CN100350097C - Manufacturing technology of formaldehydeless colour fixing agent - Google Patents
Manufacturing technology of formaldehydeless colour fixing agent Download PDFInfo
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- CN100350097C CN100350097C CNB031140017A CN03114001A CN100350097C CN 100350097 C CN100350097 C CN 100350097C CN B031140017 A CNB031140017 A CN B031140017A CN 03114001 A CN03114001 A CN 03114001A CN 100350097 C CN100350097 C CN 100350097C
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Abstract
The present invention discloses a manufacturing technology of a formaldehyde-less colour fixing agent, wherein the colour fixing agent is prepared form diethylenetriamine AE and epoxy chloropropane EP. The present invention is characterized in that the preparation technology of the formaldehyde-less colour fixing agent adopts the following steps: a, a certain amount of water and diethylenetriamine AE are added to a reactor to be stirred; b, the epoxy chloropropane EP is dropped and added, and the temperature is controlled to be less then 50 DEG C; c, the temperature is raised to 55 DEG C to 65 DEG C, the heat insulation is carried out for 0.5 to 2 hours, the temperature is then raised to 75 DEG C to 90 DEG C, and the heat-insulation reaction is carried out for 20 to 40 minutes; d, a sample is taken for testing the viscosity of a product which is cooled to the room temperature after being qualified, and then the product is discharged so that a finished product is obtained. The colour fixing agent manufactured by the present invention has the advantage of good colour fixation and colour fixing effect and accords with the requirement of environmental protection without containing formaldehyde.
Description
Technical field
The present invention relates to a kind of color-fixing agent that is used for reactive dyeing.
Background technology
The dyeing of COTTON FABRIC mainly is based on reactive dyeing at present, owing to contain hydrophilic radicals such as sulfonic group, carboxylic acid group in the reactive dyestuff molecule structure, it is limited to tend to the amount of dye that takes place because of its set of excessive concentration when dying dark color, make the dyestuff that is had a large amount of not sets on the dyeing cotton fabric, cause dyefastness defective, wet colour fastness is poor, need improve by the dyefastness of dyeing cotton fabric with color-fixing agent.Past, the general formaldehyde color-fixing agent that contains that adopts improved dyefastness, and was outstanding because of its fixing property, and economical and practically used producer to welcome deeply.But people's environmental consciousness constantly strengthens in recent years, and the America and Europe waits some countries to put into effect the pertinent regulations of the free formaldehyde content on the restriction textiles in succession, limits free content of formaldehyde on the textiles, and for example the underwear content of formaldehyde is limited in 20 * 10
-6In the ppm, the coat content of formaldehyde is limited in 300 * 10
-6In the ppm.Make the color-fixing agent that contains formaldehyde be eliminated one after another, printing and dyeing producer grows with each passing day to the demand of aldehyde-free colour stabilizer.Also the someone adopts formaldehydeless color-fixing agent, as number of patent application be 01119412, the applying date is that May 24 calendar year 2001, denomination of invention are the patent application of environment protection type color fixing agent, this environment protection type color fixing agent is made up of chitin, high-efficient penetrant OP-6, fatty alcohol-polyoxyethylene ether, water.Though above-mentioned color-fixing agent does not contain formaldehyde, has solved environmental issue, its fixing property and effect are not ideal again.
Summary of the invention
The object of the present invention is to provide a kind of fixing property and colour fixation are good, do not contain formaldehyde environmental protection color-fixing agent and process for making.
In order to achieve the above object, the present invention adopts following scheme to realize: this color-fixing agent is formulated by diethylenetriamine AE and epoxychloropropane EP, and its preparing process step is as follows:
A) get certain water gaging and diethylenetriamine AE and add in the reactor, stir;
B) drip epoxychloropropane EP, the control temperature is below 50 ℃;
C) heat to 55～65 ℃, and be incubated 0.5～2 hour; Heat to 75～90 ℃ insulation reaction 20～40 minutes again;
D) sampling and testing product viscosity is cooled to room temperature after qualified, and discharging gets product.
The color-fixing agent that adopts above-mentioned composition and process to make, can satisfy and use the client high-quality formaldehydeless demand, through application test, verified its colour fixation to the reactive dyeing fabric, the result shows: this aldehyde-free colour stabilizer FIX500 can substitute the fixation treatment that color fixing agent Y is applied to the COTTON FABRIC of reactive dyeing.
Fixation mechanism according to color-fixing agent; color-fixing agent will have positive lotus property on chemical constitution; has reactive crosslinked group; can be crosslinked voluntarily and molecular weight even as big as in drying course, forming diaphragm; and contain the building stone that has compatibility with dye molecule, also should have precipitation and complexing metal ion.In addition, for formaldehyde-free color fixing agent, require not use the raw material that contains formaldehyde when producing, production process and use can not produce formaldehyde, after the fixation treatment by dyeing and weaving thing also Diazolidinyl Urea not.Formaldehyde-free color fixing agent of the present invention belongs to cross-linking reaction type color-fixing agent, and the quaternary ammonium salt or the tertiary amine salt of some is arranged in its molecule, has the positive lotus property of certain intensity; This product does not contain formaldehyde, produce and use in also Diazolidinyl Urea not.
Be described further below in conjunction with embodiment:
The specific embodiment
The raw material that the present invention adopts: diethylenetriamine AE, epoxychloropropane EP;
Laboratory apparatus device: the four-hole boiling flask of electric blender, thermometer, condenser pipe, dropping funel is housed, the temperature self-controlled electric fireless cooker;
Its synthesis technique is: certain water gaging and diethylenetriamine AE are added in the reaction vessel, after stirring a period of time, drip epoxychloropropane EP, temperature is controlled at below 50 ℃, after dropwising, and heat temperature raising to 60 ℃, insulation reaction one hour, heat temperature raising to 80 ℃ again, insulation reaction 30 minutes.The sampling and testing product viscosity is cooled to room temperature after qualified, and discharging gets product.Product is the transparent liquid of yellow green, and is soluble in water, pH value 5～6.
In building-up process, carried out changing the be with reactive crosslinked group quantity of the amount of diethylenetriamine AE and epoxychloropropane EP than the positive lotus property of adjusting color-fixing agent and raising color-fixing agent respectively by Orthogonal Method, control reaction temperature and time are to increase the test of color-fixing agent molecular weight.Best proportioning and the optimum synthesis condition of above-mentioned aldehyde-free colour stabilizer FIX500 have finally been determined.
We find in experimentation, (1) the positive lotus property of color-fixing agent is strong more, improved obvious more by the soaping fastness of dyeing and weaving thing and perspiration fastness, and other dyefastness raising is not obvious, this is to have formed the color lake because the positive lotus property of color-fixing agent combines with ionic bond with the negative charge of REACTIVE DYES, thereby improved by the soaping fastness of dyeing and weaving thing and perspiration fastness, improve as for other dyefastness not obvious, illustrated improve REACTIVE DYES to be not only the positive electricity that relies on color-fixing agent by the dyefastness of dyeing and weaving thing with the negative charge of REACTIVE DYES with the ionic bond formed color lake that combines.(2) molal quantity of epoxychloropropane EP in the increasing proportioning, the reactive crosslinked group that increases color-fixing agent helps to improve the crock fastness of pollutant, this is because the color lake that color-fixing agent and REACTIVE DYES form mechanically is adsorbed on the fiber surface, (OH) reaction forms covalent bond to hydroxyl in the color-fixing agent on reactive crosslinked group and the gossypin molecule, also with reactive dyestuff molecule on imido grpup (NH-) go up the reactive hydrogen atom reaction and form covalent bond, thereby strengthened the adhesion between color-fixing agent and REACTIVE DYES and the fiber, improved by the crock fastness of dyeing and weaving thing.If but do not have the amount of the increase epoxychloropropane EP place restrictions on, the cross-linking reaction group surpass a certain amount of after, its colour fixation descends on the contrary to some extent because EP is many more, the molecular weight of color-fixing agent but can not improve, just and low-molecular material can increase, thereby reduced colour fixation.(3) improve reaction temperature and increase the reaction time, improve the molecular weight of color-fixing agent, make color-fixing agent in drying course, form diaphragm, further improve by the soaping fastness of dyeing and weaving thing, perspiration fastness, water logging fastness and crock fastness.
Adopt the color-fixing agent of above-mentioned manufacturing technique, through following application testing:
1, method of testing
Crock fastness is pressed GB3920-83 textiles colour fastness to rubbing test method:
Soaping fastness is pressed GB3921-83 textiles color fastness to washing test method;
GB3922-83 textiles colour fastness to perspiration test method is pressed in perspiration fastness:
Fade, staining gray scale rating;
2, experiment material
Bleached cotton cloth, reactive red 3BX, active blue KN-G, salt (technical grade), soda ash (technical grade), color fixing agent Y (our factory's production), aldehyde-free colour stabilizer FIX500,24% ammoniacal liquor (technical grade), 10% acetic acid (technical grade)
2, dye process
REACTIVE DYES 20g/l crosses padding machine, in 120 ℃ * 5min oven dry, crosses decatize liquid (salt 250g/l+40g/l soda ash), again in 120 ℃ of decatizes 5 minutes.
4, color fixing process condition and color fixing process process
The infusion process fixation: color-fixing agent consumption 2% (owf), bath raio 1: 20, time 10～15min, the working solution pH value is a normal temperature for neutral, temperature.The working solution pH value of color fixing agent Y is 5 (regulating with acetic acid).
Dipping color fixing process process: fixation → dehydration → oven dry (120 ℃).
5, color fixation fastness test
5.1 water logging fastness
[8]
Cut the sample cloth of 5 * 8cm, sew on tenderly white cotton in the front, put into 50ml (30 ± 5 ℃) distilled water dipping and take out after 6 hours, separately cloth specimen and staining cloth are put into 40 ℃ of baking ovens and are dried.With fade, staining gray scale rating.
5.2 soaping fastness
Cut 5 * 10cm sample cloth, sew on tenderly white cotton in the front, put into 100ml (95 ± 5 ℃) liquid of soaping (the strange board washing powder 4g/l+ soda ash 2g/l of wave) and handle 30min (when 10min, 20min, acutely shaking 10 times respectively), take out and separate staining cloth 40 ℃ of oven dry.With fade, staining gray scale rating.
5.3 perspiration fastness
Cut the sample cloth of 5 * 5cm, sew on the tenderly white cotton of same specification in the front, put into 40ml (37 ± 2 ℃) treatment fluid (salt 5g/l+24% ammoniacal liquor 6ml/l) and handle 30min, the two sides of clamping cloth specimen during processing with two sheet glass.After disposing, take out cloth specimen and extract, add 10% acetic acid 2.8ml and handle 30min in 37 ± 2 ℃ again.Take out and separate staining cloth 40 ℃ of oven dry.With fade, staining gray scale rating.
5.4 crock fastness
Get two of the sample cloth (do respectively to do wet friction test with) of 8 * 25cm, lie on the dull and stereotyped greasy fabric of crock fastness testing machine above.Bleach cotton fine cloth with 5 * 5cm and wrap on this machine friction circle column cap, make sarashi kanakin warp, latitude direction intersect 45 (diameter of socket cap rubbing surface is 1.5cm, is 1 kilogram to the cloth gross pressure, and traverse is 10cm during friction) with the direction of warp and weft of test cloth.On sample cloth, rub about back and forth at every turn 1 second back and forth 10 times.A sample cloth should rub respectively three times everywhere in the warp-wise front, presses the grey scale for staining rating then.Wet friction test calico should be graded after the drying in room temperature or below 40 ℃ again.
6, test result sees Table 1
Table 1 Dyeing of Cotton Fabric with Reactive Dyes colour fixation sample test result
| Dye species | Reactive red 3BX | Active blue KN-G | |||||
| The project indicator | Color-fixing agent | Blank test | Color fixing agent Y | Color-fixing agent FIX500 | Blank test | Color fixing agent Y | Color-fixing agent FIX500 |
| Crock fastness | Dry friction | 2 | 4 | 4 | 3～4 | 4 | 4 |
| Wet friction | 2 | 2～3 | 2～3 | 2 | 2～3 | 3 | |
| Soaping fastness | Former cloth fades | 3～4 | 3～4 | 4～5 | 2 | 2 | 3～4 |
| Calico staining | 3 | 4 | 4～5 | 2 | 2 | 2～3 | |
| Perspiration fastness | Former cloth fades | 3～4 | 3～4 | 4～5 | 3 | 3～4 | 3～4 |
| Calico staining | 3 | 4 | 4～5 | 2～3 | 4～5 | 4～5 | |
| The water logging fastness | Former cloth fades | 3～4 | 3～4 | 4～5 | 2 | 3 | 3～4 |
| Calico staining | 3 | 4～5 | 4～5 | 3 | 4～5 | 4～5 | |
| The influence of light of checking colors | Influential | Basic influence | Influential | Substantially there is not influence | |||
COTTON FABRIC behind the vital staining is after aldehyde-free colour stabilizer FIX500 fixation treatment of the present invention as can be seen from the table, and the dyefastness of COTTON FABRIC is improved, and all improves 1～2 grade with comparing without the COTTON FABRIC of fixation treatment.Basically do not influence the coloured light of DYED FABRICS, colour fixation all meets or exceeds color fixing agent Y.
Four, conclusion
Formaldehyde-free color fixing agent is to aim at the dyefastness that improves active dyeing cotton fabric and the color-fixing agent of developing.Experimental results show that: the fixing property of formaldehyde-free color fixing agent of the present invention and colour fixation all meet or exceed color fixing agent Y.Formaldehyde-free color fixing agent of the present invention can replace color fixing agent Y to be applied to the fixation treatment of Dyeing of Cotton Fabric with Reactive Dyes fabric fully.
Claims (2)
1. the manufacturing technique of a formaldehyde-free color fixing agent, this color-fixing agent is formulated by diethylenetriamine and epoxychloropropane, it is characterized in that, and its preparing process step is as follows:
A) get certain water gaging and diethylenetriamine and add in the reactor, stir;
B) drip epoxychloropropane, the control temperature is below 50 ℃;
C) heat to 55～65 ℃, and be incubated 0.5～2 hour; Heat to 75～90 ℃ insulation reaction 20～40 minutes again;
D) sampling and testing product viscosity is cooled to room temperature after qualified, and discharging gets product.
2. the manufacturing technique of formaldehyde-free color fixing agent according to claim 1 is characterized in that, at c) first heat temperature raising to 60 ℃ in the step, insulation reaction one hour, heat temperature raising to 80 ℃ again, insulation reaction 30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB031140017A CN100350097C (en) | 2003-03-27 | 2003-03-27 | Manufacturing technology of formaldehydeless colour fixing agent |
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|---|---|---|---|
| CNB031140017A CN100350097C (en) | 2003-03-27 | 2003-03-27 | Manufacturing technology of formaldehydeless colour fixing agent |
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| CN100350097C true CN100350097C (en) | 2007-11-21 |
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Cited By (1)
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| CN101560380B (en) * | 2008-12-12 | 2012-06-27 | 中国石油化工股份有限公司胜利油田分公司采油工艺研究院 | Preparation method of depolymerized and dispersed viscosity reducer of heavy oil |
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| CN101492888B (en) * | 2008-01-22 | 2012-12-26 | 上海德桑精细化工有限公司 | Alkali-fast aldehyde-free color stabilizer and method for preparing the same |
| CN101871173B (en) * | 2010-06-30 | 2013-07-10 | 苏州大学 | Formaldehyde-free color-fixing agent of active dye |
| CN102493232A (en) * | 2010-06-30 | 2012-06-13 | 苏州大学 | Formaldehyde-free fixing agent for active dye |
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| CN105421118A (en) * | 2016-01-08 | 2016-03-23 | 湖州市千金丝织厂 | Novel environment-friendly formaldehyde-free dye-fixing agent and preparation method thereof |
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| CN109295776A (en) * | 2018-08-29 | 2019-02-01 | 广州邦葳纺织助剂有限公司 | A kind of color fixing agent and preparation method thereof |
| CN109678220A (en) * | 2019-01-10 | 2019-04-26 | 深圳市浩天源环保科技有限公司 | A kind of decolorising agent and its preparation method and application |
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| DE3525104A1 (en) * | 1984-07-21 | 1986-01-30 | Sandoz-Patent-GmbH, 7850 Lörrach | Polycondensates, their preparation and their use |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101560380B (en) * | 2008-12-12 | 2012-06-27 | 中国石油化工股份有限公司胜利油田分公司采油工艺研究院 | Preparation method of depolymerized and dispersed viscosity reducer of heavy oil |
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