CN115772811A - Cold pad-batch dyeing process capable of preventing lyocell woven fabric from fibrillation - Google Patents

Abstract

The invention belongs to the field of textile production technology and processing, and in particular relates to a cold pad-batch dyeing process capable of preventing fibrillation of lyocell woven fabrics. The method comprises the following steps: preparing the treatment solution of amylase and penetrant, adjusting the pH of the treatment solution to 4-6, padding and desizing the lyocell woven gray fabric, rolling and stacking, washing with hot water, washing with water at normal temperature, and drying dry; pad the fabric with a solution containing an anti-fibrillation treatment agent, dry, bake, wash, and dry; prepare reactive dye dyeing solution and color fixing solution, and mix the prepared dyeing solution and color fixing solution to prepare Dyeing working solution, pad the fabric with dyeing working solution, roll up and stack, wash with hot water, soap, cold water, and dry. The invention saves the refining and bleaching process, uses the anti-fibrillation treatment agent to perform anti-fibrillation treatment before dyeing, improves the anti-fibrillation ability of the lyocell fabric, and adopts the cold pad-batch dyeing process to process the lyocell woven fabric Dyeing reduces the friction between fabric and equipment and reduces the tendency of fibrillation.

Description

Cold pad-batch dyeing process to prevent fibrillation of lyocell woven fabrics

technical field

The invention belongs to the field of textile production technology and processing, and in particular relates to a cold pad-batch dyeing process capable of preventing fibrillation of lyocell woven fabrics.

Background technique

Lyocell fiber is a regenerated cellulose fiber made from wood pulp and N-methylmorpholine-N-oxide (NMMO) as a solvent through a dry-jet wet spinning process. During the production process, the solvent recovery reaches more than 99.7%, and the waste is biodegradable, so it is recognized as a green fiber. Lyocell fiber fabric has the "comfort" like cotton, the "strength" close to polyester, the "beauty" like wool and the "touch" and "soft drape" effect like silk, and is widely used in the production of advanced textile fabrics . However, lyocell fiber has unique fibrillation characteristics. After rubbing in a wet state, fibrils with a diameter of less than 1 micron will be split in the fiber axis, making the fabric appear light-colored or "frost" or white lines. Printing and dyeing defects such as scratches or scratches. Lyocell woven fabric dyeing usually adopts open-width continuous processing technology. Under the conditions of humidity, alkali and mechanical friction, the lateral swelling of fibers makes the stiff fabric easier to fibrillate, resulting in serious fabric quality problems.

At present, the main methods to solve the fibrillation problem of lyocell woven fabrics include fiber crosslinking treatment, resin finishing and cellulase hair removal. For example, "Research Progress on Anti-fibrillation of Lyocell Fibers" introduced that Lenzing company cross-linked cellulose by using dichlorotriazine cross-linking agents. performance is significantly improved. CN201911296394.9 introduces a preparation method of non-fibrillated Lyocell fibers, using 1,3,5-triacryloylhexahydro-1,3,5-triazine (TAHT) anti-fibrillation additives to Lyocell Lyocell fiber with anti-fibrillation treatment can be worth a lyocell fiber with a relatively low fibrillation tendency. "The effect of crosslinking treatment on the fibrillation properties of Lyocell fibers" using 1,2,3,4-butanetetracarboxylic acid (BTCA) to treat Lyocell fibers can also enhance the force between fiber macromolecular chains , to some extent reduce fibrillation. "Effect of oligomeric maleic acid-citric acid cross-linking treatment on the anti-fibrillation properties of Lyocell fiber" The polycarboxylic acid citric acid (CA) and oligomeric maleic acid were mixed and reacted, and then cross-linked with Lyocell fiber. "Fibrillation Control Methods and Evaluation Criteria for Lyocell Fiber Home Textile Fabrics" introduces the research on the fibrillation of Lyocell fabrics in the finishing of dyed resins. The research shows that choosing the right resin to finish the Lyocell fibers can improve the anti-pilling Pilling rating. "Research on Fibrillation and Anti-fibrillation of Lyocell Fibers" introduces the research of cellulase on the prevention and control of fibrillation of Lyocell fabrics. This method first fibrillates Lyocell fibers under concentrated alkali conditions, and then Cellulase is used to remove the split fibrils on the surface of the fabric, so as to reduce the fibrillation tendency of fibers during production and use.

Although the above methods can prevent the fibrillation of lyocell fibers to a certain extent, it is still difficult to reduce the fibrillation of lyocell woven fabrics in the multi-process continuous processing process. For the fiber cross-linking treatment method, after the fiber is cross-linked, it needs to go through multiple processes such as spinning, weaving, pre-treatment, printing and dyeing, and post-finishing. There is more friction between the fiber and the equipment, and it is still easy to fibrillate. The resin finishing of lyocell woven fabrics is mainly carried out in the post-finishing process, not only it is difficult to reduce the fibrillation of the fabric in the pre-treatment and dyeing process, but most of the resins release formaldehyde. For the cellulase hair removal method, the process is complicated and the cost is high, and the interaction between the fiber macromolecular chains is not enhanced, and fibrillation will still occur during subsequent processing and use.

The invention is based on the processing characteristics of the lyocell woven fabric dyeing process, and under the premise of ensuring that the pretreatment and dyeing performance indicators of the lyocell fabric meet the requirements, the lyocell woven fabric is subjected to anti-fibrillation treatment during the dyeing process , not only can effectively reduce the tendency of fibrillation in the process of fabric production and use, but also has short technological process, low cost, simple and easy operation.

Contents of the invention

Aiming at the technical problem that lyocell woven fabrics are easily fibrillated by friction under wet, hot and alkaline conditions, the invention develops a cold pad-batch dyeing process for lyocell woven fabrics that can prevent fibrillation. First of all, using the synergistic effect of amylase and scouring penetrant to pre-treat the fabric, not only can achieve the required whiteness and wool effect, but also shorten the pre-treatment process and reduce the friction of the fabric; Anti-fibrillation treatment enhances the interaction of fiber macromolecular chains and prevents fabric fibrillation during dyeing and use; develops a low-temperature and low-friction cold pad-batch dyeing process for lyocell woven fabrics, which can not only prevent fibrillation The generation of the product improves the product quality and first-class product rate, and is energy-saving, environmentally friendly, and simple and easy to operate.

The cold pad-batch dyeing process that can prevent Lyocell woven fabric fibrillation of the present invention, comprises the following steps:

(1) prepare the desizing working solution of 2-14g/L amylase and 1-5g/L penetrating agent, adjust the pH of the desizing working solution to be 4-6, and pad the lyocell woven fabric gray cloth after singeing Pulp working fluid, control the liquid rate, roll up and stack at 10-40°C for a certain period of time, wash with hot water, wash with water at room temperature, and dry;

(2) preparation concentration is the anti-fibrillation treatment agent solution of 5-35g/L, the fabric after step (1) is processed is pad-rolled the solution that contains anti-fibrillation treatment agent, controls liquid carrying rate, dries, bakes drying, washing, drying;

(3) Prepare a reactive dye solution with a concentration of 5-60g/L and a color-fixing solution with a concentration of 5-40g/L, mix the prepared dye solution and color-fixing solution evenly in a certain proportion, and prepare the dyeing work liquid, the fabric padding dyeing working liquid after step (2) is processed, controls the liquid carrying rate, coils and stacks at a certain temperature for a period of time, hot water washing, soap washing, cold water washing, and drying.

in:

The penetrant described in step (1) is a non-ionic refined penetrant.

The liquid carrying rate described in step (1) is 60-90%, and the stacking time is 1-12 hours.

The liquid-carrying rate in step (2) is 60-90%, the baking temperature is 120-180° C., and the baking time is 0.5-5.0 minutes.

The anti-fibrillation treatment agent described in step (2) is trimethylolpropane-three (3-aziridinyl propionate), N, N-methylenebisacrylamide, 2,4-diamino -6-diallylamino-1,3,5-triazine, methyl ethyl ketoxime blocked hexamethylene diisocyanate, isophorone diisocyanate, polyoxyethylene laurate, epichlorohydrin hexamethylene diamine polycondensate , succinic acid, 3-hydroxy-1,3,5-pentanetriacic acid anti-fibrillation treatment agent or one or more.

The reactive dye described in step (3) is a vinyl sulfone type reactive dye; including reactive red AS, reactive orange 131, reactive blue 203, reactive blue 238, reactive black 5, reactive red 11, reactive yellow 160, reactive yellow 16, reactive Yellow 145, reactive red 194, reactive red 195, reactive red 198, reactive red 227, reactive red 240, reactive red 241, reactive red 261, reactive blue 8, reactive dark blue M-R, reactive blue 194, reactive blue 222, reactive blue 231 , Reactive Blue 19, etc.

The color-fixing solution described in step (3) is LR-01 Cerion.

The volume ratio of the dyeing solution described in step (3) and the color fast color solution is 4:1.

The liquid carrying rate described in step (3) is 60-90%.

The stacking temperature in step (3) is 10-40° C., and the stacking time is 3-16 hours.

Compared with the prior art, the present invention has the following beneficial effects:

(1) The present invention uses enzyme cold pad-batch desizing process to process lyocell woven fabric gray cloth, and under the synergistic effect of amylase and nonionic scouring penetrating agent, it is not necessary to carry out treatment procedures such as scouring and bleaching scouring, shortening The process saves dyeing and chemical auxiliaries, energy saving and environmental protection, and reduces the friction of fabrics, reducing the risk of fibrillation.

(2) The invention performs anti-fibrillation treatment on the lyocell woven fabric before dyeing, the process is simple, easy to operate, and the cost is low. Since the anti-fibrillation additive has multiple reactive groups, the hydroxyl groups on the fibers can be covalently bonded, thus enhancing the interaction between the fiber macromolecular chains and effectively inhibiting fibril splitting. For example, dimethyl ketoxime blocked hexamethylene diisocyanate, isophorone diisocyanate and other anti-fibrillation treatment agents are unblocked at high temperature, remove the blocking group, expose the isocyanate group, and then react with different molecules on the fiber The hydroxyl group on the chain undergoes an addition reaction. Trimethylolpropane-tris(3-aziridinyl propionate) anti-fibrillation treatment agent can undergo a ring-opening reaction at a lower temperature, and then exposes free methyl groups, free methyl groups and fibers The hydroxyl groups on different molecular chains undergo etherification reactions to form crosslinks. N, N-methylenebisacrylamide, 2,4-diamino-6-diallylamino-1,3,5-triazine and other anti-fibrillation additives are exposed alkenyl and different molecular chains of fibers Addition reaction of the hydroxyl groups on the fiber increases the lateral force between the fiber molecular chains, reduces its lateral swelling performance, and improves the anti-fibrillation ability. The epoxy groups of anti-fibrillation treatment agents such as polyoxyethylene laurate and epichlorohydrin hexamethylene diamine polycondensate open the ring under alkaline conditions, exposing the hydroxyl group, and the molecular chain between the lyocell fiber Different hydroxyl groups undergo substitution reactions to generate ether bonds, which increases the transverse force between fiber molecular chains and achieves the effect of preventing fibrillation. The carboxyl groups of anti-fibrillation treatment agents such as succinic acid and 3-hydroxy-1,3,5-glutaric acid undergo esterification reactions with different hydroxyl groups between the molecular chains of Lyocell fibers under alkaline conditions to form esters bond, increase the lateral force between the fiber molecular chains, and achieve the effect of preventing fibrillation.

(3) The present invention adopts the cold pad-batch salt-free dyeing process to carry out the dyeing of lyocell woven fabrics. Compared with the one-phase method and the two-phase method dyeing process, the friction between the fabric and the equipment is reduced, and the fibrillation tendency is reduced. In addition, no salt is used in the dyeing process, steaming is not required in the color fixing process, energy saving and environmental protection, and has great application prospects.

Description of drawings

Fig. 1 is the SEM picture enlarged 3000 times of the fiber surface after the step (1) treatment of embodiment 1.

Fig. 2 is a 3000 times enlarged SEM image of the fiber surface treated in step (1) of Comparative Example 1.

Fig. 3 is a 3000 times magnified SEM image of the fiber surface treated in step (1) of Comparative Example 3.

Fig. 4 is a 3000 times enlarged SEM image of the fiber surface of the lyocell fabric of Example 1 after the wet rubbing fastness test.

Figure 5 is a 3000 times magnified SEM image of the fiber surface of the lyocell fabric of Comparative Example 4 after the wet rubbing fastness test.

Figure 6 is a 3000 times magnified SEM image of the fiber surface of the lyocell fabric of Comparative Example 5 after the wet rubbing fastness test.

Fig. 7 is a 3000 times magnified SEM image of the fiber surface of the lyocell fabric of Comparative Example 6 after the wet rubbing fastness test.

Detailed ways

The present invention will be further described below in conjunction with the examples, but it does not limit the implementation of the present invention.

The TX-908 described in the comparative example of the present invention is purchased from Suzhou Jiesheng New Material Technology Co., Ltd.; scouring penetrating agent DX-3060, powder scouring agent DX-3001A, liquid scouring agent DX-3001B, wax-removing scouring agent DX- 128. Hydrogen peroxide stabilizer YJ-558A was purchased from Dongguan Jiahong Organic Silicon Technology Co., Ltd.; anti-swimming agent FM was purchased from Qingdao Dyne Chemical; LR-01 was purchased from Shandong Yellow River Delta Textile Technology Research Institute Co., Ltd. Soap flakes SFJJ were purchased from Dongguan Dongcheng Baifei Testing Instrument Company. The crosslinking agent SCA-8325 was purchased from Guangzhou Wanhua New Material Technology Co., Ltd.

All materials used in Comparative Examples and Examples are commercially available unless otherwise specified.

The padding equipment used in the examples and comparative examples of the present invention is a Werner Mathis AG type paddle car, and the stacking tool used is an HWL type oven.

Example 1

Cold pad-batch dyeing process to prevent fibrillation of lyocell woven fabrics, comprising the following steps:

(1) The lyocell woven fabric gray cloth is dipped and rolled twice with the treatment solution containing 12g/LDT-125 amylase and 2g/L of JFC penetrant, and the pH is adjusted to 4.5, and the liquid retention rate is controlled to 80%, at 25°C Roll up and stack for 12 hours, wash 2 times in hot water, then wash 2 times in normal temperature water, bath ratio 1:50, and dry;

(2) second-dipping and second-rolling the fabric in step (1) containing the solution of anti-fibrillation treatment agent N,N-methylenebisacrylamide, the concentration is 15g/L, and the liquid-carrying rate is controlled at 80%; drying; 125 Bake at ℃ for 2.5 minutes; wash 2 times with normal temperature water, 2 times with hot water, 1 time with soap (soaping agent 2g/L, bath ratio 1:30), 2 times with hot water, 2 times with normal temperature water, and dry.

(3) the lyocell woven fabric after the step (2) is dipped and rolled twice and the concentration is the former powder dyeing solution of reactive red AS of 35g/L and the LR-01 color fixing solution of 20g/L according to the volume ratio of 4 : 1 mixed working solution, control the liquid retention rate to 85%, rolled up and stacked at 25°C for 10 hours, washed lyocell woven fabrics after stacking with hot water twice, and soaped once (SFJJ 2g /L, bath ratio 1:30), washed twice at room temperature, bath ratio 1:50, and then dried.

Example 2

Cold pad-batch dyeing process to prevent fibrillation of lyocell woven fabrics, comprising the following steps:

(1) The gray cloth of lyocell woven fabric is soaked and rolled twice with the treatment solution containing 2g/LDT-125 amylase and 1g/L of JFC penetrating agent, and the pH is adjusted to 4, and the liquid carrying rate is controlled at 60%, at 10°C Roll up and stack for 12 hours, wash 2 times in hot water, then wash 2 times in normal temperature water, bath ratio 1:50, and dry;

(2) second dipping and second rolling of the fabric in step (1) contains the solution of anti-fibrillation treatment agent isophorone diisocyanate, the concentration is 5g/L, and the liquid retention rate is controlled at 60%; drying; min; wash 2 times with water at room temperature, 2 times with hot water, 1 time with soap (soaping agent 2g/L, bath ratio 1:30), 2 times with hot water, 2 times with room temperature, and dry.

(3) the LR-01 color-fixing solution that the lyocell woven fabric after the step (2) is processed is 5g/L active red AS former powder dyeing solution and the concentration is 5g/L by volume ratio 4 : 1 mixed working liquid, control the liquid retention rate to 60%, roll up and stack at 10°C for 16 hours, wash the stacked lyocell woven fabric twice with hot water, and wash once with 2g/L soap , washed twice at room temperature with a bath ratio of 1:50, and then dried.

Example 3

Cold pad-batch dyeing process to prevent fibrillation of lyocell woven fabrics, comprising the following steps:

(1) The gray cloth of lyocell woven fabric is soaked and rolled twice with the treatment liquid containing 14g/LDT-125 amylase and 5g/L of JFC penetrating agent, and the pH is adjusted to 6, and the liquid carrying rate is controlled at 90%, at 40°C Roll up and stack for 1 hour, wash 2 times with hot water, then wash 2 times with normal temperature water, bath ratio 1:50, and dry;

(2) The solution containing trimethylolpropane-three [3-(2-methyl aziridinyl) propionate] with the second dipping and second rolling of the fabric in step (1), the concentration is 35g/L, and the liquid is controlled 90%; bake at 120°C for 5 minutes; wash 2 times with water at room temperature, 2 times with hot water, 1 time with soap (soaping agent 2g/L, liquor ratio 1:30), 2 times with hot water, 2 times with water at room temperature, and dry Dry.

(3) the lyocell woven fabric after the step (2) process two dipping two rolling concentration is the reactive blue 194 dye liquor of 60g/L and the LR-01 color fixing solution of 40g/L according to the volume ratio 4:1 The mixed working solution, the liquid retention rate is controlled at 90%, rolled up and stacked at 40°C for 3 hours, the stacked lyocell woven fabric is washed twice with hot water, 2g/L soaped once, at room temperature Wash twice with water, the bath ratio is 1:50, and then dry.

Example 4

Cold pad-batch dyeing process to prevent fibrillation of lyocell woven fabrics, comprising the following steps:

(1) The gray cloth of lyocell woven fabric is dipped and rolled twice with the treatment liquid containing 12g/LDT-125 amylase and 3g/L of JFC penetrating agent, and the pH is adjusted to 4.5, and the liquid carrying rate is controlled at 80%, at 25°C Roll up and stack for 12 hours, wash 2 times in hot water, then wash 2 times in normal temperature water, bath ratio 1:50, and dry;

(2) second dipping and second rolling of the fabric in step (1) contains the solution of the anti-fibrillation treatment agent epoxy crosslinking agent SCA-8325, the concentration is 20g/L, and the liquid-carrying rate is controlled at 80%; drying; 175°C baking Bake for 2.5 minutes; wash 2 times with normal temperature water, 2 times with hot water, 1 time with soap (soaping agent 2g/L, liquor ratio 1:30), 2 times with hot water, 2 times with normal temperature water, and dry.

(3) the lyocell woven fabric after the step (2) is dipped and rolled twice and the concentration is the former powder dyeing solution of reactive red AS of 35g/L and the LR-01 color fixing solution of 20g/L according to the volume ratio of 4 : 1 mixed working solution, control the liquid retention rate to 85%, roll up and pile up at 25°C for 10 hours, wash the piled lyocell woven fabric twice with hot water, and wash once with 2g/L soap , washed twice at room temperature with a bath ratio of 1:50, and then dried.

Example 5

Cold pad-batch dyeing process to prevent fibrillation of lyocell woven fabrics, comprising the following steps:

(1) The gray cloth of lyocell woven fabric is soaked and rolled twice with the treatment liquid containing 8g/LDT-125 amylase and 4g/L of JFC penetrating agent, and the pH is adjusted to 4.5, and the liquid carrying rate is controlled at 80%, at 25°C Roll up and stack for 12 hours, wash 2 times in hot water, then wash 2 times in normal temperature water, bath ratio 1:50, and dry;

(2) second-dipping and second-rolling the fabric in step (1) with a solution containing the anti-fibrillation treatment agent 3-hydroxyl-1,3,5-pentanetrionic acid, the concentration is 5g/L, and the liquid-carrying rate is controlled at 80%; Dry; bake at 160°C for 2.5 minutes; wash twice at room temperature, wash twice with hot water, wash once with soap (soaping agent 2g/L, bath ratio 1:30), wash twice with hot water, wash twice with water at room temperature, and dry .

(3) the lyocell woven fabric after the step (2) is processed two dipping two rolling concentration is the former powder dye liquor of reactive red AS of 35g/L and the LR-01 color fixing solution that concentration is 25g/L according to volume ratio 4 : 1 mixed working liquid, control the liquid retention rate to 85%, rolled and stacked at 25°C for 10 hours, washed the Lyocell woven fabrics after stacking twice with hot water, and soaped once (soaping agent 2g/L, bath ratio 1:30), washed twice with water at room temperature, bath ratio 1:50, and then dried.

Comparative example 1

Lyocell woven fabric dyeing process includes the following steps:

(1) The gray cloth of lyocell woven fabric is dipped and rolled twice to the treatment solution containing iron ion chelating agent TX-9081g/L, scouring and penetrating agent DX-36F6g/L, NaOH20g/L, 35%H ₂ O ₂ 7g/L , control the liquid-carrying rate of 80%, roll and stack at 25°C for 15 hours, wash with hot water twice, bath ratio 1:50, and dry;

(2) the LR-01 color fixing solution that the lyocell woven fabric after the step (1) is processed is 35g/L active red AS former powder dyeing solution and the concentration is 20g/L according to volume ratio 4 : 1 mixed working solution, control the liquid retention rate to 85%, roll up and pile up at 25°C for 10 hours, wash the piled lyocell woven fabric twice with hot water, and wash once with 2g/L soap , washed twice at room temperature with a bath ratio of 1:50, and then dried.

Comparative example 2

Lyocell woven fabric dyeing process includes the following steps:

(1) the treatment liquid that contains iron ion chelating agent TX-9081g/L, NaOH15g/L, scouring and penetrating agent DX-30602.5g/L with lyocell woven gray cloth two dipping two rollings, the control liquid rate is 80%, Stack in saturated steam at 100°C, control the steaming time to 30 minutes, wash with room temperature water twice, bath ratio 1:50, and dry;

(2) the LR-01 color fixing solution that the lyocell woven fabric after the step (1) is processed is 35g/L active red AS former powder dyeing solution and the concentration is 20g/L according to volume ratio 4 : 1 mixed into the working liquid, the control liquid rate is 85%, rolled up and piled up at 25°C for 10 hours, the lyocell woven fabrics after the piled up were washed twice with hot water, washed once with 2g/L soap, Wash twice with water at room temperature, bath ratio is 1:50, and then dry.

Comparative example 3

Lyocell woven fabric dyeing process includes the following steps:

(1) The lyocell woven gray cloth is dipped and rolled twice with a treatment solution containing NaOH15g/L, and the liquid retention rate is controlled to 80%, and it is stacked at 100°C for saturated steaming, and the steaming time is controlled to be 30min, and washed with hot water for 2 times, bath ratio 1:50, drying;

(2) The lyocell woven fabric after step (1) is dipped and rolled twice contains ion chelating agent TX-9081g/L, powder scouring agent DX-3001A10g/L, liquid scouring agent DX-3001B2g/L, Wax scouring agent DX-1281g/L, hydrogen peroxide stabilizer YJ-558A 4g/L, 35% H ₂ O ₂ 6g/L treatment liquid, control pH at 10.75±0.25, control liquid retention rate to 80%, and saturate at 100°C Steam stacking, control the steaming time to 20min, wash with hot water twice, bath ratio 1:50, and dry;

(3) the lyocell woven fabric after the step (2) is dipped and rolled twice and the concentration is the former powder dyeing solution of reactive red AS of 35g/L and the LR-01 color fixing solution of 20g/L according to the volume ratio of 4 : 1 mixed working solution, control the liquid retention rate to 85%, roll up and pile up at 25°C for 10 hours, wash the piled lyocell woven fabric twice with hot water, and wash once with 2g/L soap , washed twice at room temperature with a bath ratio of 1:50, and then dried.

Comparative example 4

Lyocell woven fabric dyeing process includes the following steps:

(1) The gray cloth of lyocell woven fabric is dipped and rolled twice with the treatment liquid containing 12g/LDT-125 amylase and 3g/L of JFC penetrating agent, and the pH is adjusted to 4.5, and the liquid carrying rate is controlled at 80%, at 25°C Roll up and stack for 12 hours, wash 3 times in hot water, then wash 2 times in normal temperature water, bath ratio 1:50, and dry;

(2) The lyocell woven fabric after the step (1) treatment is dipped and rolled two times to contain the working solution of active red AS former powder 35g/L, anti-swimming agent FM15g/L, NaHCO ₃ 20g/L, NaCl50g/L , control the liquid-carrying rate at 70%; dry; steam at 100°C for 5 minutes; wash with water at room temperature 4 times, bath ratio 50:1; soap wash 2 times, bath ratio 50:1; hot water wash 2 times, bath ratio 50: 1; wash once at room temperature, bath ratio 50:1; dry.

Comparative example 5

Lyocell woven fabric dyeing process includes the following steps:

(1) The gray cloth of lyocell woven fabric is dipped and rolled twice with the treatment liquid containing 12g/LDT-125 amylase and 3g/L of JFC penetrating agent, and the pH is adjusted to 4.5, and the liquid carrying rate is controlled at 80%, at 25°C Roll up and stack for 12 hours, wash 2 times in hot water, then wash 2 times in normal temperature water, bath ratio 1:50, and dry;

(2) the lyocell woven fabric after the step (1) is processed is dipped and rolled two times and contains the former powder 35g/L of active red AS, and the working liquid of the anti-swimming agent FM15g/L controls the liquid-carrying rate at 70%; Dry; then soak and roll the color-fixing solution containing Na ₂ CO ₃ 20g/L, NaOH2g/L, and NaCl200g/L, control the liquid-carrying rate to 100%, steam at 100°C for 5min; 50:1; soaping twice, liquor ratio 50:1; hot water washing twice, liquor ratio 50:1; normal temperature water washing once, liquor ratio 50:1; drying.

Comparative example 6

Lyocell woven fabric dyeing process includes the following steps:

(1) The gray cloth of lyocell woven fabric is dipped and rolled twice with the treatment liquid containing 12g/LDT-125 amylase and 3g/L of JFC penetrating agent, and the pH is adjusted to 4.5, and the liquid carrying rate is controlled at 80%, at 25°C Roll up and stack for 12 hours, wash 2 times in hot water, then wash 2 times in normal temperature water, bath ratio 1:50, and dry;

(2) the LR-01 color fixing solution that the lyocell woven fabric after the step (1) is processed is 35g/L active red AS former powder dyeing solution and the concentration is 20g/L according to volume ratio 4 : 1 mixed working liquid, control the liquid retention rate to 85%, rolled and stacked at 25°C for 10 hours, washed lyocell woven fabrics after stacking with hot water at room temperature for 2 times, and soaped with 2g/L for 1 times, washed twice with normal temperature water, the bath ratio is 1:50, and finally dried.

According to GB/T17644-2008, according to CIE whiteness, fold the cloth sample into an opaque state, use Datacolor color measuring instrument to test under the standard light source D65, 10° viewing angle, measure 10 points and take the average value, and calculate according to Hunter's formula Whiteness: W _h ＝100-[(100-L ^* ) ² +a ^*2 +b ^*2]1/2

Table 1 Whiteness of lyocell fabrics with different pretreatment processes

Fabric pretreatment process CIE whiteness W_h gray cloth 81 Lyocell woven fabric after embodiment 1 step (1) process 91 Lyocell woven fabric after embodiment 2 step (1) process 90 Lyocell woven fabric after embodiment 3 step (1) process 90 Lyocell woven fabric after comparative example 1 step (1) process 89 Lyocell woven fabric after comparative example 2 step (1) processing 85 Lyocell woven fabric after comparative example 3 step (2) processing 91

It can be seen from the above table that the cold pad batch enzymatic desizing pretreatment process provided by the present invention has the same whiteness as the one-bath descaling and bleaching process, and the alkali desizing and scouring + bleaching process, and is better than the whiteness of the traditional alkali desizing and scouring process .

Use a Datacolor850 spectrophotometer to test the dyed fabric at any 10 points under a 10° viewing angle, a D65 light source, and a 30mm color measuring aperture. The fabric is folded to an opaque state, and the maximum absorption of the dyed fabric sample is measured 10 times. The apparent color depth (K/S value) at the wavelength.

Table 2 K/S value of Lyocell fabrics with different dyeing processes

It can be seen from the above table that the cold pad-batch salt-free dyeing process using vinylsulfone reactive dyes has a better color yield than the traditional one-phase and two-phase processes.

Wet rubbing fastness The rubbing fastness of dyed fabrics was tested according to GB/T3920-2008 "Textile Color Fastness Tests Color Fastness to Rubbing" using a rubbing color fastness meter.

Wet rubbing fastness Example 1 4-5 Example 2 4 Example 3 4-5 Example 4 4-5 Example 5 4-5 Comparative example 1 3-4 Comparative example 2 3-4 Comparative example 3 3 Comparative example 4 3-4 Comparative example 5 3-4 Comparative example 6 3-4

The lyocell woven fabric after embodiment 1 step (1) process, the lyocell woven fabric after comparative example 1 step (1) process, the lyocell woven fabric after comparative example 3 step (1) process, by SEM magnifies the lyocell fiber 3000 times, and observes the difference in the degree of fibrillation caused by different pretreatment processes on the fiber surface, as shown in Figure 1, Figure 2, and Figure 3. As can be seen from the figure, the enzymatic cold pad-batch desizing process used in the present invention has a lower fibrillation level than the one-bath process of cold pad-batch alkali desizing, scouring and bleaching and the traditional two-bath process of alkali desizing and bleaching.

The lyocell fabrics dyed in Example 1, Comparative Example 4, Comparative Example 5, and Comparative Example 6 are tested for wet rubbing fastness, and the wet rubbed Lyocell fabrics are magnified 3000 times by SEM, and the surface of the fabric is observed The differences in anti-fibrillation capabilities are shown in Figure 4, Figure 5, Figure 6, and Figure 7. As can be seen from the figure, the vinylsulfone reactive dye cold pad-batch salt-free dyeing process used in the present invention has better anti-fibrillation than the vinylsulfone reactive dye one-phase dyeing process and the vinylsulfone reactive dye two-phase dyeing process. ability, the anti-fibrillation ability of the lyocell woven fabric without carrying out the anti-fibrillation finishing process is still not as good as the solution provided by the present invention.

Claims (10)

1. the cold pad-batch dyeing process that can prevent fibrillation of lyocell woven fabric is characterized in that, comprises the following steps: (1) prepare the desizing working solution of 2-14g/L amylase and 1-5g/L penetrating agent, adjust the pH of the desizing working solution to be 4-6, and pad the lyocell woven fabric gray cloth after singeing Pulp working fluid, control the liquid rate, roll up and stack, wash with hot water, wash with normal temperature, and dry; (2) preparation concentration is the anti-fibrillation treatment agent solution of 5-35g/L, the fabric after step (1) is processed is pad-rolled the solution that contains anti-fibrillation treatment agent, controls liquid carrying rate, dries, bakes drying, washing, drying; (3) Prepare a reactive dye solution with a concentration of 5-60g/L and a color-fixing solution with a concentration of 5-40g/L, mix the prepared dye solution and color-fixing solution evenly in a certain proportion, and prepare the dyeing work liquid, the fabric treated in step (2) is pad-dyeed with the working liquid, the liquid-carrying rate is controlled, and after rolling and stacking, hot water washing, soap washing, cold water washing, and drying. 2. The cold pad-batch dyeing process capable of preventing fibrillation of lyocell woven fabrics according to claim 1, characterized in that the penetrating agent described in step (1) is a nonionic scouring penetrating agent. 3. The cold pad-batch dyeing process capable of preventing fibrillation of lyocell woven fabrics according to claim 1, characterized in that the liquid-carrying rate in step (1) is 60-90%. 4. the cold pad-batch dyeing process that can prevent lyocell woven fabric fibrillation according to claim 1, is characterized in that, the stacking temperature described in step (1) is 10-40 ℃, and the stacking time is 1-12 hours. 5. The cold pad-batch dyeing process capable of preventing fibrillation of lyocell woven fabrics according to claim 1, characterized in that the liquid-carrying rate in step (2) is 60-90%. 6. The cold pad-batch dyeing process that can prevent the fibrillation of lyocell woven fabrics according to claim 1, characterized in that, the baking temperature described in step (2) is 120-180°C, and the baking time is 0.5-180°C. 5.0 minutes. 7. the cold pad-batch dyeing process that can prevent lyocell woven fabric fibrillation according to claim 1, is characterized in that, the anti-fibrillation treatment agent described in step (2) is trimethylolpropane- Tris(3-aziridinylpropionate), N,N-methylenebisacrylamide, 2,4-diamino-6-diallylamino-1,3,5-triazine, methyl ethyl ketoxime blocked Hexamethylene diisocyanate, isophorone diisocyanate, polyoxyethylene laurate, polycondensate of epichlorohydrin hexamethylenediamine, succinic acid, 3-hydroxy-1,3,5-pentanetriacid One or more of the fibrillation treatment agents. 8. the cold pad-batch dyeing process that can prevent lyocell woven fabric fibrillation according to claim 1, is characterized in that, the reactive dyestuff described in step (3) is vinyl sulfone type reactive dyestuff. 9. The cold pad-batch dyeing process capable of preventing fibrillation of lyocell woven fabrics according to claim 1, characterized in that the liquid-carrying rate in step (3) is 60-90%. 10. the cold pad-batch dyeing process that can prevent lyocell woven fabric fibrillation according to claim 1, is characterized in that, the stacking temperature described in step (3) is 10-40 ℃, and the stacking time is 3-16 hours.

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