Preparation method of vegetable dye and dyeing process

Abstract

The invention discloses a preparation method of a vegetable dye and a dyeing process. The preparation method comprises the following steps: S1, raw material selection: selecting a Suzuki plant as a raw material; s2, low-temperature extraction: extracting a crude dye containing dihydroquercetin or quercetin by using a low-temperature extraction method; s3, collecting an extracting solution: collecting the extracting solution into a clean container; s4, filtering: removing insoluble impurities by using filter paper or other proper filter media; s5, primary separation: further removing macromolecular impurities and other non-target components by using a membrane separation technology; s6, purification and analysis: performing HPLC (High Performance Liquid Chromatography) analysis on the filtered extracting solution, and determining the initial content of dihydroquercetin or quercetin; and S7, refining and purifying: further separating and enriching target components by using column chromatography or thin layer chromatography. The method shows good dyeing compatibility for fabrics made of various materials, covers natural fiber fabrics, chemical fiber fabrics and various mixed fiber fabrics, and greatly expands the application range of the fabrics.

Description

Technical Field

[0001] The present invention relates to the technical field of plant dyes, and specifically to a preparation method and a dyeing process of plant dyes. Background Art

[0002] In the textile industry, fabric dyeing is an important link. Although traditional synthetic dyes are rich in colors and have good dyeing effects, they have serious environmental pollution problems and some are harmful to the human body. As a green and environmentally friendly alternative, plant dyes have gradually received attention. However, most of the existing plant dyes have problems such as poor color fastness, harsh dyeing conditions, and limited types of applicable fabrics, making it difficult to meet the diverse and high-quality requirements of the modern textile industry. For this reason, we propose a preparation method and a dyeing process of plant dyes. Summary of the Invention

[0003] The purpose of the present invention is to provide a preparation method and a dyeing process of plant dyes to solve the problems in the prior art.

[0004] To achieve the above purpose, the present invention provides the following technical solution: A preparation method of plant dyes, including the following steps:

[0005] S1. Raw material selection: Select the Sushanjin plant as the raw material;

[0006] S2. Low-temperature extraction: Use the low-temperature extraction method to extract the crude dye containing dihydroquercetin or quercetin;

[0007] S3. Collect the extract: Collect the extract into a clean container;

[0008] S4. Filtration: Use filter paper or other suitable filtration media to remove insoluble impurities;

[0009] S5. Preliminary separation: Use membrane separation technology to further remove macromolecular impurities and other non-target components;

[0010] S6. Purification and analysis: Perform HPLC analysis on the filtered extract to determine the initial content of dihydroquercetin or quercetin;

[0011] S7. Refined purification: Use column chromatography or thin-layer chromatography to further separate and enrich the target components; According to the HPLC results, adjust the purification conditions to achieve the required component ratio;

[0012] S8. Mixing and adjustment: If the required component ratio cannot be achieved by single extraction, it is achieved by mixing extracts from different batches;

[0013] S9. Detection: Use HPLC to detect the mixed sample again to ensure that the content of dihydroquercetin is 92%, or the content of quercetin is in the range of 30%-50%.

[0014] Preferably, after selecting the Sushanjin plant in S1, wash and cut the part of the Sushanjin plant rich in dihydroquercetin or quercetin.

[0015] Preferably, the low-temperature extraction method includes supercritical carbon dioxide extraction or freeze-drying assisted extraction method.

[0016] A dyeing process for plant dyes, using the dye prepared by the preparation method of the plant dye, the dyeing process includes the following steps:

[0017] S11. Dyeing ratio: The dye and clear water are prepared in a ratio of 0.3-0.5%.

[0018] S12. Temperature control: The dyeing temperature of polyester fabric is controlled at 140-165°C; the dyeing temperature of nylon fabric is controlled at 90-140°C.

[0019] S13. Dyeing vat adaptation: Select an overflow vat, a steaming vat or a flat vat.

[0020] S14. Dyeing: The fabric is dyed in the dyeing vat for a fixed time of 6 hours to allow the dye to fully penetrate; after dyeing, perform a reduction cleaning to remove the floating color; then perform dehydration and drying treatments, and finally use a shaping machine to shape in the temperature range of 110-220°C.

[0021] Preferably, for polyester fabric dyeing: Select an overflow vat, put 100 grams of polyester fabric into the vat; according to the ratio of dye to clear water of 0.4%, prepare 50 liters of dye solution; heat the dye solution to 150°C and keep it at a constant temperature for dyeing for 6 hours; after dyeing, perform reduction cleaning, rinse with clear water 3 times, 5 minutes each time; then perform dehydration, and the dehydration time is 10 minutes; dry at 80°C for 2 hours, and finally shape in a shaping machine at 180°C for 15 minutes.

[0022] Preferably, for nylon fabric dyeing: Put 80 grams of nylon fabric into a flat vat, prepare 40 liters of dye solution according to the ratio of dye to clear water of 0.3%; heat the dye solution to 120°C and dye for 6 hours; after dyeing, perform reduction cleaning, rinse with warm water 2 times, 8 minutes each time; after dehydration for 8 minutes, dry at 70°C for 1.5 hours, and shape in a shaping machine at 150°C for 10 minutes.

[0023] Compared with the prior art, the beneficial effects of the present invention are:

[0024] 1. This dye shows good dyeing compatibility with various material fabrics, covering natural fibers (such as cotton, linen, silk, etc.), chemical fiber fibers (such as polyester fiber, polyamide fiber, etc.) and various mixed fiber fabrics, greatly expanding its application range.

[0025] 2. Plant dyes are not only environmentally friendly but also have the function of scavenging free radicals. After 10 washes, the content of the key components of the dye can still be stably maintained at 90%, demonstrating excellent wash resistance and stability, meeting consumers' demands for high-quality dyed fabrics. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The drawings are used to provide a further understanding of the present invention and form a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation to the present invention. In the drawings:

[0027] Figure 1 is a flowchart of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0028] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Apparently, the described embodiments are some but not all of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts fall within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention.

[0029] Embodiment 1

[0030] Please refer to Figure 1 , in the embodiment of the present invention, a preparation method of a plant dye includes the following steps:

[0031] S1. Raw material selection: Select the Sushanjin plant as the raw material;

[0032] S2. Low-temperature extraction: Use the low-temperature extraction method to extract the crude dye containing dihydroquercetin;

[0033] S3. Collect the extract: Collect the extract into a clean container;

[0034] S4. Filtration: Use filter paper or other suitable filtration media to remove insoluble impurities;

[0035] S5. Preliminary separation: Use membrane separation technology to further remove macromolecular impurities and other non-target components;

[0036] S6. Purification and analysis: Perform HPLC analysis on the filtered extract to determine the initial content of dihydroquercetin;

[0037] S7, refinement and purification: use column chromatography or thin layer chromatography to further separate and enrich the target components; according to the HPLC results, adjust the purification conditions to achieve the desired component ratio;

[0038] S8. Mixing adjustment: If the required ratio of components cannot be achieved in a single extraction, it can be achieved by mixing extracts from different batches;

[0039] S9. Detection: The mixed sample was tested again using HPLC to ensure that the dihydroquercetin content was 92%.

[0040] Preferably, after selecting the Sushanjin plant in S1, the dihydroquercetin-rich part of the Sushanjin plant is washed and cut.

[0041] Preferably, the low-temperature extraction method includes supercritical carbon dioxide extraction or freeze-drying assisted extraction method.

[0042] A dyeing process of a plant dye, using a dye prepared by the preparation method of the plant dye, the dyeing process comprises the following steps:

[0043] S11. Dyeing ratio: Dye and clean water are mixed in a ratio of 0.3-0.5%;

[0044] S12. Temperature control: The dyeing temperature of polyester fabrics is controlled at 140-165℃; the dyeing temperature of nylon fabrics is controlled at 90-140℃;

[0045] S13, Dyeing tank adaptation: choose overflow tank, steam tank or flat tank;

[0046] S14, Dyeing: The fabric is dyed in the dye vat for 6 hours to allow the dye to fully penetrate. After dyeing, a reduction cleaning is performed to remove floating color. Then it is dehydrated and dried, and finally a setting machine is used to set the fabric in the temperature range of 110-220℃ to ensure that the fabric size is stable and the color is lasting.

[0047] Preferably, polyester fabric dyeing: use an overflow cylinder, put 100 grams of polyester fabric into the cylinder; prepare 50 liters of dye solution according to the ratio of dye to clean water of 0.4%; heat the dye solution to 150°C, and keep constant temperature for dyeing for 6 hours; after dyeing, perform reduction cleaning, rinse with clean water 3 times, 5 minutes each time; then dehydrate for 10 minutes; dry at 80°C for 2 hours, and finally set in a setting machine at 180°C for 15 minutes to ensure that the fabric size is stable and the color is lasting.

[0048] Preferably, for nylon fabric dyeing: Put 80 grams of nylon fabric in a flat vat, and prepare 40 liters of dye liquor according to the ratio of 0.3% of dye to clear water; Heat the dye liquor to 120 °C and dye for 6 hours; After dyeing, conduct reduction cleaning, rinse with warm water 2 times, 8 minutes each time; After dehydration for 8 minutes, dry at 70 °C for 1.5 hours, and set the shape in a shaping machine at 150 °C for 10 minutes to ensure stable fabric size and long-lasting color.

[0049] Example Two

[0050] Please refer to Figure 1 , in the embodiment of the present invention, a preparation method of a plant dye includes the following steps:

[0051] S1. Raw material selection: Select the Sushanjin plant as the raw material;

[0052] S2. Low-temperature extraction: Use the low-temperature extraction method to extract the crude dye containing quercetin;

[0053] S3. Collect the extract: Collect the extract into a clean container;

[0054] S4. Filtration: Use filter paper or other suitable filtration media to remove insoluble impurities;

[0055] S5. Preliminary separation: Use membrane separation technology to further remove macromolecular impurities and other non-target components;

[0056] S6. Purification and analysis: Conduct HPLC analysis on the filtered extract to determine the initial content of quercetin;

[0057] S7. Refined purification: Use column chromatography or thin-layer chromatography to further separate and enrich the target components; According to the HPLC results, adjust the purification conditions to achieve the required component ratio;

[0058] S8. Mixing and adjustment: If the required component ratio cannot be achieved by single extraction, it can be achieved by mixing extracts from different batches;

[0059] S9. Detection: Use HPLC to detect the mixed sample again to ensure that the quercetin content is in the range of 30% - 50%.

[0060] Preferably, after selecting the Sushanjin plant in S1, wash and cut the quercetin-rich parts of the Sushanjin plant.

[0061] Preferably, the low-temperature extraction method includes supercritical carbon dioxide extraction or freeze-drying assisted extraction method.

[0062] A dyeing process of a plant dye uses the dye prepared by the preparation method of the plant dye, and its dyeing process includes the following steps:

[0063] S11, Dyeing ratio: The dye and clear water are prepared in a ratio of 0.3 - 0.5%;

[0064] S12, Temperature control: The dyeing temperature of polyester fabric is controlled at 140 - 165 °C; the dyeing temperature of nylon fabric is controlled at 90 - 140 °C;

[0065] S13, Dyeing vat adaptation: Select an overflow vat, a steaming vat or a flat vat;

[0066] S14, Dyeing: The fabric is dyed in the dyeing vat for a fixed time of 6 hours to allow the dye to fully penetrate; after dyeing, a reduction cleaning is carried out to remove the floating color; then dehydration and drying treatments are performed, and finally the fabric is shaped in a shaping machine within the temperature range of 110 - 220 °C to ensure stable fabric size and lasting color.

[0067] Preferably, for polyester fabric dyeing: Select an overflow vat, put 100 grams of polyester fabric into the vat; prepare 50 liters of dye liquor according to the ratio of 0.4% of dye to clear water; heat the dye liquor to 150 °C and keep it at a constant temperature for dyeing for 6 hours; after dyeing, carry out reduction cleaning and rinse with clear water 3 times, 5 minutes each time; then perform dehydration, and the dehydration time is 10 minutes; dry at 80 °C for 2 hours, and finally shape in a shaping machine at 180 °C for 15 minutes to ensure stable fabric size and lasting color.

[0068] Preferably, for nylon fabric dyeing: Put 80 grams of nylon fabric into a flat vat, prepare 40 liters of dye liquor according to the ratio of 0.3% of dye to clear water; heat the dye liquor to 120 °C and dye for 6 hours; after dyeing, carry out reduction cleaning and rinse with warm water 2 times, 8 minutes each time; after dehydration for 8 minutes, dry at 70 °C for 1.5 hours, and shape in a shaping machine at 150 °C for 10 minutes to ensure stable fabric size and lasting color.

[0069] Finally, it should be noted that: The above are only the preferred embodiments of the present invention and are not used to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for preparing a plant dye, characterized in that: The following steps are involved: S1. Raw material selection: Select Sushanjin plants as raw materials; S2. Low temperature extraction: using a low temperature extraction method to extract crude dyes containing dihydroquercetin or quercetin; S3, collecting the extract: collecting the extract into a clean container; S4. Filtration: Use filter paper or other suitable filter media to remove insoluble impurities; S5. Preliminary separation: Use membrane separation technology to further remove macromolecular impurities and other non-target components; S6. Purification and analysis: performing HPLC analysis on the filtered extract to determine the initial content of dihydroquercetin or quercetin; S7, refinement and purification: use column chromatography or thin layer chromatography to further separate and enrich the target components; according to the HPLC results, adjust the purification conditions to achieve the desired component ratio; S8. Mixing adjustment: If the required ratio of components cannot be achieved in a single extraction, it can be achieved by mixing extracts from different batches; S9. Detection: Use HPLC to detect the mixed sample again to ensure that the dihydroquercetin content is 92%, or the quercetin content is in the range of 30%-50%.

2. The method for preparing a plant dye according to claim 1, characterized in that: After the Sushanjin plant is selected in S1, the part of the Sushanjin plant rich in dihydroquercetin or quercetin is washed and cut.

3. The method for preparing a plant dye according to claim 1, characterized in that: The low temperature extraction method includes supercritical carbon dioxide extraction or freeze drying assisted extraction method.

4. A dyeing process of plant dyes, characterized in that: A dye prepared by the method for preparing a plant dye according to any one of claims 1 to 3 is used, and its dyeing process comprises the following steps: S11. Dyeing ratio: Dye and clean water are mixed in a ratio of 0.3-0.5%; S12. Temperature control: The dyeing temperature of polyester fabrics is controlled at 140-165℃; the dyeing temperature of nylon fabrics is controlled at 90-140℃; S13, Dyeing tank adaptation: choose overflow tank, steam tank or flat tank; S14, dyeing: the fabric is dyed in the dye vat for 6 hours to allow the dye to fully penetrate; after dyeing, it is restored and cleaned to remove floating color; then it is dehydrated and dried, and finally it is fixed in a setting machine at a temperature range of 110-220℃.

5. A dyeing process of a plant dye according to claim 4, characterized in that: Dyeing of polyester fabric: Use an overflow cylinder and put 100 grams of polyester fabric into the cylinder; prepare 50 liters of dye solution according to the ratio of dye to clean water of 0.4%; heat the dye solution to 150℃ and keep the constant temperature for dyeing for 6 hours; after dyeing, perform reduction cleaning and rinse with clean water 3 times, 5 minutes each time; then dehydrate for 10 minutes; dry at 80℃ for 2 hours, and finally set in a setting machine at 180℃ for 15 minutes.

6. The dyeing process of a plant dye according to claim 4, characterized in that: Dyeing of nylon fabric: put 80g of nylon fabric in a flat cylinder, and prepare 40L of dye solution at a ratio of 0.3% of dye to clean water; heat the dye solution to 120℃ and dye for 6 hours; after dyeing, perform reduction cleaning and rinse with warm water twice, 8 minutes each time; After dehydration for 8 minutes, dry at 70°C for 1.5 hours and set in a setting machine at 150°C for 10 minutes.

Images