A low-temperature dyeing auxiliary agent for acetic acid fabrics and its application process

Abstract

The present invention provides a kind of acetate fabric low temperature dyeing auxiliary agent, the dyeing auxiliary agent includes the following ingredients: polyoxyethylene ether polyoxyethylene ether, sodium lignin sulfonate, peregal O 20, acetic acid, dispersant QTQ 108, porous gelatin ball and chitosan;The concentration of the dyeing and finishing auxiliary agent is:polyoxyethylene ether polyoxyethylene ether 1.8 2.5g / L, sodium lignin sulfonate 0.2 0.45g / L, peregal O 20 is 0.05 0.1g / L, acetic acid 5 10g / L, dispersant QTQ 108 is 0.5 1.2g / L, porous gelatin ball 10 20g / L, chitosan 2 5g / L, and the molecular weight of chitosan is 2000 5000Da. The present invention improves the coloring effect and the color fixing effect of acetate fiber dyeing at lower temperatures by adding modified gelatin microspheres in printing and dyeing auxiliary agents.

Description

Technical Field

[0001] The present invention relates to the field of printing and dyeing auxiliaries, and in particular to an acetic acid fabric low-temperature dyeing auxiliary and an application process thereof. Background Art

[0002] Cellulose acetate fiber, commonly known as acetate fiber, is produced from wood pulp. The cellulose in the fiber is acetylated to form a cellulose ester derivative, which is then dry-spun. It is one of the earliest chemical fibers developed in the world. Acetate fiber is divided into diacetate and triacetate depending on the degree to which the hydroxyl (-OH) groups in the cellulose are replaced by acetyl groups. Cellulose acetate fiber has a soft luster, excellent antistatic properties, good moisture absorption and quick drying properties, and a flowing fabric. It is widely used in the development of women's clothing fabrics and is very popular among consumers. However, cellulose acetate fiber has low strength, is not resistant to high temperatures, alkalis (including weak alkalis), and oxidants, and is difficult to print and dye. It also has significant coloring limitations and is prone to creases and chicken paw prints on the fabric.

[0003] Temperature control is crucial during the acetate fabric dyeing process, as it directly affects the dye's solubility, diffusion rate, and fiber absorption capacity. A suitable temperature ensures uniform dye uptake, improving dyeing quality and color fastness. If the temperature is too low, the dye may not fully dissolve, resulting in uneven dyeing and low uptake. Excessively high temperatures can cause the dye to decompose or volatilize, affecting dyeing results and color fastness. However, excessively high temperatures can also affect the fabric's dimensional stability and feel. Summary of the Invention

[0004] Technical problem to be solved: The purpose of the present invention is to provide a low-temperature dyeing auxiliary for acetate fabrics and its application process, by adding modified gelatin microspheres to the printing and dyeing auxiliary, to improve the coloring effect and fixing effect of acetate fiber dyed at lower temperatures.

[0005] Technical solution: A low-temperature dyeing auxiliary for acetate fabrics, the dyeing auxiliary comprising the following ingredients: polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, acetic acid, dispersant QTQ-108, porous gelatin balls and chitosan.

[0006] Preferably, the concentrations of the dyeing and finishing auxiliaries are: polyoxyethylene ether 1.8-2.5 g / L, sodium lignin sulfonate 0.2-0.45 g / L, peregal O-20 0.05-0.1 g / L, acetic acid 5-10 g / L, dispersant QTQ-108 0.5-1.2 g / L, porous gelatin spheres 10-20 g / L, chitosan 2-5 g / L, and the molecular weight of chitosan is 2000-5000 Da.

[0007] Preferably, the preparation method of the porous gelatin spheres is:

[0008] S11. Degumming the silk to obtain fibroin fibers, and chopping the fibroin fibers to obtain chopped fibroin fibers having a length of 0.5-2 cm;

[0009] S12. The chopped silk fibers were added to a formic acid solution for swelling, the swollen fibers were sheared at high speed, and filtered and washed to obtain nanosilk fibers;

[0010] S13. The nano-silk fibers were added to water and ultrasonically dispersed to obtain a 2-5wt% nano-silk fiber dispersion; S14. Gelatin was added to water to prepare a gelatin aqueous solution having a concentration of 10-20wt%;

[0011] S15. Calcium carbonate is added to the gelatin solution, stirred, and then the nanosilk fiber dispersion prepared in step S13 is added and stirred to obtain an aqueous phase;

[0012] S16. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion;

[0013] S17. The emulsion was placed in an ice bath, and then glutaraldehyde was added to cross-link and solidify to obtain gelatin microspheres;

[0014] S18. Add the gelatin microspheres to a dilute hydrochloric acid solution, heat and stir until no bubbles are generated in the solution, then stir and react for 5-10 minutes, filter, wash, and dry to obtain porous gelatin microspheres.

[0015] Preferably, in step S112, the concentration of formic acid is 80-98 wt %, the shearing speed is 2000-5000 r / min, and the shearing time is 5-10 min.

[0016] Preferably, in step S15, the content of calcium carbonate in the gelatin solution is 3-6 wt %, and the volume ratio of the gelatin solution to the nano-silk fiber dispersion is 1:1.

[0017] Preferably, in step S17, the volume ratio of glutaraldehyde to emulsion is 1-2:100.

[0018] Preferably, the concentration of dilute hydrochloric acid in step S178 is 0.1-0.5 mol / L, and the heating temperature is 20-30°C.

[0019] The application process of the above-mentioned low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0020] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0021] S2. Dyeing treatment: The pre-treated acetic acid fabric is placed in a dyeing machine, the water temperature is heated to 40 ° C, then the anti-wrinkle agent TF-208L and the leveling agent TF-212W are added, and the temperature is kept for 5-10 minutes. Acetic acid is added and the temperature is kept for 5 minutes. Chitosan is added and the temperature is kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls are added. After keeping the temperature for 5 minutes, the dye is added and the machine is operated after 10 minutes. The temperature is raised to 70 ° C for 10 minutes at a heating rate of 1-1.5 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine is operated for 30-60 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0022] S3. post-treating the dyed acetate fiber to obtain acetate fabric.

[0023] Preferably, the concentration of the anti-wrinkle agent TF-208L is 0.5-1 g / L, and the concentration of the leveling agent TF-212W is 0.5-1 g / L.

[0024] Beneficial effects: The low-temperature dyeing auxiliary agent for acetic acid fabrics of the present invention has the following advantages:

[0025] 1. In the present invention, the surface of the cellulose acetate has hydroxyl groups that are not replaced by acetyl groups, but the hydroxyl content is relatively low. Chitosan has hydroxyl groups and amino groups. Chitosan plays a dual role in the additive. First, chitosan can bind to the active groups on the surface of the cellulose acetate, bonding the porous gelatin spheres to the surface of the fabric in the form of a bridge. Second, the hydroxyl groups and amino groups of chitosan can react with the active groups in the dye, thereby improving the fastness of the dye. In the present invention, chitosan with a relatively small molecular weight is selected. The short molecular chain of chitosan does not affect the adsorption of dyes by the porous gelatin spheres.

[0026] 2. In the present invention, porous gelatin balls are added to the auxiliary agent. The gelatin balls are composed of gelatin and nano-silk fibers. The porous structure of the gelatin balls can adsorb more dyes, and the nano-structure of the nano-silk fibers exposes more hydroxyl and carboxyl groups on the surface. When the acetic acid fabric is dyed, the adsorption capacity of the dye molecules can be improved. The porous structure can accommodate more dye molecules faster, thereby improving the dyeing efficiency of the acetic acid fabric. DETAILED DESCRIPTION

[0027] The present invention will be further described below in conjunction with examples, which are provided to explain the present invention and are not limited to the following examples:

[0028] Example 1

[0029] The preparation method of porous gelatin spheres is as follows:

[0030] S11. Degumming the silk to obtain fibroin fibers, and chopping the fibroin fibers to obtain chopped fibroin fibers having a length of 0.5-2 cm;

[0031] S12. The chopped silk fibers were added to an 80 wt % formic acid solution and swollen for 60 min. The swollen fibers were sheared at a high speed of 5000 r / min for 5 min, and filtered and washed to obtain nanosilk fibers.

[0032] S13. The nano-silk fibers were added to water and ultrasonically dispersed to obtain a 2 wt% nano-silk fiber dispersion; S14. Gelatin was added to water to prepare a 10 wt% gelatin aqueous solution;

[0033] S15. Calcium carbonate was added to the gelatin solution, the content of calcium carbonate in the gelatin solution was 3 wt %, and after stirring, the nano-silk fiber dispersion prepared in step S13 was added, the volume ratio of the gelatin solution and the nano-silk fiber dispersion was 1:1, and stirred to obtain an aqueous phase;

[0034] S16. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion;

[0035] S17. The emulsion was placed in an ice bath, and then glutaraldehyde was added, with the volume ratio of glutaraldehyde to emulsion being 1:100, and cross-linked and solidified to obtain gelatin microspheres;

[0036] S18. Add the gelatin microspheres to a 0.1 mol / L dilute hydrochloric acid solution, heat to 20°C, and stir until no bubbles are generated in the solution. Then stir and react for 10 minutes. Filter, wash, and dry to obtain porous gelatin microspheres.

[0037] Example 2

[0038] The preparation method of porous gelatin spheres is as follows:

[0039] S11. Degumming the silk to obtain fibroin fibers, and chopping the fibroin fibers to obtain chopped fibroin fibers having a length of 0.5-2 cm;

[0040] S12. The chopped silk fibers were added to a 98 wt % formic acid solution and swollen for 20 min. The swollen fibers were sheared at a high speed of 2000 r / min for 10 min, and filtered and washed to obtain nanosilk fibers.

[0041] S13. The nano-silk fibers were added to water and ultrasonically dispersed to obtain a 5 wt% nano-silk fiber dispersion; S14. Gelatin was added to water to prepare a 20 wt% gelatin aqueous solution;

[0042] S15. Calcium carbonate was added to the gelatin solution, the content of calcium carbonate in the gelatin solution was 6 wt %, and after stirring, the nano-silk fiber dispersion prepared in step S13 was added, the volume ratio of the gelatin solution and the nano-silk fiber dispersion was 1:1, and stirred to obtain an aqueous phase;

[0043] S16. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion;

[0044] S17. The emulsion was added and placed in an ice bath, and then glutaraldehyde was added, with the volume ratio of glutaraldehyde to the emulsion being 1:50, and cross-linked and solidified to obtain gelatin microspheres;

[0045] S18. Add the gelatin microspheres to a 0.5 mol / L dilute hydrochloric acid solution, heat to 30°C, and stir until no bubbles are generated in the solution. Then stir and react for 5 minutes. Filter, wash, and dry to obtain porous gelatin microspheres.

[0046] Example 3

[0047] The preparation method of porous gelatin spheres is as follows:

[0048] S11. Degumming the silk to obtain fibroin fibers, and chopping the fibroin fibers to obtain chopped fibroin fibers having a length of 0.5-2 cm;

[0049] S12. The chopped silk fibers were added to a 92 wt% formic acid solution and swollen for 50 min. The swollen fibers were sheared at a high speed of 4000 r / min for 5 min, and filtered and washed to obtain nanosilk fibers.

[0050] S13. The nano-silk fibers were added to water and ultrasonically dispersed to obtain a 3 wt% nano-silk fiber dispersion; S14. Gelatin was added to water to prepare a 13 wt% gelatin aqueous solution;

[0051] S15. Calcium carbonate was added to the gelatin solution, the content of calcium carbonate in the gelatin solution was 5 wt %, and after stirring, the nano-silk fiber dispersion prepared in step S13 was added, the volume ratio of the gelatin solution and the nano-silk fiber dispersion was 1:1, and stirred to obtain an aqueous phase;

[0052] S16. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion;

[0053] S17. The emulsion was added and placed in an ice bath, and then glutaraldehyde was added, the volume ratio of glutaraldehyde to the emulsion was 1.8:100, cross-linked and solidified to obtain gelatin microspheres;

[0054] S18. Add the gelatin microspheres to a 0.3 mol / L dilute hydrochloric acid solution, heat to 30°C, and stir until no bubbles are generated in the solution. Then stir and react for 5 minutes. Filter, wash, and dry to obtain porous gelatin microspheres.

[0055] Example 4

[0056] The preparation method of porous gelatin spheres is as follows:

[0057] S11. Degumming the silk to obtain fibroin fibers, and chopping the fibroin fibers to obtain chopped fibroin fibers having a length of 0.5-2 cm;

[0058] S12. The chopped silk fibers were added to a 96 wt % formic acid solution and swollen for 40 min. The swollen fibers were sheared at a high speed of 3000 r / min for 10 min, and filtered and washed to obtain nanosilk fibers.

[0059] S13. The nano-silk fibers were added to water and ultrasonically dispersed to obtain a 4 wt% nano-silk fiber dispersion; S14. Gelatin was added to water to prepare a gelatin aqueous solution having a concentration of 18 wt%;

[0060] S15. Calcium carbonate was added to the gelatin solution, the content of calcium carbonate in the gelatin solution was 4 wt %, and after stirring, the nano-silk fiber dispersion prepared in step S13 was added, the volume ratio of the gelatin solution and the nano-silk fiber dispersion was 1:1, and stirred to obtain an aqueous phase;

[0061] S16. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion;

[0062] S17. The emulsion was added and placed in an ice bath, and then glutaraldehyde was added, the volume ratio of glutaraldehyde to the emulsion was 1.2:100, cross-linked and solidified to obtain gelatin microspheres;

[0063] S18. Add the gelatin microspheres to a 0.4 mol / L dilute hydrochloric acid solution, heat to 20°C, and stir until no bubbles are generated in the solution. Then stir and react for 10 minutes. Filter, wash, and dry to obtain porous gelatin microspheres.

[0064] Porous gelatin microspheres Example 1 365.2 Example 2 333.9 Example 3 385.1 Example 4 365.8

[0065] Example 5

[0066] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0067] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0068] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 5 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 60 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0069] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0070] Among them, the anti-wrinkle agent TF-208L is 1 g / L, the leveling agent TF-212W is 0.5 g / L, polyoxyethylene polyoxyethylene ether is 1.8 g / L, sodium lignin sulfonate is 0.45 g / L, peregal O-20 is 0.1 g / L, acetic acid is 5 g / L, the dispersant QTQ-108 is 1.2 g / L, the porous gelatin spheres prepared in Example 1 are 10 g / L, and chitosan is 2 g / L, and the molecular weight of chitosan is 2000 Da.

[0071] Example 6

[0072] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0073] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0074] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 10 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1.5 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 30 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0075] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0076] Among them, the anti-wrinkle agent TF-208L is 0.5 g / L, the leveling agent TF-212W is 1 g / L, polyoxyethylene polyoxyethylene ether 2.5 g / L, sodium lignin sulfonate 0.2 g / L, 0.05 g / L of peregal O-20, 10 g / L of acetic acid, 0.5 g / L of dispersant QTQ-108, 20 g / L of porous gelatin balls prepared in Example 2, and 5 g / L of chitosan, and the molecular weight of chitosan is 5000 Da.

[0077] Example 7

[0078] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0079] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0080] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 6 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 50 minutes and the temperature was lowered to 70 ° C / min at a cooling rate of 2 ° C / min.

[0081] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0082] Among them, the anti-wrinkle agent TF-208L is 0.6 g / L, the leveling agent TF-212W is 0.9 g / L, polyoxyethylene polyoxyethylene ether 2 g / L, sodium lignin sulfonate 0.25 g / L, 0.06 g / L of peregal O-20, 6 g / L of acetic acid, 0.8 g / L of dispersant QTQ-108, 13 g / L of porous gelatin balls prepared in Example 3, and 3 g / L of chitosan, and the molecular weight of chitosan is 3000 Da.

[0083] Example 8

[0084] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0085] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0086] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 9 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1.5 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 40 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0087] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0088] Among them, the anti-wrinkle agent TF-208L is 0.9 g / L, the leveling agent TF-212W is 0.6 g / L, polyoxyethylene polyoxyethylene ether 2.4 g / L, sodium lignin sulfonate 0.4 g / L, 0.09 g / L of peregal O-20, 9 g / L of acetic acid, 1 g / L of dispersant QTQ-108, 18 g / L of porous gelatin balls prepared in Example 4, 4 g / L of chitosan, and the molecular weight of chitosan is 4000 Da.

[0089] Comparative Example 1

[0090] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0091] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0092] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 9 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1.5 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 40 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0093] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0094] Among them, the anti-wrinkle agent TF-208L is 0.9 g / L, the leveling agent TF-212W is 0.6 g / L, polyoxyethylene polyoxyethylene ether 2.4 g / L, sodium lignin sulfonate 0.4 g / L, 0.09 g / L of peregal O-20, 9 g / L of acetic acid, 1 g / L of dispersant QTQ-108, 18 g / L of porous gelatin balls prepared in Example 4, 3 g / L of chitosan, and the molecular weight of chitosan is 2000 Da.

[0095] Comparative Example 2

[0096] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0097] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0098] S2. Dyeing treatment: The pre-treated acetate fabric was placed in a dyeing machine and the water temperature was heated to 40°C. Then, the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added. The temperature was kept warm for 9 minutes, and acetic acid was added. The temperature was kept warm for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping warm for 5 minutes, disperse black ECT was added. After 10 minutes, the machine was operated. The temperature was raised to 70°C at a heating rate of 1.5°C / min for 10 minutes, and then raised to 95°C at a heating rate of 0.6°C / min. The machine was operated for 40 minutes and cooled to 70°C / min at a cooling rate of 2°C / min.

[0099] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0100] Among them, the anti-wrinkle agent TF-208L is 0.9 g / L, the leveling agent TF-212W is 0.6 g / L, polyoxyethylene polyoxyethylene ether is 2.4 g / L, sodium lignin sulfonate is 0.4 g / L, peregal O-20 is 0.09 g / L, acetic acid is 6 g / L, dispersant QTQ-108 is 1 g / L, and the porous gelatin balls prepared in Example 4 are 18 g / L.

[0101] Comparative Example 3

[0102] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0103] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0104] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 5 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 60 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0105] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0106] Among them, the anti-wrinkle agent TF-208L is 1g / L, the leveling agent TF-212W is 0.5g / L, polyoxyethylene polyoxyethylene ether 1.8g / L, sodium lignin sulfonate 0.45g / L, peregal O-20 0.1g / L, acetic acid 5g / L, dispersant QTQ-108 is 1.2g / L, porous gelatin spheres 10g / L, chitosan 2g / L, and the molecular weight of chitosan is 3000Da;

[0107] The preparation method of porous gelatin spheres is as follows:

[0108] S11. Adding gelatin to water to prepare a gelatin aqueous solution having a concentration of 10 wt%;

[0109] S12. Calcium carbonate was added to the gelatin solution, the content of calcium carbonate in the gelatin solution was 5 wt %, and the mixture was stirred to obtain an aqueous phase; S13. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase being 1:10, and stirred vigorously to obtain an emulsion;

[0110] S14. The emulsion was added and placed in an ice bath, and then glutaraldehyde was added, the volume ratio of glutaraldehyde to the emulsion was 1.8:100, cross-linked and solidified to obtain gelatin microspheres;

[0111] S15. Add the gelatin microspheres to a 0.3 mol / L dilute hydrochloric acid solution, heat to 30°C, and stir until no bubbles are generated in the solution. Then stir and react for 5 minutes. Filter, wash, and dry to obtain porous gelatin microspheres.

[0112] Comparative Example 4

[0113] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0114] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0115] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 5 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 60 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0116] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0117] Among them, the anti-wrinkle agent TF-208L is 1g / L, the leveling agent TF-212W is 0.5g / L, polyoxyethylene polyoxyethylene ether 1.8g / L, sodium lignin sulfonate 0.45g / L, peregal O-20 0.1g / L, acetic acid 5g / L, dispersant QTQ-108 is 1.2g / L, porous gelatin spheres 10g / L, chitosan 2g / L, and the molecular weight of chitosan is 3000Da;

[0118] The preparation method of porous gelatin spheres is as follows:

[0119] S11. Degumming the silk to obtain fibroin fibers, and chopping the fibroin fibers to obtain chopped fibroin fibers having a length of 0.5-2 cm;

[0120] S12. The chopped silk fibers were added to a 92 wt% formic acid solution and swollen for 50 min. The swollen fibers were sheared at a high speed of 4000 r / min for 5 min, and filtered and washed to obtain nanosilk fibers.

[0121] S13. The nano-silk fibers were added to water and ultrasonically dispersed to obtain a 3 wt% nano-silk fiber dispersion; S14. Gelatin was added to water to prepare a 13 wt% gelatin aqueous solution;

[0122] S15. Calcium carbonate was added to the gelatin solution, the content of calcium carbonate in the gelatin solution was 5 wt %, and after stirring, the nano-silk fiber dispersion prepared in step S13 was added, the volume ratio of the gelatin solution and the nano-silk fiber dispersion was 1:1, and stirred to obtain an aqueous phase;

[0123] S16. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion;

[0124] S17. The emulsion was added and placed in an ice bath, and then glutaraldehyde was added, the volume ratio of glutaraldehyde to the emulsion was 1.8:100, cross-linked and solidified to obtain gelatin microspheres;

[0125] S18. Add the gelatin microspheres to a 0.3 mol / L dilute hydrochloric acid solution, heat to 30°C, and stir until no bubbles are generated in the solution. Filter, wash, and dry to obtain porous gelatin microspheres.

[0126] Comparative Example 5

[0127] The application process of the low-temperature dyeing auxiliary agent for acetate fabrics includes the following steps:

[0128] S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface of the fabric.

[0129] S2. Dyeing treatment: The pre-treated acetic acid fabric was placed in a dyeing machine, the water temperature was heated to 40 ° C, and then the anti-wrinkle agent TF-208L and the leveling agent TF-212W were added, and the temperature was kept for 5 minutes. Acetic acid was added and the temperature was kept for 5 minutes. Chitosan was added and the temperature was kept for 5 minutes. Polyoxyethylene polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108 and porous gelatin balls were added. After keeping the temperature for 5 minutes, disperse black ECT was added and the machine was run for 10 minutes. The temperature was raised to 70 ° C for 10 minutes at a heating rate of 1 ° C / min, and then raised to 95 ° C at a heating rate of 0.6 ° C / min. The machine was run for 60 minutes and cooled to 70 ° C / min at a cooling rate of 2 ° C / min.

[0130] S3. The dyed acetate fiber is post-treated to obtain acetate fabric;

[0131] Among them, the anti-wrinkle agent TF-208L is 1g / L, the leveling agent TF-212W is 0.5g / L, polyoxyethylene polyoxyethylene ether 1.8g / L, sodium lignin sulfonate 0.45g / L, peregal O-20 0.1g / L, acetic acid 5g / L, dispersant QTQ-108 is 1.2g / L, porous gelatin spheres 10g / L, chitosan 2g / L, and the molecular weight of chitosan is 3000Da;

[0132] The preparation method of porous gelatin spheres is as follows:

[0133] S11. The silk fibroin powder was added to water and ultrasonically dispersed to obtain a 3 wt % silk fibroin powder dispersion;

[0134] S12. The gelatin was added to water to prepare a gelatin aqueous solution having a concentration of 13 wt%;

[0135] S13. Calcium carbonate was added to the gelatin solution, the content of calcium carbonate in the gelatin solution was 5 wt %, and after stirring, the silk fibroin powder dispersion prepared in step S11 was added, the volume ratio of the gelatin solution and the silk fibroin powder dispersion was 1:1, and stirred to obtain an aqueous phase;

[0136] S14. The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion;

[0137] S15. The emulsion was added and placed in an ice bath, and then glutaraldehyde was added, the volume ratio of glutaraldehyde to the emulsion was 1.8:100, cross-linked and solidified to obtain gelatin microspheres;

[0138] S16. Add the gelatin microspheres to a 0.3 mol / L dilute hydrochloric acid solution, heat to 30°C, and stir until no bubbles are generated in the solution. Filter, wash, and dry to obtain porous gelatin microspheres.

[0139] Color fastness test:

[0140] Color fastness to rubbing: tested according to GB / T3920-2008;

[0141] Color fastness to washing: tested according to GB / T3921-2008;

[0142] Color fastness to water: tested according to GB / T5713-2013.

[0143] Color fastness to rubbing

[0144] Dry friction / level Wet friction / level Example 5 5 4-5 Example 6 5 5 Example 7 5 4-5 Example 8 5 4-5 Comparative Example 1 4-5 4 Comparative Example 2 4 3-4 Comparative Example 3 3-4 3-4 Comparative Example 4 4-5 4 Comparative Example 5 4 3-4

[0145] Color fastness to washing

[0146] Color change / level Hair staining / grade Cotton staining / grade Example 5 4-5 4-5 4-5 Example 6 5 4-5 4-5 Example 7 5 5 4-5 Example 8 4-5 5 4-5 Comparative Example 1 4 4 3-4 Comparative Example 2 4 3-4 4 Comparative Example 3 3-4 3-4 3-4 Comparative Example 4 4 4 4 Comparative Example 5 4 4 4

[0147] Color fastness to washing

[0148] Color change / level Hair staining / grade Cotton staining / grade Example 5 4-5 5 4-5 Example 6 5 5 4-5 Example 7 4-5 4-5 5 Example 8 5 5 4-5 Comparative Example 1 4 4 4 Comparative Example 2 4 3-4 3-4 Comparative Example 3 3-4 4 3-4 Comparative Example 4 4 4-5 4 Comparative Example 5 4 4 4

[0149] Obviously, the above embodiments are merely examples for clarity of explanation and are not intended to limit the implementation methods. Those skilled in the art will readily appreciate that other variations or modifications based on the above descriptions are possible. It is not necessary and impossible to enumerate all implementation methods here. Obvious variations or modifications arising therefrom remain within the scope of protection of the present invention.

Claims

1. A low-temperature dyeing auxiliary agent for acetic acid fabrics, characterized by: The concentrations of the dyeing auxiliaries are: polyoxyethylene ether 1.8-2.5 g / L, sodium lignin sulfonate 0.2-0.45 g / L, peregal O-20 0.05-0.1 g / L, acetic acid 5-10 g / L, dispersant QTQ-108 0.5-1.2 g / L, porous gelatin spheres 10-20 g / L, chitosan 2-5 g / L, and the molecular weight of chitosan is 2000-5000 Da; The preparation method of the porous gelatin spheres is as follows: S11. The silk was degummed to obtain fibroin fibers, and the fibroin fibers were chopped to obtain chopped fibroin fibers having a length of 0.5-2 cm; S12. The chopped silk fibers were added to a formic acid solution for swelling, the swollen fibers were sheared at high speed, filtered and washed to obtain nanosilk fibers; S13. The nano-silk fibers were added to water and ultrasonically dispersed to obtain a concentration of 2-5wt% nano-silk fiber dispersion; S14. The gelatin is added to water to prepare a gelatin aqueous solution having a concentration of 10-20wt%; S15. Calcium carbonate was added to the gelatin solution, stirred, and the nanosilk fiber dispersion prepared in step S13 was added and stirred to obtain an aqueous phase; S16 The aqueous phase was added dropwise to the oil phase of liquid paraffin and Span 80 in a volume ratio of 19:1, the volume ratio of the aqueous phase to the oil phase was 1:10, and stirred vigorously to obtain an emulsion; S17. The emulsion was added and placed in an ice bath, and then glutaraldehyde was added to cross-link and solidify to obtain gelatin microspheres; S18. Add the gelatin microspheres to a dilute hydrochloric acid solution, heat and stir until no bubbles are generated in the solution, then stir and react for 5-10 minutes. Filter, wash, and dry to obtain porous gelatin microspheres.

2. The low-temperature dyeing auxiliary agent for acetate fabric according to claim 1, characterized in that: In step S12, the concentration of formic acid is 80-98 wt %, the shearing speed is 2000-5000 r / min, and the shearing time is 5-10 min.

3. The low-temperature dyeing auxiliary agent for acetate fabric according to claim 1, characterized in that: In step S15, the content of calcium carbonate in the gelatin solution is 3-6 wt %, and the volume ratio of the gelatin solution to the nano-silk fiber dispersion is 1:

1.

4. The low-temperature dyeing auxiliary agent for acetate fabric according to claim 1, characterized in that: In step S17, the volume ratio of glutaraldehyde to emulsion is 1-2:

100.

5. The low-temperature dyeing auxiliary agent for acetate fabric according to claim 1, characterized in that: In step S18, the concentration of dilute hydrochloric acid is 0.1-0.5 mol / L, and the heating temperature is 20-30°C.

6. The application process of the low-temperature dyeing auxiliary agent for acetate fabrics according to any one of claims 1 to 5, characterized in that: The following steps are involved: S1. Pretreatment: Desizing the acetate fabric to remove oil and sizing from the surface. S2. Dyeing: Place the pretreated acetic acid fabric in a dyeing machine and heat the water to 40°C. Then, add the anti-wrinkle agent TF-208L and the leveling agent TF-212W. Keep the temperature for 5-10 minutes. Then add acetic acid and keep the temperature for 5 minutes. Then add chitosan and keep the temperature for 5 minutes. Then add polyoxyethylene ether, sodium lignin sulfonate, peregal O-20, dispersant QTQ-108, and porous gelatin balls. Keep the temperature for 5 minutes, then add the dye. After 10 minutes, operate the machine. Ramp up to 70°C at a rate of 1-1.5°C / min for 10 minutes, then to 95°C at a rate of 0.6°C / min. Run the machine for 30-60 minutes, and then cool to 70°C / min at a rate of 2°C / min. S3. Post-treating the dyed acetate fiber to obtain acetate fabric.

7. The application process of the low-temperature dyeing auxiliary agent for acetate fabrics according to claim 6, characterized in that: The concentration of the anti-wrinkle agent TF-208L is 0.5-1 g / L, and the concentration of the leveling agent TF-212W is 0.5-1 g / L.