Dyeing process of bio-based fabric
By using compound enzyme hydrolysis and grafting ethyl methacrylate phosphate treatment, the problem of insufficient dyeing performance of PLA fabric was solved, achieving efficient and economical dyeing results, and improving dyeing performance and environmental friendliness.
Patent Information
- Application Number
- CN202511181564.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-22
- Publication Date
- 2025-11-11
AI Technical Summary
Polylactic acid (PLA) fiber dyeing suffers from low dye uptake and color fastness, high processing sensitivity, and a trade-off between environmental protection and cost. Traditional dyeing processes struggle to balance performance and sustainability.
A compound enzyme hydrolysis treatment is used to generate carboxyl groups on the surface of bio-based fabrics, and ethyl methacrylate is grafted onto the fabric to improve dye affinity and diffusion ability, thus simplifying the dyeing process.
It improves the dyeing performance and color fastness of PLA fabrics, reduces processing sensitivity, simplifies the dyeing process, and has certain flame retardant and moisture-absorbing properties, resulting in significant economic benefits.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of textile fabrics, specifically to a dyeing process for bio-based fabrics. Background Technology
[0002] Polylactic acid (PLA) fiber is a fully bio-based synthetic fiber made from renewable agricultural crops such as corn and wheat through fermentation to produce lactic acid, followed by polymerization and spinning. As a green and environmentally friendly material, its core advantage lies in its complete degradation into water and carbon dioxide under industrial composting conditions, reducing life-cycle carbon emissions by more than 75% compared to polyester. It also possesses natural antibacterial properties (e.g., an antibacterial rate of over 99% against Staphylococcus aureus), weak acidity (pH≈5.5), and moisture-wicking and quick-drying functions. However, the high crystallinity and strong hydrophobicity of its molecular chains make dye penetration difficult, and its thermal stability is significantly lower than that of conventional synthetic fibers, posing potential risks for subsequent dyeing processes.
[0003] PLA fabrics, thanks to their biocompatibility and functional properties, have achieved large-scale application in three major fields: medical, textile, and industrial. In the medical field, they are certified by the National Medical Products Administration for use in absorbable surgical sutures, antibacterial dressings, and implantable stents, meeting all biosafety standards (sensitization / irritation / cytotoxicity). In the textile field, they are primarily used in sports underwear and functional clothing (such as the PLON series from Guyuan Biotechnology), utilizing their mildly acidic, skin-friendly, and moisture-wicking properties to optimize the wearing experience. In the industrial field, they replace petroleum-based nonwoven fabrics, covering food packaging (FDA certified), automotive interiors, and filtration materials. Their core competitiveness lies in their low-carbon attributes throughout the entire supply chain, from raw material cultivation to finished product recycling, precisely aligning with global carbon neutrality policies and brand environmental traceability needs. Mature supply chain systems have been established in Europe and the United States.
[0004] PLA dyeing faces three major technical bottlenecks: First, low dye uptake and color fastness. The hydrophobic surface results in a disperse dye adsorption rate of less than 30%, easily leading to "white core" defects. Furthermore, wash / sunlight fastness is generally only grade 2-3 (requiring microencapsulation technology to improve to grade 3-4). Second, significant processing sensitivity. Dyeing temperatures exceeding 110℃ can cause fiber shrinkage and degradation (breaking strength decreases by >15%). Alkaline environments (pH >7) are more prone to hydrolyzing molecular chain ester bonds, requiring strict control of alkali concentration ≤2g / L during pretreatment. Third, a conflict between environmental protection and cost. Traditional processes rely on high temperature, high pressure, and benzyl alcohol auxiliaries, resulting in heavy energy consumption and wastewater treatment burdens. While solution dyeing methods (such as adding masterbatch) avoid dyeing, they sacrifice mechanical properties (strength and toughness drop sharply when pigment content >2.5%). Current patented technologies mainly focus on the development of low-temperature carriers (such as microencapsulated dyes) and bio-enzyme modification, aiming to overcome the balance barrier between performance and sustainability. Summary of the Invention
[0005] Technical problem to be solved: The present invention provides a dyeing process for bio-based fabrics, which generates carboxyl groups on the surface of bio-based fabrics by enzymatic hydrolysis with a compound enzyme, and then grafts ethyl methacrylate onto the surface of the fabric, thereby improving the dyeing performance of bio-based fabrics.
[0006] Technical solution: A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: The bio-based fabric is placed in a compound enzyme solution and heated to obtain a bio-based fabric containing carboxyl groups. In this invention, serine hydrolase and carboxyl esterase are combined to hydrolyze bio-based fabrics. The serine hydrolase cleaves the ester bonds in the PLA main chain to directly generate terminal carboxyl groups; the carboxyl esterase hydrolyzes intermediate oligomers to release lactic acid monomers containing α-carboxyl groups. The two enzymes work together to achieve efficient accumulation of carboxyl groups, enabling the bio-based fabric to generate carboxyl groups, which facilitates subsequent grafting. S2. Surface grafting: The carboxyl-containing bio-based fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate, and then heated to obtain ethyl methacrylate-grafted bio-based fabric. In this invention, ethyl methacrylate undergoes a free radical graft copolymerization reaction with the carboxyl groups generated by the enzymatic hydrolysis pretreatment in S1, thereby grafting ethyl methacrylate onto the surface of the bio-based fabric. S3. Cationic dyeing: The bio-based fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye and then heated to obtain the dyed bio-based fabric. S4. Post-treatment: The bio-based fabric obtained in S3 is washed with water, soaped and dried to obtain dyed bio-based fabric.
[0007] Preferably, the bio-based fabric is a nylon / PLA fabric, and the blending ratio of the nylon / PLA fabric is 2~4:6~8.
[0008] In this invention, the phosphate group (pKa≈1.5~2.5) of ethyl methacrylate ionizes into a negative charge in the dyeing environment (acidic environment), significantly improving its affinity for cationic dyes. Furthermore, the phosphate group weakens the hydrogen bonds between bio-based molecular chains, lowering the glass transition temperature of PLA and making it easier for dyes to diffuse into the amorphous region. In addition, the short fatty acid chain (ethyl) of ethyl methacrylate can insert into the PLA molecular chains, reducing local crystallinity and increasing the amorphous region within the fiber, thus acting as a plasticizer. Simultaneously, it avoids excessive hydrophobicity caused by long chains, improving the dyeing performance of nylon / PLA fabrics. Preferably, the compound enzyme solution in S1 contains serine hydrolase and carboxyl esterase in a mass ratio of 1:1 to 3; The concentration of the compound enzyme solution in S1 is 1~10g / L; The pH of the compound enzyme solution in S1 is 7.0~7.5.
[0009] Preferably, the heating treatment in S1 takes 1 to 2 hours and the temperature is 50 to 60°C.
[0010] Preferably, the mass ratio of ethyl methacrylate to potassium persulfate in S2 is 10~20:1; The ratio of the carboxyl-containing bio-based fabric in S2 to the solution containing ethyl methacrylate and potassium persulfate is 1:10~30.
[0011] Preferably, the heating reaction in S2 is carried out at a temperature of 60-80°C for 1-3 hours.
[0012] Preferably, the cationic dye in S3 is any one or more of Basic Brilliant Blue B, Basic Yellow O, Basic Pink T, or Basic Green.
[0013] Preferably, the bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate in S3 to the cationic dye is 1:20~50; The heating reaction in S3 is carried out at a temperature of 60-70°C for 30-90 minutes.
[0014] Preferably, the number of water washing cycles in step S4 is 2 to 4. The soaping temperature in S4 is 50~100℃, and the time is 10~40min; The drying temperature in S4 is 40~80℃, and the drying time is 60~120min.
[0015] Beneficial effects: The present invention has the following advantages: 1. In this invention, serine hydrolase and carboxyl esterase are combined to hydrolyze PLA. The serine hydrolase cleaves the ester bonds in the PLA main chain to directly generate terminal carboxyl groups; the carboxyl esterase hydrolyzes the intermediate oligomer to release lactic acid monomers containing α-carboxyl groups. The two enzymes work together to achieve efficient accumulation of carboxyl groups, so that PLA produces carboxyl groups, which facilitates subsequent grafting. 2. In this invention, ethyl methacrylate is grafted onto the surface of PLA. The phosphate groups (pKa≈1.5~2.5) of ethyl methacrylate ionize into a negative charge in the dyeing environment (acidic environment), significantly improving the affinity for cationic dyes. Furthermore, the phosphate groups weaken the hydrogen bonds between PLA molecular chains, lowering the glass transition temperature of PLA and making it easier for dyes to diffuse into the amorphous region. In addition, the short fatty acid chains (ethyl) of ethyl methacrylate can insert into the PLA molecular chains, reducing local crystallinity and increasing the amorphous region within the fiber, thus acting as a plasticizer. This avoids excessive hydrophobicity caused by long chains, improving the dyeing performance of PLA fabrics. Moreover, no additional dyeing carrier is required, simplifying the dyeing process of PLA fabrics and offering good economic benefits. 3. In this invention, ethyl methacrylate is grafted onto the PLA surface. While improving the dyeing performance, the phosphate ester structure of ethyl methacrylate decomposes at high temperature to produce phosphoric acid, which promotes the dehydration and carbonization of the PLA surface, forming a dense carbon layer that isolates oxygen and inhibits the release of flammable gases, thus giving the bio-based fabric certain flame retardant properties. 4. In this invention, the carboxyl groups produced by the enzymatic hydrolysis of the bio-based fabric and the phosphate groups of ethyl methacrylate have good hydrophilic properties, thus giving the fabric moisture absorption properties; in addition, the presence of the nylon component ensures the strength of the fabric and avoids the loss of fabric strength after PLA hydrolysis. Detailed Implementation
[0016] The present invention will be further described below with reference to embodiments. These embodiments are illustrative of the present invention, but the present invention is not limited to these embodiments: Example 1
[0017] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 2:6 was placed in a compound enzyme solution with a concentration of 1g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase in a mass ratio of 1:1. The pH of the compound enzyme solution was 7.5. After heating at 50℃ for 1h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 10:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:10. After heating and reacting at 60°C for 1 hour, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic brilliant blue B). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:20. After heating and reacting at 60°C for 30 minutes, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed twice with water, soaped at 50℃ for 10 minutes, and finally dried at 40℃ for 60 minutes to obtain dyed nylon / PLA fabric. Example 2
[0018] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 2:8 was placed in a compound enzyme solution with a concentration of 10g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:3. The pH of the compound enzyme solution was 7.0. After heating at 60℃ for 2h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 20:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:30. After heating and reacting at 80°C for 3 hours, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic light yellow O). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate phosphate to the cationic dye is 1:50. After heating and reacting at 70°C for 90 min, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 4 times with water, soaped at 100℃ for 40 minutes, and finally dried at 80℃ for 120 minutes to obtain dyed nylon / PLA fabric. Example 3
[0019] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 3:6 was placed in a compound enzyme solution with a concentration of 5g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:2. The pH of the compound enzyme solution was 7.2. After heating at 55℃ for 1h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 15:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:25. After heating and reacting at 65°C for 1.5 h, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic green). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:35. After heating and reacting at 65°C for 60 min, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 3 times with water, soaped at 60℃ for 30 minutes, and finally dried at 70℃ for 60 minutes to obtain dyed nylon / PLA fabric. Example 4
[0020] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 3:8 was placed in a compound enzyme solution with a concentration of 5g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:2. The pH of the compound enzyme solution was 7.3. After heating at 60℃ for 2h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 12:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:15. After heating and reacting at 65°C for 2 hours, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic light yellow O). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:45. After heating and reacting at 65°C for 60 min, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 3 times with water, soaped at 80℃ for 30 minutes, and finally dried at 60℃ for 80 minutes to obtain dyed nylon / PLA fabric. Example 5
[0021] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 3:7 was placed in a compound enzyme solution with a concentration of 8 g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:2. The pH of the compound enzyme solution was 7.0. After heating at 55℃ for 1.5 h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 15:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:25. After heating and reacting at 75°C for 1.5 h, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic brilliant blue B). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:45. After heating and reacting at 65°C for 45 min, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 4 times with water, soaped at 80℃ for 30 minutes, and finally dried at 50℃ for 120 minutes to obtain dyed nylon / PLA fabric. Example 6
[0022] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 2:8 was placed in a compound enzyme solution with a concentration of 5g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:2. The pH of the compound enzyme solution was 7.5. After heating at 55℃ for 1.5h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 18:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:25. After heating and reacting at 75°C for 2 hours, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic pink). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:35. After heating and reacting at 65°C for 45 min, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 3 times with water, soaped at 80℃ for 30 minutes, and finally dried at 50℃ for 100 minutes to obtain dyed nylon / PLA fabric. Example 7
[0023] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 2:8 was placed in a compound enzyme solution with a concentration of 8g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:3. The pH of the compound enzyme solution was 7.2. After heating at 55℃ for 1.5h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 15:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:25. After heating and reacting at 65°C for 3 hours, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic brilliant blue B). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:45. After heating and reacting at 68°C for 30 minutes, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 3 times with water, soaped at 80℃ for 30 minutes, and finally dried at 50℃ for 100 minutes to obtain dyed nylon / PLA fabric. Example 8
[0024] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 2:7 was placed in a compound enzyme solution with a concentration of 8g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:2. The pH of the compound enzyme solution was 7.0. After heating at 55℃ for 1.5h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 15:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:20. After heating and reacting at 75°C for 2.5 h, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic green). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:40. After heating and reacting at 70°C for 65 minutes, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 3 times with water, soaped at 80℃ for 40 minutes, and finally dried at 60℃ for 100 minutes to obtain dyed nylon / PLA fabric. Example 9
[0025] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 2:6 was placed in a compound enzyme solution with a concentration of 8g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:2. The pH of the compound enzyme solution was 7.5. After heating at 55℃ for 1.5h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 15:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:22. After heating and reacting at 75°C for 2 hours, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic brilliant blue B). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:45. After heating and reacting at 70°C for 60 min, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 3 times with water, soaped at 80℃ for 40 minutes, and finally dried at 65℃ for 100 minutes to obtain dyed nylon / PLA fabric. Example 10
[0026] A dyeing process for bio-based fabrics includes the following steps: S1. Enzymatic hydrolysis treatment: Nylon / PLA fabric with a blend ratio of 2:8 was placed in a compound enzyme solution with a concentration of 8g / L. The compound enzyme solution contained serine hydrolase and carboxyl esterase with a mass ratio of 1:2. The pH of the compound enzyme solution was 7.5. After heating at 55℃ for 1.5h, nylon / PLA fabric containing carboxyl groups was obtained. S2. Surface grafting: The carboxyl-containing nylon / PLA fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate. The mass ratio of ethyl methacrylate to potassium persulfate is 15:1, and the bath ratio of the carboxyl-containing nylon / PLA fabric to the solution containing ethyl methacrylate and potassium persulfate is 1:25. After heating and reacting at 70°C for 2 hours, ethyl methacrylate-grafted nylon / PLA fabric is obtained. S3. Cationic dyeing: The nylon / PLA fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye (basic pink T). The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate to the cationic dye is 1:40. After heating and reacting at 65°C for 65 min, the dyed nylon / PLA fabric is obtained. S4. Post-treatment: The nylon / PLA fabric obtained in S3 is washed 3 times with water, soaped at 80℃ for 40 minutes, and finally dried at 80℃ for 110 minutes to obtain dyed nylon / PLA fabric. Comparative Example 1
[0027] The difference between this comparative example and Example 10 is that the compound enzyme solution contains only serine hydrolase and not carboxyl esterase. Comparative Example 2
[0028] The difference between this comparative example and Example 10 is that the compound enzyme solution contains only carboxyl esterase and not serine hydrolase. Comparative Example 3
[0029] The difference between this comparative example and Example 10 is that the S1 enzyme hydrolysis treatment was not performed. Comparative Example 4
[0030] The difference between this comparative example and Example 10 is that S2 surface grafting was not performed. Comparative Example 5
[0031] The difference between this comparative example and Example 10 is that the S1 enzymatic hydrolysis treatment and S2 surface grafting were not performed; instead, the nylon / PLA fabric was directly immersed in cationic dye (basic pink T) for dyeing.
[0032] Performance testing The dyed nylon / PLA fabrics obtained in Examples 1-10 and Comparative Examples 1-5 of this invention were tested, and the results are shown in the table below.
[0033] Table 1
[0034] Table 2
[0035] Table 3
[0036] Note: 1. The K / S value is an indicator of staining depth, which includes the absorption coefficient K and scattering coefficient S of the object being tested. The larger the K / S value, the higher the staining depth and the better the staining effect. In this test, the K / S value was determined using a Datacolor CS-5 spectrophotometer. 2. Fracture strength testing shall be conducted in accordance with standard GB / T3923.1-2013; 3. Fastness testing was conducted in accordance with standard GB18401-2003 "National Basic Safety Technical Specifications for Textile Products", in which the fastness to sunlight was divided into grades 1 to 8 and the fastness to washing was divided into grades 1 to 5. 4. Moisture permeability shall be tested in accordance with GB / T12704.2.B-2009 "Textiles - Test Method for Moisture Permeability of Fabrics"; 5. The basis weight of the nylon / PLA used in this invention is 100 g / m³. 2 The yarn count is 60s.
[0037] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.
Claims
1. A dyeing process for bio-based fabrics, characterized in that: Includes the following steps: S1. Enzymatic hydrolysis treatment: The bio-based fabric is placed in a compound enzyme solution and heated to obtain a bio-based fabric containing carboxyl groups. S2. Surface grafting: The carboxyl-containing bio-based fabric obtained in S1 is immersed in a solution containing ethyl methacrylate and potassium persulfate, and then heated to obtain ethyl methacrylate-grafted bio-based fabric. S3. Cationic dyeing: The bio-based fabric grafted with ethyl methacrylate phosphate obtained in S2 is immersed in cationic dye and then heated to obtain the dyed bio-based fabric. S4. Post-treatment: The bio-based fabric obtained in S3 is washed with water, soaped and dried to obtain dyed bio-based fabric.
2. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The bio-based fabric is a nylon / PLA fabric with a blending ratio of 2~4:6~8.
3. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The compound enzyme solution in S1 contains serine hydrolase and carboxyl esterase in a mass ratio of 1:1~3. And / or, the concentration of the compound enzyme solution in S1 is 1~10 g / L; And / or, the pH of the compound enzyme solution in S1 is 7.0~7.
5.
4. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The heating treatment in S1 lasts for 1 to 2 hours at a temperature of 50 to 60°C.
5. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The mass ratio of ethyl methacrylate phosphate and potassium persulfate in S2 is 10~20:1; And / or, the bath ratio of the carboxyl-containing bio-based fabric in S2 to the solution containing ethyl methacrylate and potassium persulfate is 1:10~30.
6. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The heating reaction in S2 is carried out at a temperature of 60-80°C for 1-3 hours.
7. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The cationic dye in S3 is any one or more of Basic Brilliant Blue B, Basic Yellow O, Basic Pink T, or Basic Green.
8. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The bath ratio of the nylon / PLA fabric grafted with ethyl methacrylate phosphate in S3 to the cationic dye is 1:20~50. And / or, the heating reaction in S3 is carried out at a temperature of 60~70℃ for a time of 30~90min.
9. The dyeing process for a bio-based fabric according to claim 1, characterized in that: The number of water washes in S4 is 2 to 4; And / or, the temperature of the soaping in S4 is 50~100℃ and the time is 10~40min; And / or, the drying temperature in S4 is 40~80℃ and the time is 60~120min.