A full-ecological processing and manufacturing method of functional silk fabric

Abstract

The present application belongs to the field of high-end textile processing and manufacturing, and particularly relates to a full-ecological processing and manufacturing method of functional silk fabric. Curcumin compounds are prepared into a dyeing solution, the silk fabric is immersed in the obtained dyeing solution, the dyeing solution is heated, when the temperature is raised to 65 DEG C to 75 DEG C, luteolin is dispersed in the dyeing solution according to the mass ratio of 3 to 4:1 of luteolin to curcumin compounds, the temperature is raised to 85 DEG C to 95 DEG C and then kept for a period of time, then the silk fabric is taken out from the dyeing solution, washed and dried. The silk fabric dyed by the present application has excellent and durable antioxidant activity and ultraviolet protection performance, and after repeated soaping, it can still reach more than 95% and more than 200 respectively. The problem of non-durable function caused by poor soaping fastness of natural dyeing is solved, and the full-process ecological and environmental protection processing avoids the pollution problem caused by the use of chemical dyes and metal mordant, and has good application prospect.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of high-end textile processing and manufacturing, and particularly relates to a full-ecological processing and manufacturing method of functional silk fabric. BACKGROUND

[0002] Silk is a high-grade fabric, which is soft and light in hand feeling, contains 18 kinds of amino acids required by human body, and is very similar to the amino acids contained in human skin, and is also called the second skin of human, and is highly respected by people. However, the antioxidant activity of silk fiber itself is poor; and after the aromatic amino acids in the silk fiber are irradiated, photo-oxidation causes photo-yellowing, in addition, light can also cause oxidative cleavage of polypeptide chains in the silk fiber, causing photo brittle damage, so that the ultraviolet resistance of the silk fiber is poor. Dyeing the silk fabric with natural dyes such as Chinese herbal medicines is a method of simultaneously imparting color and functionality to the silk fabric, but the silk fabric dyed with natural dyes lacks durability due to poor color fastness.

[0003] At present, the methods for increasing the color fastness of natural dyeing and improving the functional preservation rate mainly focus on mordanting, among which, the use of Fe 3+ , Al 3+ , biomass mordant chitosan and the like for mordanting is reported more frequently. However, in order to reduce the threat of metal mordant to the environment and human health, and to improve the use efficiency of biomass mordant, simplify the process flow, explore new natural biomass mordant and simple and sustainable mordanting method, and impart the silk fabric with durable antioxidant and ultraviolet protection performance, it is also imperative. SUMMARY

[0004] To solve the above technical problems, the present application provides a full-ecological processing and manufacturing method of functional silk fabric:

[0005] First, curcumin compounds are prepared into a dyeing solution, the silk fabric is immersed in the obtained dyeing solution, the dyeing solution is heated, and when the temperature is raised to 65-75 DEG C, luteolin is dispersed in the dyeing solution according to a mass ratio of 3-4:1 of curcumin compounds, the temperature is raised to 85-95 DEG C, and then the temperature is maintained for a period of time, and then the silk fabric is taken out of the dyeing solution, washed and dried.

[0006] As preferred: the extraction and preparation method of curcumin compounds is that curcumin powder is added into a mixed extraction solvent of ethanol and water for heating ultrasonic extraction, the filter cake obtained after extraction is hot-filtrated, the filter cake is added into the mixed extraction solvent again for heating ultrasonic extraction, and then hot-filtrated, the filtrate obtained by two times of hot-filtration is collected, the supernatant is collected after high-speed centrifugal treatment, and the curcumin compound powder is obtained by rotary evaporation drying.

[0007] Further, the volume ratio of ethanol and water in the mixed extraction solvent is 7:3.

[0008] Further, the mass ratio of material to liquid is 1:10 in the first heating ultrasonic extraction, and the mass ratio of material to liquid is 1:8 in the second heating ultrasonic extraction; the extraction time is 30-50 min in each time; the extraction temperature is 40-70 DEG C in each time; the ultrasonic power is 300 W in each time; and the ultrasonic frequency is 25-40 KHz in each time.

[0009] Further, the rotating speed of high-speed centrifugation is 5000-8000 rpm.

[0010] Further, the rotary evaporation is carried out under negative pressure, the evaporation temperature is 38 DEG C, and the rotating speed is 110 rpm.

[0011] Preferably, the dyeing solution is prepared by dissolving curcumin compounds in a mixed solvent of ethanol and water with a volume ratio of 1:1.

[0012] Preferably, the pH of the dyeing solution is adjusted to 3.0-5.0 by using citric acid before the silk fabric is immersed in the dyeing solution.

[0013] Preferably, the silk fabric is immersed in the dyeing solution with a bath ratio of 1:50.

[0014] Preferably, the heating rate is 2 DEG C / min.

[0015] Preferably, the holding time is 60 min.

[0016] The present application has the following beneficial effects:

[0017] When the natural yellow pigment curcumin compounds and luteolin are used together to dye the silk fabric, the luteolin plays the role of a mordant. The main action is that the curcumin compounds mainly exist in the form of diketones under acidic conditions, the carbonyl in the structure can form a ketal with the ortho-hydroxyl on the B ring in the structure of luteolin, and the meta-phenolic hydroxyl on the A ring in the structure of luteolin can become a hydrogen donor and combine with the carbonyl in the structure of curcumin compounds by intermolecular hydrogen bonding, and then the ketone carbonyl on the C ring in the structure of luteolin acts as a hydrogen acceptor and accepts hydrogen from the -NH2 on the silk fiber. The complex formed in this way increases the number of hydrogen bond donors and acceptors, thereby more stably combining with the amino groups and amide carbonyl groups on the amino acid residues in the structure of the silk fiber by intermolecular hydrogen bonding or ionic bonding. The process of mordanting provides favorable physical conditions for this combination, improves the binding fastness of the natural dye complex to the silk fiber, and improves the antioxidant performance and ultraviolet protection performance of the silk fabric dyed by curcumin compounds.

[0018]

[0019] When R1=R2=OCH3, it is curcumin; when R1=H, R2=OCH3, it is demethoxycurcumin; and when R1=R2=H, it is bisdemethoxycurcumin. At present, curcumin compounds obtained directly through extraction (such as the extraction operation in the present application) are generally considered to be a mixture mainly containing the above three compound components (curcumin, demethoxycurcumin, and bisdemethoxycurcumin);

[0020]

[0021] The mordanting process is simple, time-saving, cost-saving, and green and environmentally friendly, and the components used are all natural biomass materials, avoiding pollution and harm caused by synthetic dyes and metal mordants, and meeting the requirements of green and ecological textile processing. In addition, the silk fabric obtained has persistent antioxidant activity and ultraviolet protection performance, plays a protective role on the human body, and provides a new idea for the preparation of biomedical textiles. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 A time-temperature coordinate process flow chart of the natural dye mordanting method of the silk fabric of the present application;

[0023] Figure 2 An antioxidant performance comparison chart between the silk fabric directly dyed with curcumin compounds in Example 2, the silk fabric directly dyed with NY-722 acid synthetic dyes in Comparative Example 3, and the blank silk fabric without dyeing treatment;

[0024] Figure 3 An ultraviolet protection performance comparison chart between the silk fabric directly dyed with curcumin compounds in Example 2, the silk fabric directly dyed with NY-722 acid synthetic dyes in Comparative Example 3, and the blank silk fabric without dyeing treatment;

[0025] Figure 4 An antioxidant performance comparison chart between the silk fabric directly dyed with curcumin compounds in Example 2, the silk fabric dyed with curcumin compounds and then mordant-treated with chitosan in Comparative Example 2, and the silk fabric dyed with curcumin compounds and then mordant-treated with luteolin in Example 3;

[0026] Figure 5 An ultraviolet protection performance comparison chart between the silk fabric directly dyed with curcumin compounds in Example 2, the silk fabric dyed with curcumin compounds and then mordant-treated with chitosan in Comparative Example 2, and the silk fabric dyed with curcumin compounds and then mordant-treated with luteolin in Example 3;

[0027] Figure 6A comparison chart of the ability to maintain the antioxidant performance of the silk fabric of Example 2 directly dyed with the curcumin compound, the silk fabric of Example 1 dyed with the curcumin compound and treated with the same medium of luteolin (the columnar chart group for representing the same kind of silk fabric has three columns from left to right representing "0 times", "1 time", and "5 times", respectively);

[0028] Figure 7 A comparison chart of the ability to maintain the ultraviolet protection performance of the silk fabric of Example 2 directly dyed with the curcumin compound, the silk fabric of Example 1 dyed with the curcumin compound and treated with the same medium of luteolin (the columnar chart group for representing the same kind of silk fabric has three columns from left to right representing "0 times", "1 time", and "5 times", respectively);

[0029] Figure 8 A color schematic diagram of the silk fabric of Example 1 dyed with the curcumin compound and treated with the same medium of luteolin.

[0030] Figure 9 A color schematic diagram of the silk fabric of Example 4 directly treated with luteolin. DETAILED DESCRIPTION

[0031] (1) Preparation of the curcumin compound:

[0032] The curcumin powder was added to the mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating ultrasonic extraction, the solid-liquid mass ratio was 1:10, the extraction temperature was 40-70℃, the ultrasonic power was 300w, the ultrasonic frequency was 25-40KHz, the extraction time was 30-50min, and after extraction, hot suction filtration was performed,

[0033] The obtained filter cake was again added to the mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating ultrasonic extraction, the solid-liquid mass ratio was 1:8, the extraction temperature was 40-70℃, the ultrasonic power was 300w, the ultrasonic frequency was 25-40KHz, the extraction time was 30-50min, and after extraction, hot suction filtration was performed,

[0034] The filtrates obtained by two times of suction filtration were collected, and after high-speed centrifugation at 5000-8000rpm, the supernatant was collected, and the curcumin compound powder was obtained by rotary evaporation drying at 38℃ under negative pressure at 110rpm;

[0035] (2) Natural dye mordanting of silk fabric:

[0036] The curcumin compound is dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution, the pH of the dyeing solution is adjusted to 3.0-5.0 with citric acid, and then the silk fabric is immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution is heated at a rate of 2 ℃ / min based on an initial temperature of 30 ℃, and when the temperature is raised to 65-75 ℃, luteolin is dispersed in the dyeing solution at a mass ratio of 3-4:1 with respect to the curcumin compound. After being heated to 85-95 ℃ and kept for 60 min, the temperature is naturally cooled to room temperature (25 ℃). The silk fabric is taken out of the dyeing solution, washed with tap water, and dried.

[0037] Example 1

[0038] (1) Preparation of curcumin compound:

[0039] Curcuma powder (obtained by crushing and sieving curcuma roots with a pulverizer) is added to a mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating ultrasonic extraction, with a material-liquid mass ratio of 1:10, an extraction temperature of 60 ℃, an ultrasonic power of 300 w, an ultrasonic frequency of 30 KHz, and an extraction time of 40 min. After extraction, hot suction filtration is performed,

[0040] The obtained filter cake is again added to a mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating ultrasonic extraction, with a material-liquid mass ratio of 1:8, an extraction temperature of 70 ℃, an ultrasonic power of 300 w, an ultrasonic frequency of 30 KHz, and an extraction time of 30 min. After extraction, hot suction filtration is performed,

[0041] The filtrates obtained by two times of suction filtration are collected, and the supernatant is collected after high-speed centrifugation at 6000 rpm. The supernatant is dried by rotary evaporation at 38 ℃ and 110 rpm under negative pressure to obtain a curcumin compound powder;

[0042] (2) Natural dye mordanting of silk fabric:

[0043] The curcumin compound prepared in step (1) is dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution, the pH of the dyeing solution is adjusted to 3.0 with citric acid, and then the silk fabric is immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution is heated at a rate of 2 ℃ / min based on an initial temperature of 30 ℃, and when the temperature is raised to 70 ℃, luteolin is dispersed in the dyeing solution at a dosage of 2 g / L. After being heated to 90 ℃ and kept for 60 min, the temperature is naturally cooled to room temperature. The silk fabric is taken out of the dyeing solution, washed with tap water, and dried to obtain a yellow silk fabric (luteolin mordanted dyed silk fabric, LMF).

[0044] The antioxidant and UV protection properties of the mordanted silk fabric in this embodiment, as well as the durability of these properties after soaping, were tested and evaluated.

[0045] Among them, the antioxidant properties are achieved through the use of silk fabrics to protect ABTS. ·+ The removal rate is used to determine the result: 10 mg of silk fabric is immersed in 10 mL of ABTS. ·+ In the solution, its absorbance was measured after 30 minutes, and the result was calculated using the formula 100% × (A). control -A sample ) / A control Calculate, where A control It is ABTS ·+ The initial absorbance of the solution, A sample ABTS is applied after immersing the silk fabric for 30 minutes. ·+ The absorbance of the solution;

[0046] The UV protection factor (UPF) was obtained by testing with a YG(B)912E textile UV protection performance tester (Wenzhou Darong Textile Instrument Co., Ltd.). Each sample was tested five times and the average value was taken.

[0047] The soaping procedure is as follows: Immerse the silk fabric in a soap solution containing 5g / L of standard soap powder at a bath ratio of 1:50, soap at 40℃ for 30 minutes, then remove the silk fabric, rinse thoroughly with tap water, and air dry. After five rounds of soaping using this procedure, repeat the above steps to test the anti-oxidation and UV protection properties of the silk fabric.

[0048] The test results showed that the mordanted silk fabric in this embodiment achieved an antioxidant activity of 97.31% and an ultraviolet protection factor (UVP) of 242.97 before soaping. After one round of soaping, the antioxidant activity and UV protection factor were 96.48% and 233.10, respectively. Furthermore, after five rounds of soaping, the antioxidant activity and UV protection factor remained at 96.08% and 215.82, respectively. In contrast, the untreated blank silk fabric had antioxidant properties and a UV protection factor of only 12.62% and 7.92, respectively. This indicates that the above treatment method resulted in excellent and durable antioxidant and UV protection properties for the silk fabric.

[0049] Example 2

[0050] The difference from Example 1 is that curcumin-based compounds were used for direct staining, and luteolin was not introduced (the decrease in treatment agent dosage due to the lack of luteolin was compensated for by an equal mass of curcumin-based compounds). All other operations were the same as in Example 1.

[0051] (1) Same as step (1) in Example 1;

[0052] (2) Dyeing of silk fabric:

[0053] The curcumin compound prepared in step (1) was dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution at a dosage of 13% owf. After adjusting the pH of the dyeing solution to 3.0 with citric acid, the silk fabric was immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution was heated at a rate of 2°C / min based on an initial temperature of 30°C, and then kept at 90°C for 60 min. After natural cooling to room temperature, the silk fabric was taken out of the dyeing solution, washed with tap water, and then dried to obtain a yellow silk fabric (crude curcumin dyed silk fabric, CSF).

[0054] The antioxidant and ultraviolet protection properties of the silk fabric dyed with the curcumin compound in this example were detected and evaluated, and the specific detection operation was consistent with that in Example 1. The detection results showed that the antioxidant activity of the silk fabric dyed with the curcumin compound in this example (without soaping) was 70.57%, and the ultraviolet protection factor was 139.92. After one round of soaping, the antioxidant activity and the ultraviolet protection factor were 53.16% and 135.21, respectively. After five rounds of soaping, the antioxidant activity and the ultraviolet protection factor were 47.78% and 124.65, respectively.

[0055] Example 3

[0056] The difference compared with Example 1 is that luteolin is used for post-mordanting. The rest of the operations are the same as those in Example 1.

[0057] (1) The same as step (1) in Example 1;

[0058] (2) Dyeing of silk fabric:

[0059] The curcumin compound prepared in step (1) was dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution at a dosage of 13% owf. After adjusting the pH of the dyeing solution to 3.0 with citric acid, the silk fabric was immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution was heated at a rate of 2°C / min based on an initial temperature of 30°C, and then kept at 90°C for 60 min. After natural cooling to room temperature, the silk fabric was taken out of the dyeing solution, washed with tap water, and then dried to obtain a yellow silk fabric (crude curcumin dyed silk fabric, CSF).

[0060] (3) Post-mordanting

[0061] The silk fabric obtained in step (2) is immersed in a mixed solvent of ethanol and water with a volume ratio of 1:1 at a bath ratio of 1:50, the mixed solvent is heated at a rate of 2°C / min based on the initial temperature of 30°C, and when the temperature is raised to 70°C, luteolin is dispersed in the mixed solvent at a dosage of 2 g / L, and after heating to 90°C, it is kept for 60 min, and then naturally cooled to room temperature. After the silk fabric is taken out of the mixed solvent, it is washed thoroughly with tap water and dried, and a yellow silk fabric is obtained.

[0062] The antioxidant and ultraviolet protection properties of the silk fabric treated by the post-mordanting method in this example are detected and evaluated, and the specific detection operation is consistent with that in Example 1. The detection results show that the antioxidant activity of the silk fabric treated by the post-mordanting method in this example (without soaping) is only 55.26%, and the ultraviolet protection factor is 114.57.

[0063] Comparing Example 2 and Example 3, it can be seen that in Example 2, after direct dyeing with curcumin compounds, the fabric is endowed with certain antioxidant and ultraviolet protection effects, and in Example 3, the antioxidant and ultraviolet protection effects are greatly reduced after further post-mordanting with luteolin based on Example 2. Therefore, the applicant believes that luteolin and curcumin compounds have a competitive binding relationship on silk fabric, and the binding ability of luteolin to silk fabric is stronger than that of curcumin. Therefore, the luteolin added in Example 3 "competes" with the curcumin that is directly combined on the silk fabric, and the curcumin that is "competed" down is not easy to recombine with luteolin or silk fabric, resulting in a decrease in the total amount of curcumin on the fabric and a decrease in efficacy.

[0064] In Example 1, most of the curcumin compounds are first combined with luteolin to form a complex, and then dyed on the silk fabric, so the above-mentioned "competed" down situation is not easy to occur.

[0065] Example 4

[0066] Only luteolin is used to treat the fabric, and curcumin compounds are not used for dyeing (the decrease in the amount of treatment agent caused by the absence of curcumin compounds is supplemented by an equal amount of luteolin), and the rest of the operations are the same as in Example 1.

[0067] Treatment of silk fabric with luteolin:

[0068] After adjusting the pH of the mixed solvent with a volume ratio of ethanol and water of 1:1 to 3.0 with citric acid, the silk fabric was immersed in the obtained mixed solvent at a bath ratio of 1:50, the temperature of the mixed solvent was increased at a rate of 2℃ / min based on the initial temperature of 30℃, and when the temperature was increased to 70℃, luteolin was dispersed in the mixed solvent at a dosage of 2.6g / L, the temperature was increased to 90℃ and then kept for 60min, and then naturally cooled to room temperature. After the silk fabric was taken out of the mixed solvent, it was washed thoroughly with tap water and then dried in the air to obtain a light yellow silk fabric.

[0069] The antioxidant and ultraviolet protection properties of the silk fabric treated with luteolin in this example were detected and evaluated, and the specific detection operation was consistent with that in Example 1. The detection results showed that the antioxidant activity of the silk fabric treated with luteolin in this example (without soaping) was 53.45%, and the ultraviolet protection factor was 75.58.

[0070] As can be seen from Example 4, after the silk fabric was treated with luteolin alone, the fabric was endowed with certain antioxidant and ultraviolet protection properties, but the effects were very limited, and were significantly lower than the antioxidant and ultraviolet protection properties exhibited when the silk fabric was treated with curcumin compounds alone in Example 2. At this time, if only the general rule is followed: when luteolin and curcumin compounds are used together, if they are simply mixed and dyed, the protection effect that can be achieved should only be between Example 4 and Example 2 (the total amount of treatment agent is the same), far from the detection effect of Example 1. Thus, from another angle, it is proved that in Example 1 representing the present scheme, luteolin and curcumin compounds do not simply mix in the silk dyeing process, but work synergistically: after the combination of the two, more number of hydrogen bond donors and acceptors are formed on curcumin compounds, so that curcumin compounds can be combined on silk fibers in a larger amount and more stably, significantly improving the dyeing rate and greatly improving the antioxidant and ultraviolet protection properties of the silk fabric.

[0071] Example 5

[0072] Compared with Example 1, the difference is that luteolin is added at the beginning of the dyeing operation. The rest of the operations are the same as those in Example 1.

[0073] (1) The same as step (1) of Example 1;

[0074] (2) Natural dye mordanting of the silk fabric:

[0075] The curcumin compound prepared in step (1) is dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution, and the pH of the dyeing solution is adjusted to 3.0 with citric acid. Then, luteolin is dispersed in the dyeing solution at a dosage of 2 g / L, and silk fabric is immersed in the obtained dyeing solution at a bath ratio of 1:50. The temperature of the dyeing solution is increased at a rate of 2 ℃ / min based on an initial temperature of 30 ℃, and then the temperature is maintained at 90 ℃ for 60 min. Then, the temperature is naturally cooled to room temperature. After the silk fabric is taken out of the dyeing solution, it is washed with tap water and dried to obtain a yellow silk fabric.

[0076] The antioxidant activity and ultraviolet protection performance of the silk fabric treated by the same bath mordanting process in this example are detected and evaluated, and the specific detection operation is consistent with that in Example 1. The detection results show that the antioxidant activity of the silk fabric treated by the same bath mordanting process in this example (without soaping) is 81.42%, and the ultraviolet protection coefficient is 195.06. After one round of soaping, the antioxidant activity and ultraviolet protection performance are 77.06% and 186.95, respectively. After five rounds of the above soaping, the antioxidant activity and ultraviolet protection coefficient are 70.32% and 173.57, respectively.

[0077] As can be seen from Example 5, if luteolin and curcumin compounds are used together to dye the silk fabric at the beginning, the dyeing effect is not negligible compared with Example 1. The applicant believes that in Example 1 representing the present scheme, luteolin is added at 70 ℃. Compared with regular temperature increase, luteolin is more likely to combine with curcumin compounds under sudden heating. Therefore, the influence of luteolin on the dyeing of curcumin compounds in Example 1 is more obvious, resulting in a higher dyeing degree.

[0078] Example 6

[0079] The operation parameters for preparing the curcumin compound by extraction in step (1) are changed, and the remaining operations are the same as in Example 1.

[0080] (1) Preparation of curcumin compound by extraction:

[0081] The turmeric powder is added to a mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating and ultrasonic extraction, and the solid-liquid mass ratio is 1:10, the extraction temperature is 70 ℃, the ultrasonic power is 300 w, the ultrasonic frequency is 40 KHz, and the extraction time is 30 min. After extraction, the hot filtrate is extracted,

[0082] The obtained filter cake is again added to a mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating and ultrasonic extraction, and the solid-liquid mass ratio is 1:8, the extraction temperature is 70 ℃, the ultrasonic power is 300 w, the ultrasonic frequency is 40 KHz, and the extraction time is 30 min. After extraction, the hot filtrate is extracted,

[0083] The filtrate obtained by collecting the filtrate twice was treated by high-speed centrifugation at 5000 rpm, and the supernatant was collected and dried by rotary evaporation at 38°C under negative pressure at 110 rpm to obtain a curcumin compound powder;

[0084] (2) Natural dye mordanting of silk fabric:

[0085] The curcumin compound prepared in step (1) was dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution at a dosage of 3% owf. After adjusting the pH of the dyeing solution to 3.0 with citric acid, the silk fabric was immersed in the obtained dyeing solution at a bath ratio of 1:50. The temperature of the dyeing solution was increased at a rate of 2°C / min based on an initial temperature of 30°C, and at 70°C, luteolin was dispersed in the dyeing solution at a dosage of 2 g / L. After heating to 90°C and maintaining for 60 min, the temperature was naturally cooled to room temperature. The silk fabric was taken out of the dyeing solution, washed thoroughly with tap water, and dried to obtain a yellow silk fabric.

[0086] The antioxidant and ultraviolet protection properties of the silk fabric treated by the same bath mordanting in this example were detected and evaluated, and the specific detection operation was consistent with that in Example 1. The detection results showed that the antioxidant activity of the silk fabric before soaping after mordanting in this example reached 95.84%, and the ultraviolet protection factor reached 246.17. After one round of soaping, the antioxidant activity and ultraviolet protection properties were 94.86% and 232.58, respectively. After five rounds of the above soaping, the antioxidant activity and ultraviolet protection factor could still reach 94.22% and 219.61, respectively.

[0087] Example 7

[0088] The operation parameters for preparing the curcumin compound were changed in step (1), and the remaining operations were the same as in Example 1.

[0089] (1) Preparation of curcumin compound:

[0090] The curcumin powder was added to a mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating ultrasonic extraction, with a solid-liquid mass ratio of 1:10, an extraction temperature of 40°C, an ultrasonic power of 300w, an ultrasonic frequency of 25KHz, and an extraction time of 50 min. After extraction, the hot filtrate was filtered,

[0091] The obtained filter cake was again added to a mixed extraction solvent of ethanol and water in a volume ratio of 7:3 for heating ultrasonic extraction, with a solid-liquid mass ratio of 1:8, an extraction temperature of 40°C, an ultrasonic power of 300w, an ultrasonic frequency of 25KHz, and an extraction time of 50 min. After extraction, the hot filtrate was filtered,

[0092] The filtrate obtained by collecting and twice filtering was treated by high-speed centrifugation at 8000 rpm, and the supernatant was collected and dried by rotary evaporation at 38°C under negative pressure at 110 rpm to obtain a powder of curcumin compounds;

[0093] (2) Natural dye mordanting of silk fabric:

[0094] The curcumin compound prepared in step (1) was dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution at a dosage of 3% owf. After adjusting the pH of the dyeing solution to 3.0 with citric acid, the silk fabric was immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution was heated at a rate of 2°C / min based on an initial temperature of 30°C, and at 70°C, luteolin was dispersed in the dyeing solution at a dosage of 2 g / L. After heating to 90°C, the temperature was maintained for 60 min, and then the temperature was naturally cooled to room temperature. The silk fabric was taken out of the dyeing solution, washed with tap water, and dried to obtain a yellow silk fabric.

[0095] The antioxidant and ultraviolet protection properties of the silk fabric treated by the same bath mordanting in this example were detected and evaluated, and the specific detection operation was consistent with that in Example 1. The detection results showed that the antioxidant activity of the silk fabric before soaping after mordanting in this example reached 96.05%, and the ultraviolet protection factor reached 235.62. After one round of soaping, the antioxidant activity and ultraviolet protection properties were 95.27% and 221.89, respectively. After five rounds of the above soaping, the antioxidant activity and ultraviolet protection factor could still reach 94.56% and 210.24, respectively.

[0096] The same silk fabric was treated by dyeing using some other types of mordants or dyes in the art, and the dyeing effect was compared with that of Example 1 representing the present scheme:

[0097] Comparative Example 1

[0098] The difference compared with Example 1 is that the common biomass mordant chitosan is used for the same mordanting treatment:

[0099] (1) The same as step (1) of Example 1;

[0100] (2) Natural dye mordanting of silk fabric:

[0101] The curcumin compound prepared in step (1) was dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution at a dosage of 3% owf. After adjusting the pH of the dyeing solution to 3.0 with citric acid, the silk fabric was immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution was heated at a rate of 2°C / min based on an initial temperature of 30°C, and when the temperature reached 70°C, chitosan was dispersed in the dyeing solution at a dosage of 2 g / L. After heating to 90°C and maintaining for 60 min, the temperature was naturally cooled to room temperature. The silk fabric was taken out of the dyeing solution, rinsed thoroughly with tap water, and dried to obtain a yellow silk fabric (chitosan mordanted dyed silk fabric, CMF).

[0102] The antioxidant and ultraviolet protection properties of the silk fabric mordanted with chitosan in this comparative example were detected and evaluated, and the specific detection operation was consistent with that in Example 1. The detection results showed that the antioxidant activity of the silk fabric (without soaping) after mordanting with chitosan in this example was 72.86%, and the ultraviolet protection factor was 153.88.

[0103] In this comparative example, compared with direct treatment with curcumin compounds, the protection effect of the silk fabric after mordanting with chitosan mordanting curcumin compounds was limitedly improved.

[0104] Comparative Example 2

[0105] The difference compared with Example 1 is that a common biomass mordant chitosan is used for post-mordanting treatment:

[0106] (1) The same as step (1) of Example 1;

[0107] (2) Dyeing of silk fabric:

[0108] The curcumin compound prepared in step (1) was dissolved in a mixed solvent of ethanol and water in a volume ratio of 1:1 to prepare a dyeing solution at a dosage of 3% owf. After adjusting the pH of the dyeing solution to 3.0 with citric acid, the silk fabric was immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution was heated at a rate of 2°C / min based on an initial temperature of 30°C, and when the temperature reached 70°C, chitosan was dispersed in the dyeing solution at a dosage of 2 g / L. After heating to 90°C and maintaining for 60 min, the temperature was naturally cooled to room temperature. The silk fabric was taken out of the dyeing solution, rinsed thoroughly with tap water, and dried to obtain a yellow silk fabric (chitosan mordanted dyed silk fabric, CMF).

[0109] (3) Post-mordanting treatment

[0110] The silk fabric obtained in step (2) was immersed in a mixed solvent of ethanol and water with a volume ratio of 1:1 at a bath ratio of 1:50. The mixed solvent was heated at a rate of 2°C / min based on an initial temperature of 30°C, and when the temperature was raised to 70°C, chitosan was dispersed in the mixed solvent at a dosage of 2 g / L. After heating to 90°C, the temperature was maintained for 60 min, and then the temperature was naturally cooled to room temperature. The silk fabric was taken out of the mixed solvent, rinsed thoroughly with tap water, and then air-dried.

[0111] The antioxidant activity and UV protection performance of the silk fabric after the post-mordanting treatment of the present comparative example were detected and evaluated respectively, and the specific detection operation was consistent with that in Example 1. The detection results showed that the antioxidant activity of the silk fabric after the post-mordanting treatment of the present example (without soaping) was only 16.25%, and the UV protection factor was 42.48.

[0112] Comparative Example 3

[0113] The difference compared with Example 1 is that NY-722 acid synthetic yellow dye (Jiangsu Dewang Chemical Industry Co., Ltd.) is used instead of natural extract dye for direct dyeing, and no mordant is introduced (the decrease in the amount of treatment agent caused by the absence of mordant is compensated by the same amount of NY-722):

[0114] Dyeing of silk fabric:

[0115] NY-722 was dissolved in a mixed solvent of ethanol and water with a volume ratio of 1:1 at a dosage of 13% owf to prepare a dyeing solution. After adjusting the pH of the dyeing solution to 3.0 with citric acid, the silk fabric was immersed in the obtained dyeing solution at a bath ratio of 1:50. The dyeing solution was heated at a rate of 2°C / min based on an initial temperature of 30°C, and after heating to 90°C, the temperature was maintained for 60 min, and then the temperature was naturally cooled to room temperature. The silk fabric was taken out of the dyeing solution, rinsed thoroughly with tap water, and then air-dried to obtain a yellow silk fabric (NY-722 dyed silk fabric, NSF).

[0116] The antioxidant activity and UV protection performance of the silk fabric after the dyeing of the present comparative example were detected and evaluated respectively, and the specific detection operation was consistent with that in Example 1. The detection results showed that the antioxidant activity of the directly dyed silk fabric of the present example (without soaping) was only 25.28%, and the UV protection factor was 63.04.

Claims

1. A fully eco-friendly processing and manufacturing method for functional silk fabrics, characterized in that: The method is as follows: First, a dye solution containing curcumin compounds is prepared. Before immersing the silk fabric in the dye solution, the pH of the dye solution is adjusted to 3.0–5.0 with citric acid. After immersing the silk fabric in the dye solution, the dye solution is heated. When the temperature reaches 65°C–75°C, luteolin is dispersed in the dye solution at a mass ratio of 3–4:1 to the curcumin compounds. The temperature is then raised to 85°C–95°C and maintained for 60 minutes. After cooling, the silk fabric is removed from the dye solution, washed, and dried. The extraction and preparation method of the curcumin compounds is as follows: Curcumin powder is added to a mixed extraction solvent of ethanol and water for heated ultrasonic extraction. After extraction, the mixture is filtered while hot. The resulting filter cake is added to the mixed extraction solvent again for heated ultrasonic extraction and filtered while hot. The filtrates obtained from the two filtrations are collected. After high-speed centrifugation, the supernatant is collected and dried by rotary evaporation to obtain the curcumin compound powder.

2. The all-ecological processing and manufacturing method of functional silk fabrics as described in claim 1, characterized in that: In the mixed extraction solvent, the volume ratio of ethanol to water is 7:

3.

3. The all-ecological processing and manufacturing method of functional silk fabrics as described in claim 1, characterized in that: The material-to-liquid mass ratio for the first ultrasonic extraction was 1:10, and the material-to-liquid mass ratio for the second ultrasonic extraction was 1:

8. The extraction time for each extraction was 30–50 min, the extraction temperature was 40–70 °C, the ultrasonic power was 300 W, and the ultrasonic frequency was 25–40 kHz.

4. The all-ecological processing and manufacturing method of functional silk fabrics as described in claim 1, characterized in that: The dye solution is prepared by dissolving curcumin-like compounds in a mixed solvent of ethanol and water in a volume ratio of 1:

1.

5. The all-eco-friendly processing and manufacturing method of functional silk fabrics as described in claim 1, characterized in that: The silk fabric is immersed in the dye solution at a bath ratio of 1:

50.

6. The all-eco-friendly processing and manufacturing method of functional silk fabrics as described in claim 1, characterized in that: The heating rate is 2℃ / min.

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