldehyde-free active dye fixing agent of the present invention, operate according to following steps:
1, the shitosan adding with 1 weight portion contains 1 weight portion sodium hydrate aqueous solution, isopropyl alcohol is a solvent, be heated to 55 ℃ under stirring, behind the constant temperature alkalization 4h again water-bath be heated to 60 ℃, reaction vessel is placed on the ultrasonic washing instrument, under 100W power, act on, drip the solution of the 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride of 6 weight portions, the control drop rate drips off the back 70 ℃ of following isothermal reaction dischargings after 3 hours; Slip is adjusted to suction filtration behind the pH=7.0 with the hydrochloric acid of ω=0.1, and filter residue continues to wash suction filtration (three times repeatedly) with soaked in absolute ethyl alcohol with the ethanol water washing by soaking and the suction filtration (three times repeatedly) of 60ml ω=0.85; At last material is placed air dry oven, be not higher than under 70 ℃ in temperature and be dried to constant weight, obtain component 1.The molecular weight of used shitosan is about 30000, and deacetylation is more than 90%.
The main reaction equation is as follows:
2, under 60 ℃ the bad oxygen chloropropane of 3 weight portions slowly is added dropwise in the aqueous solution that contains 1 weight portion triethylene tetramine, stirring reaction 30min obtains the light yellow clarifying liquid body, transfers pH to neutral with acetic acid again, obtains component 2.
The main reaction equation is as follows:
3, when REACTIVE DYES institute dyeing cotton fabric is carried out fixation, by 1: 3 mass ratio component 1 and component 2 preparation fixation are bathed, the color-fixing agent consumption is with respect to 3% of DYED FABRICS weight, it is neutral regulating pH, 60 ℃ of temperature, bath raio were 1: 15 (fabric and the mass ratio that adds the fixation liquid of final preparation behind the water), with DYED FABRICS fixation treatment 30 minutes, take out oven dry, and wash.
The inventive method is mainly used in the fixation treatment of Dyeing of Cotton Fabric with Reactive Dyes fabric.This method can improve crock fastness, washing fastness and the light fastness of fabric, and does not influence coloured light and fabric feeling, and the color-fixing agent that makes does not contain formaldehyde, and nontoxic, environmental protection is a kind of novel printing and dyeing assistant.
The specific embodiment:
Below in conjunction with specific embodiment the inventive method is further specified.
Embodiment 1: the COTTON FABRIC of selecting reactive brilliant red x-3b dyeing for use.
(1) 1 weight portion shitosan adds and contains 1 weight portion sodium hydrate aqueous solution, isopropyl alcohol is a solvent, be heated to 55 ℃ under stirring, behind the constant temperature alkalization 4h again water-bath be heated to 60 ℃, reaction vessel is placed on the ultrasonic washing instrument, under 100W power, act on, drip the solution of the 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride of 6 weight portions, the control drop rate drips off 70 ℃ of following isothermal reaction dischargings after 3 hours; Slip is adjusted to suction filtration behind the pH=7.0 with the hydrochloric acid of ω=0.1, and filter residue continues to wash suction filtration (three times repeatedly) with soaked in absolute ethyl alcohol with the ethanol water washing by soaking and the suction filtration (three times repeatedly) of 60ml ω=0.85; At last material is placed air dry oven, be not higher than under 70 ℃ in temperature and be dried to constant weight, obtain component 1.The molecular weight of used shitosan is about 30000, and deacetylation is more than 90%.
(2) under 60 ℃ the epoxychloropropane of 3 weight portions slowly is added dropwise in the aqueous solution that contains 1 weight portion triethylene tetramine, stirring reaction 30min obtains the light yellow clarifying liquid body, transfers pH to neutral with acetic acid again, obtains component 2.
(3) by 1: 3 mass ratio component 1 and component 2 configuration fixation are bathed, the color-fixing agent consumption is 3% (heavy to DYED FABRICS), it is neutral regulating pH, 60 ℃ of temperature; bath raio is 1: 15 (fabric and the mass ratio that adds the fixation liquid of final preparation behind the water);, take out oven dry, and wash with DYED FABRICS fixation treatment 30 minutes.
The dependence test method: fastness to rubbing is pressed the GB/T3920-2002 test; Color fastness to washing is pressed GB/T 3921.1-2002 test.Change color is a benchmark with the cloth without fixation treatment, grades with gray scale GB250-1995 and grey scale for assessing staining of colour GB251-1995 with the evaluation variable color.The test light fastness, cloth to be measured is covered each 3 centimetres at two ends with lighttight black card, be flat on 60cm place under the uviol lamp then, open the light source irradiation and be placed on dark place in 8 hours 2 hours, observe the situation of fading of fabric, select the COTTON FABRIC of reactive brilliant red x-3b dyeing for use.The result is as follows:
Table-1
From table-1 as can be seen, chitosan quaternary ammonium salt pair REACTIVE DYES reactive brilliant red x-3b has colour fixation preferably, and every fastness can improve about half grade substantially.
Embodiment 2:
Select reactive brilliant bule X-B for use
RThe COTTON FABRIC of dyeing.
(1) 1 weight portion shitosan adds and contains 1 weight portion sodium hydrate aqueous solution, isopropyl alcohol is a solvent, be heated to 55 ℃ under stirring, behind the constant temperature alkalization 4h again water-bath be heated to 60 ℃, reaction vessel is placed on the ultrasonic washing instrument, under 100W power, act on, drip the solution of the 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride of 6 weight portions, the control drop rate drips off 70 ℃ of following isothermal reaction dischargings after 3 hours; Slip is adjusted to suction filtration behind the pH=7.0 with the hydrochloric acid of ω=0.1, and filter residue continues to wash suction filtration (three times repeatedly) with soaked in absolute ethyl alcohol with the ethanol water washing by soaking and the suction filtration (three times repeatedly) of 60ml ω=0.85; At last material is placed air dry oven, be not higher than under 70 ℃ in temperature and be dried to constant weight, obtain component 1.The molecular weight of used shitosan is about 30000, and deacetylation is more than 90%.
(2) under 60 ℃ the epoxychloropropane of 3 weight portions slowly is added dropwise in the aqueous solution that contains 1 weight portion triethylene tetramine, stirring reaction 30min obtains the light yellow clarifying liquid body, transfers pH to neutral with acetic acid again, obtains component 2.
(3) by 1: 3 mass ratio component 1 and component 2 configuration fixation are bathed, the color-fixing agent consumption is 3% (heavy to DYED FABRICS), it is neutral regulating pH, 60 ℃ of temperature; bath raio is 1: 15 (fabric and the mass ratio that adds the fixation liquid of final preparation behind the water);, take out oven dry, and wash with DYED FABRICS fixation treatment 30 minutes.
Method of testing is selected reactive brilliant bule X-B for use with embodiment 1
RThe COTTON FABRIC of dyeing, the result is as follows:
Table-2
From table-2 as can be seen, chitosan quaternary ammonium salt pair REACTIVE DYES reactive brilliant bule X-B
RColour fixation is preferably arranged, and every fastness can improve about half grade substantially.
Embodiment 3:
Select the COTTON FABRIC of reactive brilliant yellow K-6G dyeing for use.
(1) 1 weight portion shitosan adds and contains 1 weight portion sodium hydrate aqueous solution, isopropyl alcohol is a solvent, be heated to 55 ℃ under stirring, behind the constant temperature alkalization 4h again water-bath be heated to 60 ℃, reaction vessel is placed on the ultrasonic washing instrument, under 100W power, act on, drip the solution of the 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride of 6 weight portions, the control drop rate drips off 70 ℃ of following isothermal reaction dischargings after 3 hours; Slip is adjusted to suction filtration behind the pH=7.0 with the hydrochloric acid of ω=0.1, and filter residue continues to wash suction filtration (three times repeatedly) with soaked in absolute ethyl alcohol with the ethanol water washing by soaking and the suction filtration (three times repeatedly) of 60ml ω=0.85; At last material is placed air dry oven, be not higher than under 70 ℃ in temperature and be dried to constant weight, obtain component 1.The molecular weight of used shitosan is about 30000, and deacetylation is more than 90%.
(2) under 60 ℃ the epoxychloropropane of 3 weight portions slowly is added dropwise in the aqueous solution that contains 1 weight portion triethylene tetramine, stirring reaction 30min obtains the light yellow clarifying liquid body, transfers pH to neutral with acetic acid again, obtains component 2.
(3) by 1: 3 mass ratio component 1 and component 2 configuration fixation are bathed, the color-fixing agent consumption is 3% (heavy to DYED FABRICS), it is neutral regulating pH, 60 ℃ of temperature; bath raio is 1: 15 (fabric and the mass ratio that adds the fixation liquid of final preparation behind the water);, take out oven dry, and wash with DYED FABRICS fixation treatment 30 minutes.
Method of testing is selected the COTTON FABRIC of reactive brilliant yellow K-6G dyeing for use with embodiment 1, and the result is as follows:
Table-3
From table-3 as can be seen, chitosan quaternary ammonium salt pair REACTIVE DYES reactive brilliant yellow K-6G has colour fixation preferably, and every fastness can improve about half grade substantially.
Claims (2)
1. the preparation method of a formaldehyde-free active dye fixing agent is characterized in that the compounded formula of color-fixing agent is made up of two kinds of components, and the mass ratio of component 1 and component 2 is 1: 3; Wherein component 1 is 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride resulting chitosan quaternary ammonium salt of grafted chitosan under the ultrasonic wave effect, component 2 is response type color-fixing agent that 1 weight portion triethylene tetramine and 3 weight portion epichlorohydrin reactions obtain, operate according to following steps: the shitosan adding of 1 weight portion is contained 1 weight portion sodium hydrate aqueous solution, isopropyl alcohol is a solvent, be heated to 55 ℃ under stirring, behind the constant temperature alkalization 4h again water-bath be heated to 60 ℃, reaction vessel is placed on the ultrasonic washing instrument, under 100W power, act on, drip the solution of the 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride of 6 weight portions, the control drop rate drips off the back 70 ℃ of following isothermal reaction dischargings after 3 hours; Slip is adjusted to suction filtration behind the pH=7.0 with the hydrochloric acid of ω=0.1, and filter residue three times repeatedly, continues to wash suction filtration with soaked in absolute ethyl alcohol, three times repeatedly with the ethanol water washing by soaking and the suction filtration of 60ml ω=0.85; At last material is placed air dry oven, be not higher than under 70 ℃ in temperature and be dried to constant weight, obtain component 1; Under 60 ℃ 3 weight portion epoxychloropropane slowly are added dropwise in the aqueous solution that contains 1 weight portion triethylene tetramine, stirring reaction 30min obtains the light yellow clarifying liquid body, transfers pH to neutral with acetic acid again, obtains component 2; When REACTIVE DYES institute dyeing cotton fabric is carried out fixation, by 1: 3 mass ratio component 1 and component 2 preparation fixation are bathed, the color-fixing agent consumption is with respect to 3% of DYED FABRICS weight, and it is neutral regulating pH, 60 ℃ of temperature, fabric is 1: 15 with the mass ratio that adds the fixation liquid of finally preparing behind the water.
2. the preparation method of a kind of formaldehyde-free active dye fixing agent according to claim 1, the molecular weight that it is characterized in that used shitosan is 30000, deacetylation is more than 90%.
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| CN115852719A (en) * | 2022-09-30 | 2023-03-28 | 浙江越新印染有限公司 | Silicon-containing color fixing additive and application thereof in cotton printing and dyeing |
| CN115852719B (en) * | 2022-09-30 | 2024-03-26 | 浙江越新印染有限公司 | Silicon-containing color fixing auxiliary agent and application thereof in cotton printing and dyeing |
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