专利摘要:
Ecological procedure of emulsion and low temperature dyeing of synthetic fibers and their mixtures. The present invention proposes a new process of dyeing at low temperature (below the boiling point of water), for synthetic fibers, especially polyester, including textured ones, with the use of a microemulsion of dyes that are commonly called " scattered. " its objective is to replace the traditionally called dye transporters, due to pollution problems, their unwanted odor and their toxicity. Instead of the transporter, this procedure is based on the solubilization of the dispersed dye in a microdispersion of an organic solvent in water, such as N-butyl acetate, achieving its stabilization before dyeing and maintaining it during the dyeing process with the aid of a phosphoglyceride stabilizer (soy lecithin). (Machine-translation by Google Translate, not legally binding)
公开号:ES2638738A1
申请号:ES201630513
申请日:2016-04-22
公开日:2017-10-23
发明作者:Francisco Javier CARRIÓN FITÉ
申请人:Universitat Politecnica de Catalunya UPC;
IPC主号:
专利说明:

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c) Dye auxiliary product: It is an emulsion of the O / W type, formed by the organic solvent chosen, n-butyl acetate, among those of physicochemical characteristics indicated above (published in: Low toxicity solvents ”Dr. Leonardo Borgioli from
C.T.C. Spain. Products and Equipment for Restoration, Getafe, Madrid), used in any concentration in an aqueous solution as a continuous phase with the application of a phosphoglyceride, preferably soy lecithin, as an emulsifier from among the families of indicated surfactants. This emulsion requires a diameter of average particle from 100 nm to 600 nm. These submicron particles are necessary to obtain them with the application of the mechanical force necessary to disintegrate the dispersed phase (organic organic solvent) in the continuous phase (water), with the use of any vigorous agitation system for O / W emulsions. One of them is the use of an ultrasonic generator, working at the necessary frequency and giving the power per suitable bath volume, and / or high speed propeller stirrer. This emulsion can be prepared concentrated to be applied by dilution to the dye bath, or in diluted form and applied directly.
The amount of organic solvent required microdispersed in the dye bath is between 0.01% and 30% by volume, and the concentration of emulsifier is between 0.1 to 35 g.L-1
d) Temperature; The temperature can be any within the range formed by the ambient temperature and the boiling point of the chosen solvent.
e) Bathroom relationship. The bath ratio is any of those used in conventional dyes, whether short or long.
f) Electrolytes: The dyeing can be carried out free of electrolytes or in the presence of any type required for conventional dyeing with dispersed dyes or those used for dyeing or natural, animal or synthetic fibers in the case of mixtures of fibers
g) Water for dyeing. The water used can be rectified, distilled or hard, of any hardness between 0 and 60º HF.
h) Presence of other dyes. All types of soluble dyes can be solubilized in the aqueous continuous phase of those used in the dyeing of natural fibers,
or synthetic
i) Dyeing times. The dyeing time is the one necessary to obtain the total or maximum possible depletion of the dye or dyes in the dyeing bath, which will be longer the lower the dyeing temperature, therefore, at room temperature the dyeing times will have more long In general, optimal dyeing times have been approximately twice the time of a conventional dye without conveyor or high temperature.
The use of said microdispersion of the organic solvent in water with the dispersed dye solubilized therein, allows dyeing synthetic fibers, alone or in admixture with other textile materials, in any physical state of presentation of the material, such as flock , wick, yarn or fabric and with any treatment of the fibers such, and as a texturing procedure. This dyeing, as indicated, is carried out at a low temperature or at room temperature, with the consequent energy savings compared to the most expensive conventional methods and without the inconvenience of shrinking items produced in high temperature dyeing methods. .
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a) Dyeing process
Dyes: Dispersed dyes of low molecular weight were used The dyes chosen were the following: a) Rubi Foron E-5R (low molecular weight), b) Foron Blue SE-GLF (medium molecular weight) and c) Blue Foron RD-E ( dye mixture, as indicated by the supplier)
Organic solvent. The pure n-butyl acetate supplied by Panreac with a molecular weight of 116.16 g.mol-1 was used. To dissolve the emulsifier used prior to its application, n-octane was used for synthesis supplied by Merck, with a molecular weight of 114.23 g.mol-1.
Emulsifying product: The amphoteric surfactant used as emulsifier of the solvent and dye was Carlo Erba's pure soy lecithin of 100% purity. It was dissolved in the n-octane solvent, prior to its introduction into the dye bath, at a concentration of 80 g.L-1.
Solvent for textile extraction of the dispersed dye. The 99.8% N-N dimethyl formamide supplied by Panreac, molecular weight 73.10 g.mol-1 was used.
Tincture bath:
The dye bath was prepared in a LINITEST laboratory dyeing apparatus, equipped with hermetically sealed cans of 300 ml capacity
The amount of matter in each boat was 3 grams of polyester fabric.
Dye concentration: 2% dispersed dye
Bathroom ratio: 1/60
Emulsion, used as the dyeing aid. It was prepared with 6% of the amphoteric surfactant, which corresponded to 2.25 ml of the indicated lecithin dissolved at the concentration of 80 gL-1 in n-octane, and was dispersed with 3 ml of n-butyl acetate, in one volume Total 180 ml with hardness free water. This emulsion was helped with mechanical energy by applying agitation with a propeller shaker first and then with ultrasound (2 w / ml, for 1 minute). This emulsion of the auxiliary product was achieved in the presence of 2% s.p.f of the dispersed dye (previously solubilized in the solvent), all with the volume of bath required according to the indicated bath ratio (180 ml, in this case).
The temperatures tested were as follows. 73ºC and 95ºC (they remained constant throughout the dyeing process)
The tinctures were made in Linitest equipment, provided with 300 ml cans with the same ingredients indicated (it was prepared in an initial bath and distributed in equal parts, 180 ml in this case by the various removable tincture cans at different times, with the same ingredients and the same temperature), in order to obtain kinetics at a constant temperature. Consequently, the chosen times ranged from 5 to 240 min, with a shorter time compendium at a higher temperature (95ºC-100ºC) and longer times at temperatures below these temperatures.
Later washing of the tinctures. After the dyes, three rinses were made with rectified water, free of hardness and subsequently washed at 40 ° C for 30 minutes each of the dyes with a non-ionic surfactant Hostapal MRZ.fl from Archroma at the concentration of 0.5 gL- 1 to extract all surface dye from samples not absorbed during dyeing.
The equipment used for washing the stained samples was the Launder-Ometer, with 5 550 ml cans for each sample. Each 3 gram sample was washed in a 150 ml bath of wash solution under the indicated conditions.
Determination of the absorbed dye, after dyeing and subsequent washing. The determination of the dye absorbed by the polyester fabric was made from the
10 desorption by NN, dimethyl formamide (DMF) and making its calculation from the corresponding calibration lines of each dispersed dye (Linearities given by Beer's Law between Absorbance as a function of the concentration of the dye dispersed in DM, at maximum wavelength in the visible spectrum in the spectrophotometer). 15 TABLE 1
Dye kinetics of standard 30A polyester fabric with Rubi Foron E-5R dye at 73ºC and 95ºC (Initial concentration: 20 g dye / K fiber)
Time (min) g dye / K fiber
73 ° C 95º C
5 1,5945,074
10 3,4227,659
30 4,6898,628
fifty -9,289
60 6,551-
70 -10,642
90 7,59613,689
120 8,99513,400
150 10,04413,200
200 11.06-
240 13,600
twenty TABLE 2
25 Dye kinetics of standard 30A polyester fabric with the Blue Foron SE-GLF dye at 73º and 95ºC (Initial concentration: 20 g dye / K fiber)
Time (min) g dye / K fiber 73ºC 95ºC
5 1,4272,921
10 1,4903,313
30 1,9744,600
fifty 2,2355,287
70 2,4135,707
90 2,5105,855
120 2,6007,191
150 3,2007,977
TABLE 3
Dye kinetics of standard 30A polyester fabric with Blue Foron RD-E dye at 73 ° C (Initial concentration: 20 g dye / K fiber)
Time (min) g dye / K fiber 73ºC 95ºC
5 1.291.06
10 1.312.07
30 1.432.73
fifty 1.483.19
70 1.703.36
90 2.003.63
120 2.714.65
150 2.795.23
TABLE 4
Test of solidity of the tinctures to the domestic washing during 30 min, at 40ºC with phosphate-free ECE detergent (Composition ISO 105-C08), according to the norm UNE-EN-ISO 105-C08), applying the norm UNE-EN-ISO 106 -C06. Color fastness test. Part C06: color fastness to domestic and commercial washing (ISO: 105-C06: June 2010)
degradation discharge
 Dif. Color PESCO
Rubin Foron E-5R (tincture 95ºC and 240 minutes) 554-5
Blue Foron RD-E (tincture of 95ºC and 150 minutes) 4-54-55
Blue Foron SE-GLF (tincture of 95ºC and 150 minutes) 4-53-44-5
TABLE 5
Test of solidity of the dyes to the heat treatment. The standard UNE ISO 105-XII of Test of solidity of the dyes to the ironing was applied (ISO 105-X11: 1994). Revision April 1997
Degradation Discharge
110 ° C 150ºC200ºC 110 ° C150ºC200ºC
Rubin Foron E-5R (tincture 95ºC and 240 minutes) 54-54553-4
Blue Foron RD-E (tincture of 95ºC and 150 minutes) 554-5554-5
Blue Foron SE-GLF (tincture of 95ºC and 150 minutes) 54-54554-5
In view of the results of the kinetics of Figures 1-2 and 3 and Tables 1-2 and 3) of dyeing of the indicated dyes, the Rubi Foron E-5R dye (of low molecular weight) showed higher absorption values by the fiber, and the Blue Foron RD-E dye (mixture of
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权利要求:
Claims (1)
[1]
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引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题
ES2011848A6|1988-07-25|1990-02-16|Univ Politecnica De Cataluna I|Process for the low temperature emulsion dyeing of synthetic fibres and their mixtures|CN109505160A|2018-11-02|2019-03-22|长沙浩然医疗科技有限公司|A kind of textile dyeing and printing technique|
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