Short process printing technique for polyester-cotton blended fabric

Abstract

The application discloses a short-process printing process of polyester-cotton blended fabric, which comprises screen printing by using active disperse dyes containing double active groups and steaming by using alcohol vapor; the double active groups include hydroxyethyl sulfone sulfate group and CH2CH(OH)CH2X (X is Br or Cl); the CH2CH(OH)CH2X can be converted into an epoxy group under alkaline conditions and can react with the alcohol vapor during the steaming process to realize the cross-linking between dye molecules, so that the effects of improving the fixation efficiency and shortening the process flow are achieved, and then the printed fabric with high color depth and high color fastness is obtained.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of printing and dyeing technology, in particular to a short process printing technology for polyester-cotton blended fabric. BACKGROUND

[0002] Due to the difference in physical and chemical properties of polyester and cotton fibers, the dyeing and printing performance of polyester-cotton blended fabric is different, and it is important to choose a suitable printing method. At present, the printing methods of polyester-cotton blended fabric are divided into two categories: pigment printing and dye printing. Pigment printing is to adhere pigments to the surface of the fabric through adhesives, resulting in poor hand feeling. The prior art generally uses disperse / reactive dye printing and disperse / reduction dye printing to dye polyester-cotton blended fabric, but the post-processing of the two methods is complicated, the water consumption is large, the sewage treatment pressure is large, and further improvement is needed.

[0003] One of the ways to solve the problem is to use reactive disperse dyes for printing. Reactive disperse dyes refer to disperse dyes with active groups that can form chemical bonds with fibers. Such dye molecules contain a temporarily soluble anionic water-soluble group, which allows them to be water-soluble and dispersed and to be dyed on cotton fibers. Then it can be converted to a non-ionic under certain conditions, and then it can be dyed on polyester like disperse dyes. Using reactive disperse dyes for polyester-cotton printing can shorten the process flow, but there are still problems such as insufficient dyeing rate on polyester, poor clarity of printed patterns, and cotton staining.

[0004] In view of this, the present application is proposed. SUMMARY

[0005] The present application provides a short process printing technology for polyester-cotton blended fabric, which aims to reduce the printing process and time of polyester-cotton blended fabric, improve the clarity, apparent color depth and color fastness of printing, and improve the problem of cotton staining.

[0006] The present application is implemented as follows:

[0007] A short process printing technology for polyester-cotton blended fabric, comprising the following steps:

[0008] (1) preparing printing color paste; the printing color paste comprises the following components in mass percentage: 1-5% reactive disperse dye, 1-5% alkali agent, 0.8-1.2% resist salt S, 3-7% urea, 60% 75% paste, and the balance is water;

[0009] The reactive disperse dye has the following formula I molecular structure:

[0010]

[0011] In the formula, R1 and R2 are independently selected from H or Br; Ar is R3 is H or CH3; R4 is H or NHCOCH3; R5 is CH2CH(OH)CH2Cl or CH2CH(OH)CH2Br; R6 is alkyl with carbon number of 1-4, C a H 2a CN, C b H 2b X, CH2CH(OH)CH2Cl or CH2CH(OH)CH2Br, a, b are independently any integer from 1 to 4, X is Br or Cl;

[0012] (2) printing by screen printing;

[0013] (3) baking;

[0014] (4) steaming with alcohol vapor;

[0015] (5) washing;

[0016] (6) drying.

[0017] The present application adopts active disperse dye to print polyester-cotton blended fabric, and adopts screen printing to combine paste and printing into one step, thus simplifying the process flow. Further, the present application adopts alcohol vapor to improve the fixation efficiency of the active disperse dye, thus simplifying the washing step, greatly simplifying the process flow, reducing water consumption and wastewater discharge. Specifically, the active disperse dye designed and developed by the present application has double active groups, including hydroxyethyl sulfone sulfate group and CH2CH(OH)CH2X (X is Br or Cl). The hydroxyethyl sulfone sulfate group can be decomposed into ethyl sulfone under alkaline conditions, and can be chemically bonded with the hydroxyl group on the cotton fiber, thus being fixed on the cotton fiber. The water solubility of the decomposed molecule is reduced, thus increasing the affinity to polyester fiber and facilitating diffusion into the interior of the polyester fiber. CH2CH(OH)CH2X can be removed as HX and converted into epoxy group under alkaline conditions. The epoxy group can be crosslinked with alcohol hydroxyl group during steaming with alcohol vapor, thus increasing the adhesion of the dye on the surface of the textile through crosslinking. Therefore, the active disperse dye provided by the present application is used in combination with alcohol vapor for steaming, which can shorten the printing process flow, improve the dyeing of the dye, thus improving the printing efficiency, and improving the color depth and color fastness of the printing.

[0018] In some embodiments, the paste comprises sodium alginate.

[0019] In some embodiments, the paste comprises sodium alginate and gamma-polyglutamic acid.

[0020] Preferably, in the paste, the mass ratio of sodium alginate and gamma-polyglutamic acid is (80:20) to (95:5).

[0021] Gamma-polyglutamic acid has good water-locking ability, and appropriate addition can reduce the bleeding phenomenon of printing paste and improve the clarity of printing; and the thixotropy of gamma-polyglutamic acid is relatively good, which can effectively improve the flow stability of the paste, so as to smoothly pass through the screen and transfer to the fabric; however, gamma-polyglutamic acid should not be too much or too little, too much can easily lead to too low viscosity of the printing paste, and aggravate bleeding; too little can hardly play its modification role.

[0022] In some embodiments, the percentage content of water in the paste is 88% to 95%.

[0023] In some embodiments, the viscosity of the paste at 25°C under normal pressure is 31000 to 33000 cps.

[0024] In some embodiments, the alcohol in the alcohol-containing steam is at least one selected from the group consisting of methanol, ethanol and propanol.

[0025] In some embodiments, the alcohol-containing steam further contains triethylamine.

[0026] Further introducing triethylamine in the steam in steaming can improve the reactivity of alcohol and epoxy group, improve the fixation effect, and thus improve the color depth and color fastness of printing.

[0027] In some embodiments, the flow rate of alcohol in the alcohol-containing steam is 1 to 2 t / h.

[0028] In some embodiments, the flow rate of triethylamine in the alcohol-containing steam is 0.2 to 0.5 t / h.

[0029] In some embodiments, the alkali agent is at least one selected from the group consisting of sodium bicarbonate, sodium carbonate, sodium hydroxide and potassium hydroxide.

[0030] In some embodiments, the screen printing method includes rotary screen printing or flat screen printing.

[0031] In some embodiments, the baking temperature is 150 to 250°C, and the baking time is 8 to 15 min.

[0032] In some embodiments, the steaming temperature is 90 to 110°C, and the steaming time is 5 to 15 min.

[0033] In some embodiments, the washing temperature is 60°C, and the bath ratio is 1: (20 to 30).

[0034] In some embodiments, the preparation method of the reactive disperse dye comprises the following steps:

[0035] S1, preparation of diazonium component: the para-ester or its derivative is diazotized under the action of hydrochloric acid and sodium nitrite to obtain the diazonium component;

[0036] S2, preparation of coupling component: the aniline or its derivative is stirred with halogenated epoxide propane under the action of catalyst to obtain the coupling component after first purification;

[0037] S3, preparation of reactive disperse dye: the coupling component is dissolved in acid solution, then the diazonium component is added to perform coupling reaction, and the reactive disperse dye is obtained after second purification.

[0038] In some embodiments, the para-ester or its derivative in step S1 comprises para-ester or bromo-para-ester.

[0039] In some embodiments, the molar ratio of the para-ester or its derivative, sodium nitrite and hydrogen chloride in hydrochloric acid is 1:1.05-1.3:2-4.

[0040] In some embodiments, the temperature of the diazotization reaction is 0-5°C, and the time is 1-2h.

[0041] In some embodiments, the aniline or its derivative in step S2 comprises at least one of aniline, N-alkylaniline, N-phenylcyanamide, anilinoacetonitrile, 3-(phenylamino)propionitrile, 4-(phenylamino)butyronitrile, chloromethylaniline, N-(3-chloropropyl)aniline, o-toluidine, m-aminoacetanilide, N-(3-amino-4-methylphenyl)acetamide, N-methyl-o-toluidine, N-ethyl-2-methylaniline, N-[3-(methylamino)phenyl]acetamide, 3-N-ethylaminoacetanilide, N1-[3-(ethylamino)-4-methylphenyl]acetamide, N-{3-[(cyanomethyl)amino]phenyl}acetamide, N-(o-tolyl)cyanamide, N-methyl-1-naphthylamine and N1-[3-(ethylamino)-4-methylphenyl]acetamide.

[0042] In some embodiments, the halogenated epoxide propane is epichlorohydrin or epibromohydrin.

[0043] In some embodiments, the molar ratio of the aniline or its derivative to the halogenated epoxide propane is 1:5-15.

[0044] In some embodiments, the catalyst is an organic ammonium salt, preferably tetrabutylammonium bromide or benzyltriethylammonium chloride.

[0045] In some embodiments, the catalyst is added in an amount of 2% of the mass of the aniline or its derivative.

[0046] In some embodiments, the temperature of the stirring reaction is 30-50 DEG C, and the time of the stirring reaction is 24-36 hours.

[0047] In some embodiments, the first purification refers to distillation under reduced pressure at 120 DEG C.

[0048] In some embodiments, the acid solution in step S3 is a 10-30% aqueous solution of hydrogen chloride or acetic acid.

[0049] In some embodiments, the molar ratio of the diazonium component to the coupling component is 1:1.

[0050] In some embodiments, the second purification comprises filtering the reaction solution at 5-10 DEG C, then rinsing the filter cake with saturated sodium chloride aqueous solution and water at 0-5 DEG C in sequence, and finally drying.

[0051] The present application has the following advantages:

[0052] The present application provides a short process printing technology for polyester-cotton blended fabric, which realizes printing of polyester-cotton with the same paste by using reactive disperse dyes, and improves the fixation degree of dyes on polyester by using a specific steaming process, so as to shorten the washing and fixation process, reduce the staining of cotton, and improve the color depth and color fastness of the fabric. Further, the paste used in the present application contains γ-polyglutamic acid, which has excellent water retention and thixotropy, so as to improve the water absorption of the fabric and the flow stability of the paste, thereby reducing the pattern edge burrs caused by infiltration, and improving the clarity of printing. BRIEF DESCRIPTION OF DRAWINGS

[0053] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed in the embodiments will be briefly introduced as follows, and it should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as a limitation on the scope, and for those skilled in the art, other related drawings can also be obtained without creative labor on the basis of these drawings.

[0054] Figure 1 The infrared spectrum of dye 1 and dye 2 prepared for example 1 and example 3;

[0055] Figure 2 The infrared spectrum of dye 3 and dye 4 prepared for example 4 and example 5. DETAILED DESCRIPTION

[0056] In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. If specific conditions are not specified in the embodiments, conventional conditions or manufacturer recommended conditions are adopted. If the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased in the market.

[0057] In the description of the embodiments of the present application, the technical terms "first", "second" and the like are only used to distinguish different objects, and cannot be understood as indicating or implying relative importance or implicitly indicating the number, specific order or primary and secondary relationship of the indicated technical features.

[0058] Reference to "embodiments" herein means that the specific features, structures or properties described in connection with the embodiments can be included in at least one embodiment of the present application. The appearance of this phrase at various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment to other embodiments.

[0059] In the embodiments of the present application, the term "or / and" is only a description of the association relationship of the associated objects, which means that there can be three relationships, for example, A or / and B, which can represent the three cases of A alone, A and B together, and B alone.

[0060] In addition, the character " / " herein generally represents an "or" relationship between the associated objects before and after it.

[0061] In the embodiments of the present application, the meaning of "multiple" is two or more (including two), and similarly, "multiple groups" means two or more groups (including two groups), and "multiple layers" means two or more layers (including two layers), unless otherwise specified and limited.

[0062] In the embodiments of the present application, the meaning of "at least one" is one or more than one.

[0063] The specific meanings of the above terms in the embodiments of the present application can be understood by those skilled in the art according to specific circumstances.

[0064] The features and properties of the present application will be further described below in combination with embodiments.

[0065] Embodiment 1

[0066] A short process printing process for polyester-cotton blended fabric, comprising the following steps:

[0067] (1) Preparation of printing paste

[0068] The printing paste formula, calculated by mass percentage, comprises the following components: 3% active disperse dye (dye 1), 2.8% sodium bicarbonate, 1% resist salt S, 5% urea, 70% sodium alginate paste, and the balance is water.

[0069] The sodium alginate paste has a sodium alginate mass percentage content of 8%, and is prepared as follows: sodium alginate powder is added to water, homogenized for 2 hours, then swelled by standing, and finally water is added to constant volume and stirred until uniform, and the viscosity at 25°C is 32000±1000cps.

[0070] The active disperse dye has the following molecular structure, denoted as Dye 1:

[0071]

[0072] The maximum absorption wavelength of the dye is tested using a Hitachi U-3310 UV spectrophotometer, and the melting point of the dye is measured using an MP90 melting point apparatus. The maximum absorption wavelength of Dye 1 is 461 nm, and the dye is yellow, with a melting point of 136°C.

[0073] (2) Perform rotary screen printing, and the printed pattern includes lines and blocks. A Japanese Toyo Shien magnetic bar rotary screen printing machine is used, with a rotary screen mesh of 105 meshes, a 15 magnetic bar is used, and the speed is 20 m / min. The specification of the polyester-cotton blended fabric is 21s x 21s, 108 x 58;

[0074] (3) Baking: baking at 150°C for 10 min;

[0075] (4) Alcohol steaming: temperature is 100°C, and time is 8 min. The steam composition includes ethanol and triethylamine, the flow rate of ethanol is 1.5 t / h, and the flow rate of triethylamine is 0.4 t / h;

[0076] (5) Water washing: water temperature is 60°C, and the bath ratio is 1:20.

[0077] (6) Drying.

[0078] The preparation method of the active disperse dye includes the following steps:

[0079] (1) Preparation of the diazonium component: disperse the para-ester in water, cool to 0-5°C, then add concentrated hydrochloric acid, and stir for 20 min. Add 30 wt% sodium nitrite aqueous solution dropwise, and complete the dropwise addition in 30 min. Then stir for 1 h to perform the diazotization reaction, and finally add sulfamic acid and stir for 20 min to eliminate excess nitrous acid, to obtain the diazonium component. The molar ratio of the para-ester, sodium nitrite, and hydrogen chloride in the hydrochloric acid is 1:1.1:3;

[0080] (2) Preparation of the coupling component: N-butyl aniline, epichlorohydrin, and catalyst tetrabutylammonium bromide were mixed, stirred until completely clear, stirred at 40°C for 36 h, then distilled under reduced pressure at 120°C to obtain a viscous coupling component; wherein the molar ratio of N-butyl aniline to epichlorohydrin was 1:10; the amount of tetrabutylammonium bromide added was 2% of the mass of N-butyl aniline;

[0081] (3) Preparation of the reactive disperse dye: the coupling component was dissolved in a 10 wt% hydrochloric acid solution, cooled to 0-5°C, and the diazonium component was added dropwise, which was completed in 30 min, then sodium bicarbonate was added to adjust the pH to 3, and the coupling reaction was carried out at 20°C for 3 h, the reaction end point was tested with 0.5% H acid solution, the reaction liquid was cooled to 5-10°C, and the filter cake was washed with 0-5°C saturated sodium chloride aqueous solution and water in turn, and dried at 60°C to obtain the reactive disperse dye (dye 1); wherein the mass ratio of the coupling component to the 10 wt% hydrochloric acid solution was 1:1; the molar ratio of the molar amount of the coupling component to the molar amount of the diazonium component was 1:1.

[0082] Through the above preparation method, the yield of dye 1 (calculated as p-ester) was 95.4%.

[0083] The infrared spectrum of dye 1 (tested by KBr pressing method) is shown in the following figure: Figure 1 The absorption peaks near 1600 cm -1 , 1500 cm -1 , and 1450 cm -1 are the skeletal vibration peaks of benzene rings, the absorption peak near 830 cm -1 corresponds to the bending vibration peak of C-H of disubstituted aromatic rings, the two absorption peaks at 2850-2950 cm -1 correspond to the symmetric and antisymmetric stretching vibration peaks of alkyl C-H; the strong absorption peak at 3600-3200 cm -1 corresponds to the stretching vibration peak of hydroxyl group; the absorption peaks at 1350-1260 cm -1 correspond to the in-plane bending vibration peak of secondary alcohol OH, the absorption peak near 1100 cm -1 is the C-O stretching vibration peak of secondary alcohol; the two absorption peaks near 1330 cm -1 and 1140 cm -1 correspond to the symmetric and antisymmetric stretching vibration absorption peaks of -SO2-.

[0084] Example 2

[0085] The difference from Example 1 is that the composite paste is used instead of the sodium alginate paste, and the mass percentage content of γ-polyglutamic acid in the composite paste is 0.8%, and the mass percentage content of sodium alginate is 7.2%, and the preparation method is as follows: sodium alginate powder and γ-polyglutamic acid powder are added to water, homogenized for 2h, then swelled by standing, and finally water is added to constant volume and stirred until uniform, and the viscosity at 25°C is 32000±1000cps.

[0086] Example 3

[0087] The difference from Example 2 is that dye 2 is used instead of dye 1 as the active disperse dye to prepare the printing paste, and the molecular structure of dye 2 is as follows:

[0088]

[0089] The maximum absorption wavelength of dye 2 is 458nm, which is yellow, and the melting point is 132°C.

[0090] The preparation method of dye 2 includes the following steps:

[0091] (1) The same as Example 1;

[0092] (2) Preparation of coupling component: aniline, epichlorohydrin, and catalyst tetrabutylammonium bromide are mixed and stirred until completely clear, and then stirred at 40°C for 36h, and then distilled at 120°C under reduced pressure to obtain a viscous coupling component; wherein the molar ratio of aniline to epichlorohydrin is 1:15; the addition amount of tetrabutylammonium bromide is 2% of the mass of aniline;

[0093] (3) The same as Example 1.

[0094] Through the above preparation method, the yield of dye 2 (calculated as p-ester) is 96.6%.

[0095] The infrared spectrum of dye 2 (tested by KBr pressing method) is shown in the accompanying Figure 1 , compared with dye 1, the absorption peak intensity at 3600-3200cm -1 increases greatly, indicating that the alcohol hydroxyl content increases.

[0096] Example 4

[0097] A short process printing process for polyester-cotton blended fabric, including the following steps:

[0098] (1) Preparation of printing paste

[0099] The printing paste formula, calculated by mass percentage, includes the following components: 1% active disperse dye (dye 3), 1.2% sodium bicarbonate, 0.8% resist salt S, 3% urea, 75% composite paste, and the balance is water.

[0100] The mass percentage of the γ-polyglutamic acid in the composite paste is 0.8%, and the mass percentage of the sodium alginate is 7.2%. The preparation method is as follows: the sodium alginate powder and the γ-polyglutamic acid powder are added into water, homogenized for 2 hours, then swelled by standing, finally, water is added to constant volume and stirred until uniform, and the viscosity at 25℃ is 32000±1000cps.

[0101] The active disperse dye has the following molecular structure, which is denoted as dye 3.

[0102]

[0103] The dye 3 has a maximum absorption wavelength of 548nm, is red, and has a melting point of 181℃.

[0104] (2) rotary screen printing is performed, same as in Example 1;

[0105] (3) baking: baking at 210℃ for 8min;

[0106] (4) alcohol steaming: the temperature is 90℃, and the time is 5min; the steam composition includes ethanol and triethylamine, the flow rate of the ethanol is 1t / h, and the flow rate of the triethylamine is 0.2t / h;

[0107] (5) water washing: same as in Example 1.

[0108] (6) drying.

[0109] The preparation method of the active disperse dye includes the following steps:

[0110] (1) preparation of the diazonium component: bromo-p-ester is dispersed in water, cooled to 0-5℃, then concentrated hydrochloric acid is added, and stirred for 20min, then 30wt% sodium nitrite aqueous solution is added dropwise, and the dropwise addition is completed in 30min, then the solution is stirred for 1h for diazotization reaction, finally, sulfamic acid is added and stirred for 20min to eliminate excess nitrous acid, to obtain the diazonium component; wherein the molar ratio of bromo-p-ester, sodium nitrite and hydrogen chloride in hydrochloric acid is 1:1.1:3;

[0111] (2) preparation of the coupling component: N1-[3-(ethylamino)-4-methylphenyl]acetamide, epichlorohydrin and catalyst tetrabutylammonium bromide are mixed, stirred until completely clear, stirred at 50℃ for 36h, then distilled at 120℃ under reduced pressure, to obtain the viscous coupling component; wherein the molar ratio of N1-[3-(ethylamino)-4-methylphenyl]acetamide and epichlorohydrin is 1:15; the addition amount of tetrabutylammonium bromide is 2% of the mass of N1-[3-(ethylamino)-4-methylphenyl]acetamide;

[0112] (3) Preparation of the reactive disperse dye: the coupling component is dissolved in 30 wt% acetic acid aqueous solution, cooled to 0-5℃, and the diazonium component is added dropwise, which is completed in 30 min, then sodium bicarbonate is added to adjust the pH to 4, and the coupling reaction is carried out at 20℃ for 3 h, the reaction end point is tested with 0.5% H acid solution, the reaction solution is cooled to 5-10℃, and then filtered while cold, and the filter cake is washed with 0-5℃ saturated sodium chloride aqueous solution and water in sequence, and dried at 60℃ to obtain the reactive disperse dye (dye 3); wherein the mass ratio of the coupling component to 30 wt% acetic acid aqueous solution is 1:1; the molar ratio of the coupling component to the diazonium component is 1:1.

[0113] By the above preparation method, the yield of dye 3 (calculated as bromo-p-substituted ester) is 93.8%. The infrared spectrum of dye 3 is shown in Figure 2. Figure 2

[0114] Example 5

[0115] A short process printing process for polyester-cotton blended fabric, comprising the following steps:

[0116] (1) Preparation of printing paste

[0117] The printing paste formula, calculated by mass percentage, comprises the following components: 5% reactive disperse dye (dye 3), 4.3% sodium bicarbonate, 1.2% resist salt S, 7% urea, 60% composite paste, and the balance is water.

[0118] Among them, the mass percentage content of γ-polyglutamic acid in the composite paste is 0.8%, and the mass percentage content of sodium alginate is 7.2%, and the preparation method is as follows: sodium alginate powder and γ-polyglutamic acid powder are added to water, homogenized for 2 h, then swelled by standing, and finally water is added to constant volume and stirred until uniform, and the viscosity at 25℃ is 32000±1000 cps.

[0119] The reactive disperse dye has the following molecular structure, which is referred to as dye 4:

[0120]

[0121] The maximum absorption wavelength of dye 3 is 495 nm, which is orange, and the melting point is 154℃.

[0122] (2) Perform flat screen printing, using Japan's East Shen flat screen printing machine;

[0123] (3) Baking: baking at 170℃ for 15 min;

[0124] (4) Alcohol steaming: temperature is 110℃, time is 15 min; the composition of the steam includes ethanol and triethylamine, the flow rate of ethanol is 2 t / h, and the flow rate of triethylamine is 0.5 t / h;​

[0125] (5) Water washing: same as Example 1.

[0126] (6) Drying.

[0127] The preparation method of the reactive disperse dye (Dye 4) comprises the following steps:

[0128] (1) Preparation of diazonium component: same as Example 4;

[0129] (2) Preparation of coupling component: N-{3-[(cyanomethyl)amino]phenyl}acetamide, epichlorohydrin, and catalyst tetrabutylammonium bromide are mixed, stirred until completely clear, stirred at 50°C for 36h, then distilled under reduced pressure at 120°C to obtain the coupling component in a viscous state; wherein the molar ratio of N-{3-[(cyanomethyl)amino]phenyl}acetamide to epichlorohydrin is 1:15; the addition amount of tetrabutylammonium bromide is 2% of the mass of N-{3-[(cyanomethyl)amino]phenyl}acetamide;

[0130] (3) Preparation of reactive disperse dye: same as Example 4.

[0131] Through the above preparation method, the yield of Dye 4 (calculated based on bromo para-ester) is 95.6%. The infrared spectrum of Dye 4 is shown in FIG. 2. Figure 2

[0132] Example 5

[0133] The difference from Example 2 is that Dye 5 is used instead of Dye 1 as the reactive disperse dye, and the baking temperature is 170°C and the time is 15min; wherein the molecular structural formula of Dye 5 is as follows:

[0134]

[0135] The light absorption wavelength of Dye 5 is 512nm, which is orange red, and the melting point is 162°C.

[0136] The preparation method of Dye 5 comprises the following steps:

[0137] (1) Same as Example 1;

[0138] (2) Preparation of coupling component: N-methyl-1-naphthylamine, epichlorohydrin, and catalyst benzyltriethylammonium chloride are mixed, stirred until completely clear, stirred at 40°C for 36h, then distilled under reduced pressure at 120°C to obtain the coupling component in a viscous state; wherein the molar ratio of N-methyl-1-naphthylamine to epichlorohydrin is 1:5; the addition amount of benzyltriethylammonium chloride is 2% of the mass of N-methyl-1-naphthylamine;

[0139] (3) Same as Example 1. ​

[0140] The yield of dye 5 (calculated as p-ester) is 95.7% by the above preparation method.

[0141] Example 7

[0142] The difference from Example 2 is that the mass percentage content of γ-polyglutamic acid in the composite paste is 0.4%, and the mass percentage content of sodium alginate is 7.6%. The preparation method is as follows: the sodium alginate powder and the γ-polyglutamic acid powder are added into water, homogenized for 2h, then left to swell, and finally water is added to constant volume and stirred until uniform, and the viscosity at 25℃ is 32000±1000cps.

[0143] Example 8

[0144] The difference from Example 2 is that the mass percentage content of γ-polyglutamic acid in the composite paste is 1.6%, and the mass percentage content of sodium alginate is 6.4%. The preparation method is as follows: the sodium alginate powder and the γ-polyglutamic acid powder are added into water, homogenized for 2h, then left to swell, and finally water is added to constant volume and stirred until uniform, and the viscosity at 25℃ is 32000±1000cps.

[0145] Example 9

[0146] The difference from Example 2 is that no triethylamine is introduced during alcohol distillation.

[0147] Comparative Example 1

[0148] The difference from Example 3 is that dye 6 is used instead of dye 1 as the dye, and the molecular structure of dye 6 is as follows:

[0149]

[0150] The maximum absorption wavelength of dye 6 is 118nm, which is yellow, and the melting point is 117℃.

[0151] The preparation method of dye 6 comprises the following steps:

[0152] (1) Preparation of diazonium component: aniline is dispersed in water, cooled to 0-5℃, then concentrated hydrochloric acid is added, and stirred for 20min, then 30wt% sodium nitrite aqueous solution is added dropwise, and the dropwise addition is completed in 30min, then the solution is stirred for 1h for diazotization reaction, and finally sulfamic acid is added and stirred for 20min to eliminate excess nitrous acid, to obtain the diazonium component; wherein the molar ratio of aniline, sodium nitrite and hydrogen chloride in hydrochloric acid is 1:1.1:3;

[0153] (2) The same as Example 3;

[0154] (3) The same as Example 3.

[0155] The yield of dye 6 (calculated as aniline) was 98.3% by the above preparation method.

[0156] Comparative Example 2

[0157] The differences from Example 3 are as follows:

[0158] (1) The printing paste formula comprises the following components by mass percentage: 3% active disperse dye (dye 2 of Example 3), 2.8% sodium bicarbonate, 1% resist salt S, 5% urea, 2% ethylene glycol, 68% composite paste (same as Example 3), and the balance is water.

[0159] (2) Instead of alcohol steaming, the printing fabric is steamed by conventional steaming, and the specific steaming steps are as follows: the temperature is 102°C, the time is 10 min, and the steam flow is 1.5 t / h.

[0160] Comparative Example 3

[0161] The differences from Example 3 are as follows:

[0162] (1) The printing paste formula comprises the following components by mass percentage: 3% active disperse dye (dye 6 of Comparative Example 1), 2.8% sodium bicarbonate, 1% resist salt S, 5% urea, 2% ethylene glycol, 68% composite paste (same as Example 3), and the balance is water.

[0163] (2) Instead of alcohol steaming, the printing fabric is steamed by conventional steaming, and the specific steaming steps are as follows: the temperature is 102°C, the time is 10 min, and the steam flow is 1.5 t / h.

[0164] Test Example 1: Paste removal rate

[0165] The mass of the polyester-cotton blended fabric before printing, after printing (including printing and drying), and after post-treatment (including baking, steaming, washing, and drying) is tested, corresponding to m1, m2, and m3, respectively. Each test must be conducted after the corresponding process is completed and the fabric is left to stand for 24 h under standard temperature and humidity. The paste removal rate is calculated as (m2-m3) / (m2-m1) x 100%, and the results are shown in Table 1.

[0166] Test Example 2: Printing clarity

[0167] Two groups of straight lines were printed on the polyester-cotton blended fabric, each group consisting of three parallel straight lines, one group being thin lines with length x width = 10 cm x 100 pm, and the other group being thick lines with length x width = 10 cm x 1000 pm. The fineness of the lines was tested under a microscope, with one point on each 1 cm interval of each straight line being tested for line width, and a total of 30 points for each group of lines, and finally the average width and coefficient of variation (coefficient of variation = sample standard deviation ÷ average) of each group of lines were calculated, with the results shown in Table 1.

[0168] Table 1

[0169]

[0170] The paste removal rate refers to the ease of removal of the paste from the fabric during the post-printing process. The paste removal rate directly affects the printing effect and the hand feeling of the fabric. If the paste removal rate is too low, the paste is difficult to remove from the fabric, which can result in unclear printing, and even affect the air permeability and comfort of the fabric. Therefore, it is crucial to control the paste removal rate. In the present application, the average width and coefficient of variation of the lines are used to evaluate the clarity of the printed pattern. The greater the deviation of the average width from 100 pm and / or 1000 pm, the greater the degree of colorant penetration. The greater the coefficient of variation, the greater the degree of numerical dispersion, i.e. the worse the clarity of the pattern outline. In Example 1 and Example 2 of the present application, sodium alginate paste and composite paste containing γ-polyglutamic acid are used respectively, and there is a significant difference in paste removal rate and printing clarity between the two. Since γ-polyglutamic acid is added to the paste in Example 2, it has a higher paste removal rate and printing clarity. The reason is that γ-polyglutamic acid has a higher water retention capacity, reducing the penetration of the colorant. In addition, the addition of γ-polyglutamic acid can effectively improve the thixotropy of the paste, so that it has better thixotropy under the action of shear force, thereby transferring to the fabric through the screen. The composite paste in Examples 2, 7 and 8 contains different proportions of γ-polyglutamic acid. From the results, it can be seen that as the content of γ-polyglutamic acid increases, the paste removal rate is higher, but the printing clarity first increases and then decreases. The reason is that γ-polyglutamic acid has stronger hydrophilicity, making it easier to remove. Although the water absorption rate of γ-polyglutamic acid is higher than that of sodium alginate, it does not have a sugar ring rigid structure, so its viscosity is lower than that of sodium alginate. Therefore, if the content is too high, it will cause the viscosity of the colorant to decrease too much, which will even exacerbate the penetration. The dye 2 used in Example 3 can produce two epoxy groups under the action of alkali and heat, causing excessive crosslinking during baking and alcohol steaming, and even bonding with the paste, resulting in a decrease in paste removal rate.

[0171] Test Example 3 Apparent Color Depth

[0172] The apparent color depth K / S value of the printed fabric was tested using a Datacolor 650 tester.

[0173] Test Example 4 Color Fastness

[0174] The soaping fastness of the dyed fabric was tested according to GB / T 3921-2008 Textiles- Colour fastness to soaping; the rubbing fastness of the dyed fabric was tested according to GB / T 3920-2008 Textiles- Colour fastness to rubbing; the fastness to sunlight of the dye was tested according to GB / T 8427-2008 Textiles- Colour fastness to artificial light: xenon arc.

[0175] Table 2

[0176]

[0177]

[0178] From the results in the table, it can be seen that the printing obtained by the method provided in the application has good color depth K / S value and color fastness. Comparative Example 1 has lower dyeing rate of the dye due to the absence of hydroxyethyl sulfone sulfate group in the dye, which reduces the reactivity of the dye with cotton fibers, thus the K / S value is lower; but the color fastness is higher because the dye is attached to the surface of the fabric through chemical bonding or cross-linking. Comparative Example 2 does not use alcohol steaming, but adds alcohol substances to the color paste and uses the conventional steaming method, and the K / S value of the printing is lower than that of Example 3, because the alcohol substances are in contact with the color paste in the steaming mode, which improves the contact degree and reactivity of the two, thus facilitating the polymerization reaction. The dye of Comparative Example 3 does not contain hydroxyethyl sulfone sulfate group and does not undergo alcohol steaming, thus the K / S value is the worst.

[0179] Example 2 has greater apparent color depth of the printing due to the addition of polyglutamic acid in the paste of Example 1, because the v-polyglutamic acid improves the thixotropy of the paste and the affinity with the polyester fibers, thus it is better to attach to the surface of the blended fabric through the screen mesh, but the color fastness is not much different because the dyes of the two are the same. Example 3 has more cross-linking groups of the reactive disperse dye than Example 1, but does not significantly improve the color fastness of the printing, but rather makes the K / S value of the printing decrease, and the possible reason is that the alkyl butyl group is used instead of -CH2CHOHCH2Cl, which improves the molar absorption coefficient of the dye. Example 4 uses red dye 3, and although the content of the dye in the color paste is lower, a higher K / S value is still obtained. Example 5 uses orange dye 4, and because the content of the dye in the color paste is higher, the K / S value is also higher. The K / S values of Example 7 and Example 8 are both lower than Example 2 because the content of the γ-polyglutamic acid in the paste of Example 7 is lower and the content of the γ-polyglutamic acid in the paste of Example 8 is higher, because too high γ-polyglutamic acid makes the penetration of the color paste worse, and too low γ-polyglutamic acid makes the permeability of the color paste decrease, both of which are not conducive to the retention of the color paste on the surface of the fabric. Example 9 does not add triethylamine during alcohol steaming, and triethylamine as a catalyst reduces the reactivity of the epoxy group with alcohol, thus the K / S value and the color fastness decrease.

[0180] The preferred embodiments of the present application have been described above with the intent to enable those skilled in the art to make and use it. Various modifications to these embodiments will remain apparent to those skilled in the art, and the generic principles defined herein can be applied to other embodiments. The scope of the application is defined by the appended claims.

Claims

1. A short-process printing process for polyester-cotton blended fabrics, characterized in that, Includes the following steps: (1) Prepare printing paste; The printing paste, by mass percentage, includes the following components: 1%~5% reactive disperse dye, 1%~5% alkali agent, 0.8~1.2% anti-dyeing salt S, 3~7% urea, 60%~75% paste, and the remainder is water; The paste includes sodium alginate and γ-polyglutamic acid; The reactive disperse dye has the following molecular structure: Formula I: , Formula I; In the formula, R1 and R2 are independently selected from H or Br; Ar is... or R3 is H or CH3; R4 is H or NHCOCH3; R5 is CH2CH(OH)CH2Cl or CH2CH(OH)CH2Br; R6 is an alkyl group with 1-4 carbon atoms, C a H 2a CN, C b H 2b X, CH2CH(OH)CH2Cl or CH2CH(OH)CH2Br, where a and b are independent integers from 1 to 4, and X is Br or Cl; (2) Printing is performed using screen printing; (3) Baking; (4) Steaming with alcohol-containing steam; (5) Wash with water; (6) Drying.

2. The short-process printing process for polyester-cotton blended fabrics according to claim 1, characterized in that, In the paste, the mass ratio of sodium alginate to γ-polyglutamic acid is (80:20) to (95:5).

3. The short-process printing process for polyester-cotton blended fabrics according to claim 1, characterized in that, The water content in the paste is 88% to 95%.

4. The short-process printing process for polyester-cotton blended fabrics according to any one of claims 1 to 3, characterized in that, The viscosity of the paste at 25°C and normal pressure is 31,000~33,000 cps.

5. The short-process printing process for polyester-cotton blended fabrics according to claim 1, characterized in that, In step (4), the alcohol in the alcohol-containing vapor is selected from at least one of methanol, ethanol and propanol.

6. The short-process printing process for polyester-cotton blended fabrics according to claim 5, characterized in that, The alcohol vapor in step (4) also contains triethylamine.

7. The short-process printing process for polyester-cotton blended fabrics according to claim 5 or 6, characterized in that, The flow rate of alcohol in the alcohol-containing vapor is 1~2 t / h.

8. The short-process printing process for polyester-cotton blended fabrics according to claim 7, characterized in that, The flow rate of triethylamine in the alcohol-containing vapor is 0.2~0.5 t / h.

9. The short-process printing process for polyester-cotton blended fabrics according to any one of claims 1, characterized in that, The alkaline agent is at least one of sodium bicarbonate, sodium carbonate, sodium hydroxide, and potassium hydroxide; And / or, the screen printing method includes rotary screen printing or flat screen printing; And / or, the baking temperature is 150~250℃, and the baking time is 8~15min; And / or, the temperature of the steam is 90~110℃, and the steaming time is 5~15min; And / or, the water washing temperature is 60°C and the bath ratio is 1:(20~30).

10. The short-process printing process for polyester-cotton blended fabrics according to any one of claims 1, characterized in that, The preparation method of the reactive disperse dye includes the following steps: S1, Preparation of the diazo component: The para-ester or its derivative is subjected to a diazotization reaction in the presence of hydrochloric acid and sodium nitrite to obtain the diazo component; S2, Preparation of the coupling component: Aniline or its derivatives are reacted with halopropylene oxide under a catalyst and stirred. After a first purification, the coupling component is obtained. S3, Preparation of reactive disperse dye: The coupling component is dissolved in an acid solution, and then a diazo component is added to carry out a coupling reaction. After a second purification, the reactive disperse dye is obtained.

11. The short-process printing process for polyester-cotton blended fabrics according to claim 10, characterized in that, The para-ester or its derivative mentioned in step S1 includes para-esters or brominated para-esters; And / or, the molar ratio of the para-ester or its derivative, sodium nitrite, and hydrogen chloride in hydrochloric acid is 1:1.05~1.3:2~4; And / or, the diazotization reaction is carried out at a temperature of 0~5℃ for 1~2h.

12. The short-process printing process for polyester-cotton blended fabrics according to claim 10, characterized in that, The aniline or its derivatives mentioned in step S2 include at least one of aniline, N-alkylaniline, N-phenylcyanamide, aniline acetonitrile, 3-(phenylamino)propionitrile, 4-(phenylamino)butyronitrile, chloromethylaniline, N-(3-chloropropyl)aniline, o-aniline, m-aminoacetaniline, N-(3-amino-4-methylphenyl)acetamide, N-methyl-o-methylaniline, N-ethyl-2-methylaniline, N-[3-(methylamino)phenyl]acetamide, 3-N-ethylaminoacetaniline, N-{3-[(cyanomethyl)amino]phenyl}acetamide, N-(o-tolyl)cyanamide, N-methyl-1-naphthylamine, and N1-[3-(ethylamino)-4-methylphenyl]acetamide; And / or, the halopropylene oxide is epichlorohydrin or epibromopropane; And / or, the molar ratio of aniline or its derivative to halopropylene oxide is 1:5 to 15; And / or, the catalyst is an organic ammonium salt, namely tetrabutylammonium bromide or benzyltriethylammonium chloride; And / or, the amount of catalyst added is 2% of the mass of aniline or its derivative; And / or, the temperature of the stirring reaction is 30~50℃, and the stirring reaction time is 24~36h; And / or, the first purification refers to vacuum distillation at 120°C.

13. The short-process printing process for polyester-cotton blended fabrics according to claim 10, characterized in that, The acid solution mentioned in step S3 is an aqueous solution with a percentage content of 10% to 30% for hydrogen chloride or acetic acid; And / or, the molar ratio of the diazo component to the coupling component is 1:1; And / or, the second purification includes filtering the reaction solution at 5-10°C, then washing the filter cake sequentially with a saturated sodium chloride aqueous solution at 0-5°C and water, and finally drying.

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