Preparation method and application of berry tea functional dye

Abstract

The invention relates to a berry tea functional dye and a preparation method and application thereof. The functional dye is obtained by extracting berry tea as a raw material. The functional dye comprises the following components by mass percentage: a flavonoid component, a flavanol component, a flavonol component, a dihydroflavone component and a polyphenol component. The preparation method comprises the following steps: old berry tea leaves→alcohol extraction→solid-liquid separation→concentration→extraction→washing→drying to obtain a solid berry tea functional dye. Then, under suitable mordanting conditions, the berry tea dye is used for dyeing natural fibers, which not only gives the fabric a bright and beautiful color, but also gives the fabric a certain antibacterial function. The invention uses old berry tea leaves to prepare the functional dye, thereby improving the utilization rate of biological resources, and combines extraction technology to enrich the antibacterial functional components of berry tea pigments, which are used for creating fiber functional materials, and has important theoretical significance and practical value.

Description

Technical Field

[0001] The invention relates to the technical field of plant extraction and hydrogenation dyes and printing and dyeing, and more specifically, to a preparation method and application of a berry tea functional dye. Background Art

[0002] Berry tea, scientifically known as Ampelopsis grossedentata, is a deciduous vine of the genus Ampelopsis in the family Vitaceae. It is also known as vine tea, fairy grass, longevity vine, Tujia nectar, etc. It is mainly distributed in Hunan, Hubei, Yunnan, Guizhou and other places. The native plant grows in red sandstone at an altitude of 400-1300m. It is a unique tea plant with unique active ingredients and high application value in my country. It has the characteristics of wide geographical distribution, large biological yield and high economic benefits. After years of scientific research on collection and processing, bionic cultivation, pharmacology and nutrition, it has laid a relatively solid foundation for the development of the tea industry. It has now become an important industry for poverty alleviation and rural revitalization in rural areas.

[0003] It is reported that berry tea contains a natural plant cream, the main active ingredient of which is flavonoids, with an average total flavonoid content of more than 6%. It is the plant with the highest flavonoid content among all the plants discovered so far, and is called the "king of flavonoids" (Zhang Tiantian et al., 2018). Berry tea mainly contains a variety of chemical components such as volatile oils, flavonoids, polysaccharides, etc., which have anti-inflammatory, antitussive, expectorant, analgesic, antioxidant, lipid-lowering, blood sugar-lowering, anti-hypertensive, and immune-enhancing effects (Wang Huan et al., 2005). However, the current berry tea production can only utilize some young stems and leaves. The large amount of branches, leaves and old leaves produced by pruning and shaping every year can only be left to rot naturally as waste, which significantly reduces the comprehensive utilization value of berry tea resources.

[0004] Natural dyes come from nature, belong to nature, and have good biodegradability. Previous studies have shown that natural dyes can not only dye unique and soft colors, but also give fabrics added value, such as giving dyed fabrics a unique fragrance, and obtaining mosquito repellent, antibacterial, anti-ultraviolet and other functions. Applying natural dyes to dye natural fiber fabrics can make the fabrics eco-friendly and green and healthy with natural dyes from nature, and can achieve the full naturalization of cotton and linen fabrics, which is in line with modern people's pursuit of ecological green. Wang Qiong et al. reported that berry tea leaves are the raw materials of plant natural dyes, but did not mention the functionality of their dyes and dyed products. Therefore, it is of great significance to efficiently extract flavonoid berry tea natural dyes, systematically study their dyeing and antibacterial properties on natural fiber fabrics, and develop fiber functional materials. Summary of the invention

[0005] Based on the above technical problems existing in the prior art, the present invention provides a method for preparing a berry tea functional dye. The functional dye extracted from berry tea as raw material can be applied to natural fiber printing and dyeing, so that the obtained natural fiber has a better antibacterial effect.

[0006] In order to achieve the above object, the technical solution of the present invention is as follows:

[0007] A method for preparing a berry tea functional dye, the method comprising the following steps:

[0008] The old leaves of berry tea are crushed, added with ethanol solution, and extracted with ultrasound assistance; then the solid and liquid are separated and the filtrate is collected; ethyl acetate is used for extraction, the ethyl acetate extracts are combined, and the ethyl acetate is completely rotary evaporated; ethanol is used for washing and rotary evaporation until the ethanol is completely evaporated to obtain the berry tea functional dye.

[0009] In some embodiments, the preparation method comprises the following steps:

[0010] S1. Crush the old berry tea leaves and pass through a 60-mesh sieve;

[0011] S2, adding the crushed old berry tea leaves to an ethanol solution at a material-liquid ratio of 1 g: 20-50 mL, heating to 50-80° C., and performing alcohol extraction by ultrasonication;

[0012] S3, after the ultrasound is finished, the solid and liquid are separated and the filtrate is collected;

[0013] S4, concentrating the filtrate to 1 / 4-1 / 10 of the original volume to obtain a concentrated solution;

[0014] S5, extracting the concentrated solution with ethyl acetate until the ethyl acetate layer solution is nearly colorless; combining the ethyl acetate extracts, and completely rotary evaporating the ethyl acetate;

[0015] S6. Wash with 1-2 times the volume of ethanol to replace the dye into the ethanol, and rotary evaporate at 60°C until the ethanol is completely evaporated to obtain a solid berry tea functional dye.

[0016] In some embodiments, in step S2, the mass concentration of the ethanol solution is 60-90%.

[0017] In some embodiments, in step S3, solid-liquid separation is performed by suction filtration.

[0018] In some embodiments, in step S4, the filtrate is concentrated at 40-60° C. using a rotary evaporation method.

[0019] The present invention also provides a berry tea functional dye obtained by any of the above-mentioned implementation methods, wherein the functional components in the dye are calculated by mass percentage (component mass / dye mass), and the content of each functional component is as follows:

[0020] Flavonoids 15-20%

[0021] Flavanol component 2-5%

[0022] Flavonol component 0.1-0.3%

[0023] Flavonoids 8-12%

[0024] Polyphenol component 0.05-0.15%.

[0025] The present invention also provides application of the above-mentioned berry tea functional dye in the dyeing process in the fiber printing and dyeing process.

[0026] The present invention also provides a fiber with antibacterial function, which comprises the above-mentioned berry tea functional dye.

[0027] In some embodiments, the fibers include natural fibers, and the natural fibers include at least one of cotton, linen, wool, and silk.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] The present invention uses berry tea plants as raw materials, and obtains an extract including flavonoid components, flavanol components, flavonol components, dihydroflavone components and polyphenol components through a specific method. The extract can be used as a functional dye in natural fiber dyeing to make the fiber have both excellent color and antibacterial effect.

[0030] The invention prepares functional dyes from old berry tea leaves, enriches the antibacterial functional components of berry tea pigments by using extraction technology, and uses the dyes for creating fiber functional materials, thereby greatly improving the economic benefits of berry tea processing.

[0031] The invention prepares functional dyes with old berry tea leaves, recycles agricultural wastes, protects the environment, improves the utilization rate of biological resources, and has significant ecological benefits. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 The dyeing effect of mulberry silk dyed with alum mordant (mulberry silk - aluminum mordant) in Example 1;

[0033] Figure 2 The dyeing effect of wool dyed with alum (wool-aluminum mordant) in Example 1;

[0034] Figure 3 The dyeing effect of the alum mordant dyed hemp (pure hemp - aluminum mordant) of Example 1;

[0035] Figure 4 The dyeing effect of alum mordant dyeing cotton (pure cotton - aluminum mordant dyeing) in Example 1;

[0036] Figure 5 This is the dyeing effect of the ferrous sulfate mordant dyeing silk (mulberry silk - iron mordant dyeing) in Example 2;

[0037] Figure 6 The dyeing effect of wool dyed with ferrous sulfate mordant dyeing (wool - iron mordant dyeing) in Example 2;

[0038] Figure 7 The dyeing effect of flax dyed with ferrous sulfate mordant (pure flax - iron mordant) in Example 2;

[0039] Figure 8 This is the dyeing effect of cotton dyed with ferrous sulfate mordanting (pure cotton - iron mordanting) in Example 2.

[0040] Fig. 9 The antibacterial effect of berry tea functional dye on Staphylococcus aureus.

[0041] Fig.10 The antibacterial effect of berry tea functional dye on Escherichia coli.

[0042] Fig.11 The antibacterial effect of berry tea functional dye on Shigella dysenteriae. DETAILED DESCRIPTION

[0043] Many specific details are set forth in the following description to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways than those described herein, and those skilled in the art can make similar modifications without violating the connotation of the present invention, so the present invention is not limited to the specific implementation disclosed below.

[0044] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0045] Example 1

[0046] A method for preparing a berry tea functional dye comprises the following steps:

[0047] S1, crushing: collect 500g of old leaves of berry tea after pruning, crush them, and pass through a 60-mesh sieve;

[0048] S2, ultrasound: add 15L of 70% ethanol solution to the crushed old berry tea leaves, and extract by ultrasound at 60°C for 2h;

[0049] S3, filtration: use a circulating water vacuum pump to filter the residue and collect the filtrate;

[0050] S4, rotary evaporation: at 50°C, evaporate and concentrate the filtrate to 1 / 5 of the original volume to obtain a concentrated solution;

[0051] S5, extraction: extracting the concentrated solution with ethyl acetate until the ethyl acetate layer solution is almost colorless, combining the ethyl acetate extracts; and drying the extracts by rotary evaporation at 50°C;

[0052] S6, washing: washing with 1-2 times volume of ethanol, replacing the dye into the ethanol, and rotary evaporating at 60°C until the ethanol is completely evaporated to obtain 20.8g of solid berry tea functional dye;

[0053] S7. Dissolving: dissolving the solid berry tea functional dye in pure water to obtain liquid berry tea functional dye.

[0054] Comparative Example 1

[0055] A method for preparing a berry tea functional dye comprises the following steps:

[0056] S1, crushing: collect 500g of old leaves of berry tea after pruning, crush them, and pass through a 60-mesh sieve;

[0057] S2, ultrasound: add 15L of 70% ethanol solution to the crushed old berry tea leaves, and extract by ultrasound at 60°C for 2h;

[0058] S3, filtration: use a circulating water vacuum pump to filter the residue and collect the filtrate;

[0059] S4, rotary evaporation: at 50°C, evaporating and concentrating the filtrate to 1 / 5 of the original volume to obtain a concentrated solution; rotary drying the concentrated solution at 50°C;

[0060] S6, washing: washing with 1-2 times volume of ethanol, replacing the dye into the ethanol, and rotary evaporating at 60°C until the ethanol is completely evaporated to obtain 21.3 g of solid berry tea functional dye;

[0061] S7. Dissolving: dissolving the solid berry tea functional dye in pure water to obtain liquid berry tea functional dye.

[0062] The berry tea solid functional dye obtained in Example 1 and Comparative Example 1 was tested, and its functional components are shown in Table 1. The content of each functional component is calculated by the following formula: Component content (%) = (B / A) × 100%

[0063] In the above formula, A is the sample mass of berry tea leaf solid functional dye; B is the mass of each functional component of berry tea leaf solid functional dye. It can be seen that the components of berry tea leaf solid functional dye in the embodiment are higher than those in the comparative example, and it is inferred that its antibacterial effect is also better than that in the comparative example.

[0064] Table 1 Composition and content of solid functional dyes

[0065]

[0066]

[0067] Application of berry tea functional dyes in natural fiber fabric printing and dyeing:

[0068] (1) Coal dyeing with alum as mordant

[0069] Take 0.8-1.2L of the liquid berry tea functional dye obtained in Example 1, heat it to 80-85°C while stirring, add 8-12g of alum as a mordant, take 15-25g (dry weight) of the fabric to be dyed (mulberry silk, wool, pure linen, pure cotton) that has been soaked in advance, wring it out and put it into the dye solution, dye it at a constant temperature of 80-85°C for 40min, and constantly arrange the fabric during the dyeing to make the dyeing uniform. Take it out after 40min, squeeze out the excess dye solution, wash it thoroughly with clean water, wash off the floating color with a phosphorus-free neutral soap solution, and dry it.

[0070] The dyed fabric obtained is Figure 1-Figure 4 shown.

[0071] (2) One-bath mordant with ferrous sulfate as mordant

[0072] Take 0.8-1.2L of the liquid berry tea functional dye obtained in Example 1, heat it to 80-85°C while stirring, add 0.3-0.5g of ferrous sulfate as a mordant, take 15-25g (dry weight) of the fabric to be dyed (mulberry silk, wool, pure linen, pure cotton) that has been soaked in advance, wring it out and put it into the dye solution, dye it at a constant temperature of 80-85°C for 40min, and constantly arrange the fabric during the dyeing to make the dyeing uniform. Take it out after 40min, squeeze out the excess dye solution, wash it thoroughly with clean water, wash off the floating color with a phosphorus-free neutral soap solution, and dry it.

[0073] The dyed fabric obtained is Figure 5-Figure 8 As shown, the color is bright and beautiful.

[0074] The color fastness performance test of the textiles dyed with the berry tea leaf dye provided in the embodiment and the comparative example is shown in Table 2. It can be seen that the berry tea leaf extract in the embodiment has good color fastness performance after being dyed on the fabric, while the color fastness of the comparative example is poor.

[0075] Table 2 Comparison of color fastness of natural fibers dyed with berry tea dyes

[0076]

[0077]

[0078] Experimental study on antibacterial effect of berry tea functional dye

[0079] 1) Culture medium preparation

[0080] LB liquid medium: YEAST 5g / L, peptone 10g / L, NaCl 10g / L

[0081] LB solid medium: YEAST 5g / L, peptone 10g / L, NaCl 10g / L, Agar 20g / L

[0082] The above culture medium is prepared according to the dosage and sterilized in a high-pressure steam autoclave at 121°C for 20 minutes. The solid culture medium is poured into a sterile plate in an ultra-clean workbench and cooled for later use.

[0083] 2) Bacteria activation

[0084] Escherichia coli, Staphylococcus aureus, and Shigella dysenteriae were inoculated into test tubes containing 5 mL of LB liquid culture medium, respectively. After culturing in a constant temperature shaking incubator at 37°C for 20 h, the culture solution was diluted and spread on a solid culture medium plate. The plate was then inverted and cultured in a 37°C biochemical incubator until colonies appeared.

[0085] 3) Preparation of bacterial solution

[0086] Pick a single colony and inoculate it into a test tube containing 5 mL of liquid culture medium, shake it well, and place it in a constant temperature shaking incubator at 37°C and 150 r / min for 6 hours. Pour all of it into a flask containing 100 mL of liquid culture medium. Continue to incubate for 6 hours, then take 6 mL and inoculate it into a flask containing 300 mL of liquid culture medium and incubate for 12 hours. Use the bacterial solution gradient dilution method to adjust the bacterial solution concentration to 10 -1 , 10 -2 , 10 -3 , 10 -4 , 10 -5 , 10 -6 , 10 -7 , take 200ul of bacterial solution and apply it to plates to verify the appropriate growth concentration of each bacteria.

[0087] 4) Determination of the diameter of the antibacterial transparent zone by paper diffusion method

[0088] Ordinary qualitative filter paper was punched into circular paper pieces with a diameter of 6 mm, sterilized at 121°C for 20 min, and dried (60°C) for later use.

[0089] Under sterile conditions, take 200ul of bacterial solution and evenly spread it on the surface of the solid culture medium. Then use sterile tweezers to pick up a paper and stick it on the surface of the solid culture medium. Then take 20ul of sample (berry tea functional dye concentration 100mg / ml) and put it on the paper. Incubate at 37℃ for 18h, observe and accurately measure the diameter of the transparent circle. At the same time, set up CK (40% acetone solution) negative and kanamycin positive controls.

[0090] 5) Measurement results

[0091] The diameter of the transparent zone of the alcohol-extracted functional dye with a sample concentration of 100 mg / ml on Escherichia coli / Shigella dysenteriae is 8-9 mm; the diameter of the transparent zone on Staphylococcus aureus is 14.7 mm. Figure 9-11 As shown, the antibacterial effect is good.

[0092] The antibacterial properties of the dyed textiles were tested according to the GB / T20944.3-2008 test method using the berry tea leaf dye provided in the examples and comparative examples. The antibacterial rate was calculated by the following formula: Antibacterial rate (%) = (1-B / A) × 100%

[0093] In the above formula, A is the average number of colonies on the fabric not dyed with berry tea dye; B is the average number of colonies on the fabric dyed with berry tea dye. The antibacterial rates of different fabrics are shown in Table 3. It can be seen that the berry tea extract in the embodiment has good antibacterial performance after being dyed on the fabric. The antibacterial effect of the comparative example is poor.

[0094] Table 3 Comparison of antibacterial effect of dyed fabrics

[0095]

[0096] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0097] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A method for preparing a berry tea functional dye, characterized in that: The following steps are involved: S1. Crush the old berry tea leaves and pass through a 60-mesh sieve; S2. Add the crushed old berry tea leaves to an ethanol solution with a mass concentration of 60-90% at a material-liquid ratio of 1 g: 20-50 mL, heat to 50-80° C., and perform alcohol extraction by ultrasound; S3, after the ultrasound is finished, the solid and liquid are separated and the filtrate is collected; S4, concentrating the filtrate to 1 / 4-1 / 10 of the original volume to obtain a concentrated solution; S5, extracting the concentrated solution with ethyl acetate until the ethyl acetate layer solution is nearly colorless; combining the ethyl acetate extracts, and completely rotary evaporating the ethyl acetate; S6, washing with 1-2 times volume of ethanol, replacing the dye into the ethanol, and rotary evaporating at 60°C until the ethanol is completely evaporated to obtain a solid berry tea functional dye; The functional components in the berry tea functional dye are calculated by mass percentage, and the content of each functional component is as follows: Flavonoids 15-20% Flavanol component 3-5% Flavonol component 0.1-0.3% Flavonoids 8-12% Polyphenol component 0.05-0.15%.

2. The method for preparing the berry tea functional dye according to claim 1, characterized in that: In step S3, solid-liquid separation is performed by suction filtration.

3. The method for preparing the berry tea functional dye according to claim 1, characterized in that: In step S4, the filtrate is concentrated at 40-60° C. by rotary evaporation.

4. The berry tea functional dye obtained by the preparation method according to any one of claims 1 to 3.

5. The use of the berry tea functional dye according to claim 4 in fiber printing and dyeing is used in the printing and dyeing process.

6. A fiber with antibacterial function, characterized in that: Including the berry tea functional dye as described in claim 4.

7. The fiber with antibacterial function according to claim 6, characterized in that: The fibers include natural fibers, and the natural fibers include at least one of cotton, linen, wool, and silk.

Images