Preparation method and dyeing method of vegetable dye capable of dyeing synthetic fibers
By column chromatography and high performance liquid chromatography separation and purification of Xinjiang purpura extract, a variety of single pigments were obtained, and applied to synthetic fiber fabrics through direct dyeing methods, solving the problem of single plant dye chromatography in the prior art, achieving high dyeing rate and good fastness.
Patent Information
- Application Number
- CN202411660089.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2025-04-15
AI Technical Summary
In the prior art, there are fewer varieties of plant dyes used for synthetic fiber dyeing, and there is a problem of single chromatography, which makes it difficult to meet the needs of high dyeing rates, good fastness and diverse chromatography.
The Xinjiang comfrey extract was isolated and purified by column chromatography and high performance liquid chromatography to obtain single pigments such as β,β-dimethacryl comfreylin, acetyl comfreylin and levocfreylin, and applied to synthetic fiber fabrics by direct dyeing.
It has achieved efficient dyeing of synthetic fiber fabrics, with high dyeing rate, good K/S value, excellent soap washing fastness and sun burning fastness, and expanded the dyeing chromatography of plant dyes.
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Figure CN119823591A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to a plant dye, in particular to a method for preparing the plant dye and a method for dyeing synthetic fiber fabrics, and belongs to the technical field of dyeing and finishing of synthetic fiber fabrics. Background Art
[0002] With the development of dyeing and finishing industry, people begin to pay attention to the use of plant dyes. Synthetic fibers are widely used in textiles, clothing, home furnishing and other fields, and synthetic fiber dyeing is an important link in the modern textile industry. It is not only related to the beauty and market competitiveness of textiles, but also involves production efficiency and environmental protection. The traditional dyeing process of synthetic fibers may produce chemical pollutants. Therefore, the use of plant dyes to dye synthetic fibers can not only obtain natural and soft colors, meet consumers' demand for healthy and environmentally friendly products, but also add the ecological health function of plant dyes to the fabric, making the product more functional. However, there are few varieties of plant dyes that can be used for synthetic fiber dyeing, and there is a problem of single color spectrum. Summary of the invention
[0003] The object of the present invention is to provide a method for preparing a plant dye capable of dyeing synthetic fibers and a dyeing method thereof. The plant dye has a high dye uptake rate on synthetic fiber fabrics, a good K / S value, and good fastness, thereby expanding the plant dye dyeing color spectrum of synthetic fiber fabrics.
[0004] In order to solve the above technical problems, the following technical solutions are adopted:
[0005] A method for preparing a plant dye capable of dyeing synthetic fibers, characterized by comprising the following steps:
[0006] (1) weighing Xinjiang lithospermum officinale, and extracting it to obtain lithospermum officinale extract powder;
[0007] (2) using column chromatography, dissolving the lithospermum extract powder with a small amount of dichloromethane, and loading the lithospermum dichloromethane phase into a silica gel column by wet column loading for separation;
[0008] (3) eluting with a petroleum ether / ethyl acetate elution system of different volume ratios and an ethyl acetate / isopropanol elution system of different volume ratios, and collecting the eluents;
[0009] (4) Thin layer chromatography was used to prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate and formic acid as a developing solvent to identify the eluent, and the R f The eluent with the same value can obtain a high-purity single-substance pigment solution;
[0010] (5) using high performance liquid chromatography to qualitatively and quantitatively detect the separated elemental pigment solution;
[0011] (6) The obtained high-purity single substance pigment solution is subjected to rotary evaporation and freeze-drying to obtain a pigment solid powder.
[0012] After optimization, the step (1) comprises the following steps: weighing Xinjiang lithospermum officinale powder, placing it in 50-95% ethanol at a solid-liquid ratio of 1:10-1:30, extracting at a constant temperature of 40-60°C for 60-120 minutes, filtering, vacuum rotary evaporation and freeze-drying to obtain lithospermum officinale extract powder for storage.
[0013] After optimization, the step (2), the column filling process includes: weighing silica gel (200-300 mesh), adding petroleum ether and stirring evenly, filling it in a chromatography column with a diameter of 25mm*400mm, controlling the column filling height to be 25cm, washing the silica gel column with an elution solvent under pressure for about 10min, and rebalancing the silica gel column under normal pressure for 2h; taking the extract powder, concentrating and drying it, adding dichloromethane solvent to dissolve it, loading the sample, and waiting for the dichloromethane phase of lithospermum to penetrate into the silica gel.
[0014] After optimization, in the step (3), the volume ratio of the petroleum ether / ethyl acetate elution system includes: a, petroleum ether: ethyl acetate is 100:0, and the elution time is 20 min; b, petroleum ether: ethyl acetate is 30:1, and the elution time is 120 min; c, petroleum ether: ethyl acetate is 20:1, and the elution time is 60 min; d, petroleum ether: ethyl acetate is 15:1, and the elution time is 60 min; e, petroleum ether: ethyl acetate is 10:1, and the elution time is 30 min; f, petroleum ether: ethyl acetate is 5:1, and the elution time is 60 min; g, petroleum ether: ethyl acetate is 0:100, and the elution time is 30 min.
[0015] After optimization, in the step (3), the volume ratio of the ethyl acetate / isopropanol elution system includes: a. ethyl acetate:isopropanol is 10:1, and the elution time is 30 min; b. ethyl acetate:isopropanol is 0:1, and the elution time is 20 min.
[0016] After optimization, in the step (4), the ratio of petroleum ether: carbon tetrachloride: ethyl acetate: formic acid is prepared to be 5:5:0.6:0.1; and the thin layer chromatography plate is selected as a G-type high-efficiency silica gel plate 50*100 mm.
[0017] After optimization, the chromatographic conditions of the high performance liquid chromatography in step (5) are: the high performance liquid chromatograph is LC-20ADXR, and the chromatographic column conditions are Shim-pack GIS C18 (250mm×4.6mm, 5μm); PAD detector; acetonitrile and 0.05% formic acid aqueous solution were used as mobile phase, and the gradient elution program was as follows: the initial acetonitrile concentration was 66%, the acetonitrile concentration was 66% to 70% from 0 to 5min; the acetonitrile concentration was 70% to 80% from 5 to 20min; the acetonitrile concentration was 80% to 85% from 20 to 25min; the acetonitrile concentration was 85% from 25 to 38min; the acetonitrile concentration was 85% to 66% from 38 to 40min; the acetonitrile concentration was 66% from 40 to 50min; detection wavelength: 275nm; flow rate: 1mL / min; column temperature: 30℃; injection volume: 10μL; standard reference substances were β,β-dimethylacryloylshikonin, acetylshikonin, and L-shikonin.
[0018] A dyeing method for plant dyes capable of dyeing synthetic fibers is characterized by: preparing a dyeing solution with pigment solid powder, wetting a synthetic fiber fabric, and putting the fabric into the dyeing solution at room temperature; adjusting the pH value, and dyeing the synthetic fiber with a direct dyeing process; after dyeing, taking out the synthetic fiber fabric, washing it with clean water, soaping it, and drying it.
[0019] After optimization, a dye solution is prepared at 2% (owf) and a bath ratio of 1:40-60; the synthetic fiber fabric is a polyester fabric, a nylon fabric or a polylactic acid fabric. During the dyeing process, the pH value is adjusted to 4-8, the dyeing temperature is slowly increased to 100-130°C at a heating rate of 1°C / min and kept warm for 40-80min, and then taken out after being cooled to 30°C at a rate of 2°C / min.
[0020] After optimization, the process conditions for soap washing were: water was added at a bath ratio of 1:20, 2 g / L of soap flakes were added, and soap washing was performed at 60° C. for 20 min.
[0021] The above technical solution has the following beneficial effects:
[0022] The invention extracts pigment from Xinjiang lithospermum by ethanol extraction, separates Xinjiang lithospermum extract into single pigment and mixed pigment by column chromatography, and carries out qualitative and quantitative measurement by high performance liquid chromatography to obtain shikonin plant dye.
[0023] The invention dyes the synthetic fiber fabric by single pigment and mixed pigment to obtain the synthetic fiber fabric with high K / S value and good soap fastness and sunlight fastness. BRIEF DESCRIPTION OF THE DRAWINGS The present invention will be further described below in conjunction with the accompanying drawings Figure 1 The HPLC chromatogram of lithospermum pigment in Example 1 is shown; Figure 2 The HPLC chromatogram of lithospermum pigment in Example 2 is shown; Figure 3 It is the HPLC chromatogram of lithospermum pigment of embodiment 3. DETAILED DESCRIPTION
[0024] The present invention aims to provide a method for preparing a plant dye capable of dyeing synthetic fibers and a dyeing method thereof, wherein the plant dye has a high dye uptake rate on synthetic fiber fabrics, a good K / S value, and good fastness, and expands the plant dye dyeing color spectrum of synthetic fiber fabrics. The present invention is further described below in conjunction with specific embodiments, and it should be noted that the following description is only for the purpose of explaining the present invention and does not limit its content.
[0025] Embodiment 1:
[0026] (1) Weigh 40 g of dried Xinjiang lithospermum officinale, crush it into powder using a high-speed grinder, put it into 95% ethanol at a solid-liquid ratio of 1:20, and extract it at a constant temperature of 50° C. for 120 min. Then filter it, evaporate it under reduced pressure, and freeze-dry it to obtain an extract powder to be stored for later use.
[0027] (2) Weigh an appropriate amount of silica gel (200-300 mesh), add an appropriate amount of petroleum ether and stir evenly, fill it into a chromatographic column with a diameter of 25mm*300mm, control the column height to be 25cm, rinse the silica gel column with elution solvent under pressure for about 10min, and then equilibrate the silica gel column under normal pressure for 2h. Take 2g of the extract powder, concentrate and dry it, add 4ml of dichloromethane solvent to dissolve it, load the sample, wait for the sample to penetrate into the silica gel, and elute it with a petroleum ether / ethyl acetate elution system. The solvent ratio is shown in Table 1.
[0028] Table 1 Eluent ratio and gradient elution time
[0029]
[0030] (3) Prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate, and formic acid as a developing solvent in a ratio of 5:5:0.6:0.1, spot the sample using a capillary tube, spot the sample in a volume of 2 μL, and irradiate with white light to obtain R f Value result. Merge R f A single pigment solution with a value of 0.8;
[0031] (4) After high performance liquid chromatography testing, R f The single pigment solution with a value of 0.8 is β,β-dimethylacryloylshikonin, and the HPLC test results are as follows Figure 1 shown.
[0032] The chromatographic conditions of the HPLC test were as follows: the HPLC instrument was LC-20ADXR (purchased from Shimadzu Corporation, Japan), and the chromatographic column was Shim-pack GIS C18 (250mm×4.6mm, 5μm); PAD detector; acetonitrile and 0.05% formic acid aqueous solution were selected as mobile phase, and the gradient elution program was 66% acetonitrile concentration at the beginning, 66% to 70% acetonitrile concentration at 0-5min; 70% to 80% acetonitrile concentration at 5-20min; 80% to 85% acetonitrile concentration at 20-25min; 85% acetonitrile concentration at 25-38min; 85% to 66% acetonitrile concentration at 38-40min; 66% acetonitrile concentration at 40-50min; detection wavelength: 275nm; flow rate: 1mL / min; column temperature: 30℃; injection volume: 10μL; standard reference substances were β,β-dimethylacryloylshikonin, acetylshikonin, and L-shikonin (98%, purchased from Shanghai Tongtian Biotechnology Co., Ltd.). The following examples use the same test conditions.
[0033] (5) The single pigment solution is subjected to rotary evaporation and freeze-drying to obtain pigment solid powder.
[0034] (6) After the synthetic fiber fabric is wetted at room temperature, it is placed in a 2% (owf) lithospermum pigment dye solution at a bath ratio of 1:50, the pH value is adjusted to 5, the temperature is raised to 130° C. at 1° C. / min, and then kept warm for 60 min. After the temperature is lowered and the fabric is taken out, washed with water, soaped, and dried.
[0035] The results of direct dyeing of synthetic fiber fabrics with β,β-dimethylacryloylshikonin are shown in Table 2.
[0036] Table 2 Direct dyeing of synthetic fiber fabrics with β,β-dimethylacryloylshikonin
[0037]
[0038] Embodiment 2:
[0039] (1) Weigh 40 g of dried Xinjiang lithospermum officinale, crush it into powder using a high-speed grinder, put it into 95% ethanol at a solid-liquid ratio of 1:20, and extract it at a constant temperature of 50° C. for 120 min. Then filter it, evaporate it under reduced pressure, and freeze-dry it to obtain an extract powder to be stored for later use.
[0040] (2) Weigh an appropriate amount of silica gel (200-300 mesh), add an appropriate amount of petroleum ether and stir evenly, fill it into a chromatographic column with a diameter of 25mm*300mm, control the column height to be 25cm, rinse the silica gel column with elution solvent under pressure for about 10min, and then equilibrate the silica gel column under normal pressure for 2h. Take 2g of the extract powder, concentrate and dry it, add 4ml of dichloromethane solvent to dissolve it, load the sample, wait for the sample to penetrate into the silica gel, and elute it with a petroleum ether / ethyl acetate elution system. The solvent ratio is shown in Table 1 above.
[0041] (3) Prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate, and formic acid as a developing solvent in a ratio of 5:5:0.6:0.1, spot the sample using a capillary tube, spot the sample in a volume of 2 μL, and irradiate with white light to obtain R f Value result. Merge R f A single pigment solution with a value of 0.65;
[0042] (4) After high performance liquid chromatography testing, R f The single pigment solution with a value of 0.65 is acetylshikonin. The HPLC test results are as follows Figure 2 shown.
[0043] (5) The single pigment solution is subjected to rotary evaporation and freeze-drying to obtain pigment solid powder.
[0044] (6) After the synthetic fiber fabric is wetted at room temperature, it is placed in a 2% (owf) lithospermum pigment dye solution at a bath ratio of 1:50, the pH value is adjusted to 5, the temperature is raised to 130° C. at 1° C. / min, and then kept warm for 60 min. After the temperature is lowered and the fabric is taken out, washed with water, soaped, and dried.
[0045] The results of acetylshikonin dyeing synthetic fiber fabrics are shown in Table 3.
[0046] Table 3 Acetylshikonin dyeing synthetic fiber fabric
[0047]
[0048] Embodiment 3:
[0049] (1) Weigh 40 g of dried Xinjiang lithospermum officinale, crush it into powder using a high-speed grinder, put it into 95% ethanol at a solid-liquid ratio of 1:20, and extract it at a constant temperature of 50° C. for 120 min. Then filter it, evaporate it under reduced pressure, and freeze-dry it to obtain an extract powder to be stored for later use.
[0050] (2) Weigh an appropriate amount of silica gel (200-300 mesh), add an appropriate amount of petroleum ether and stir evenly, fill it into a chromatographic column with a diameter of 25mm*300mm, control the column height to be 25cm, rinse the silica gel column with elution solvent under pressure for about 10min, and then equilibrate the silica gel column under normal pressure for 2h. Take 2g of the extract powder, concentrate and dry it, add 4ml of dichloromethane solvent to dissolve it, load the sample, wait for the sample to penetrate into the silica gel, and elute it with a petroleum ether / ethyl acetate elution system. The solvent ratio is shown in Table 1 above.
[0051] (3) Prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate, and formic acid as a developing solvent in a ratio of 5:5:0.6:0.1, spot the sample using a capillary tube, spot the sample in a volume of 2 μL, and irradiate with white light to obtain R f Value result. Merge R f A single pigment solution with a value of 0.38;
[0052] (4) After high performance liquid chromatography testing, R f The single pigment solution with a value of 0.38 is L-shikonin. The HPLC test results are as follows Figure 3 shown.
[0053] (5) The single pigment solution is subjected to rotary evaporation and freeze-drying to obtain pigment solid powder.
[0054] (6) After the synthetic fiber fabric is wetted at room temperature, it is placed in a 2% (owf) lithospermum pigment dye solution at a bath ratio of 1:50, the pH value is adjusted to 5, the temperature is raised to 130° C. at 1° C. / min, and then kept warm for 60 min. After the temperature is lowered and the fabric is taken out, washed with water, soaped, and dried.
[0055] The results of dyeing synthetic fiber fabrics with L-shikonin are shown in Table 4.
[0056] Table 4 L-shikonin dyeing synthetic fiber fabric
[0057]
[0058] Embodiment 4:
[0059] (1) Weigh 40 g of dried Xinjiang lithospermum officinale, crush it into powder using a high-speed grinder, put it into 95% ethanol at a solid-liquid ratio of 1:20, and extract it at a constant temperature of 50° C. for 120 min. Then filter it, evaporate it under reduced pressure, and freeze-dry it to obtain an extract powder to be stored for later use.
[0060] (2) Weigh an appropriate amount of silica gel (200-300 mesh), add an appropriate amount of petroleum ether and stir evenly, fill it into a chromatographic column with a diameter of 25mm*300mm, control the column height to be 25cm, rinse the silica gel column with elution solvent under pressure for about 10min, and then equilibrate the silica gel column under normal pressure for 2h. Take 2g of the extract powder, concentrate and dry it, add 4ml of dichloromethane solvent to dissolve it, load the sample, wait for the sample to penetrate into the silica gel, and elute it with a petroleum ether / ethyl acetate elution system. The solvent ratio is shown in Table 1 above.
[0061] (3) Prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate, and formic acid as a developing solvent in a ratio of 5:5:0.6:0.1, spot the sample using a capillary tube, spot the sample in a volume of 2 μL, and irradiate with white light to obtain R f Value result. Merge R f The pigment solutions with values of 0.8 and 0.65 were subjected to rotary evaporation and freeze drying to obtain pigment solid powder.
[0062] (4) After the synthetic fiber fabric is wetted at room temperature, it is put into a 2% (owf) lithospermum pigment dye solution at a bath ratio of 1:50, the pH value is adjusted to 5, the temperature is raised to 130° C. at 1° C. / min, and then the temperature is kept for 60 min. After the temperature is lowered and the fabric is taken out, washed with water, soaped, and dried.
[0063] The results of dyeing synthetic fiber fabrics with the mixed pigment of β,β-dimethylacryloylshikonin and acetylshikonin are shown in Table 5.
[0064] Table 5 Synthetic fiber fabrics dyed with mixed pigments of β,β-dimethylacryloylshikonin and acetylshikonin
[0065]
[0066] Embodiment 5:
[0067] (1) Weigh 40 g of dried Xinjiang lithospermum officinale, crush it into powder using a high-speed grinder, put it into 95% ethanol at a solid-liquid ratio of 1:20, and extract it at a constant temperature of 50° C. for 120 min. Then filter it, evaporate it under reduced pressure, and freeze-dry it to obtain an extract powder to be stored for later use.
[0068] (2) Weigh an appropriate amount of silica gel (200-300 mesh), add an appropriate amount of petroleum ether and stir evenly, fill it into a chromatographic column with a diameter of 25mm*300mm, control the column height to be 25cm, rinse the silica gel column with elution solvent under pressure for about 10min, and then equilibrate the silica gel column under normal pressure for 2h. Take 2g of the extract powder, concentrate and dry it, add 4ml of dichloromethane solvent to dissolve it, load the sample, wait for the sample to penetrate into the silica gel, and elute it with a petroleum ether / ethyl acetate elution system. The solvent ratio is shown in Table 1 above.
[0069] (3) Prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate, and formic acid as a developing solvent in a ratio of 5:5:0.6:0.1, spot the sample using a capillary tube, spot the sample in a volume of 2 μL, and irradiate with white light to obtain R f Value result. Merge R f The pigment solutions with values of 0.8 and 0.38 were subjected to rotary evaporation and freeze drying to obtain pigment solid powder.
[0070] (4) After the synthetic fiber fabric is wetted at room temperature, it is put into a 2% (owf) lithospermum pigment dye solution at a bath ratio of 1:50, the pH value is adjusted to 5, the temperature is raised to 130° C. at 1° C. / min, and then the temperature is kept for 60 min. After the temperature is lowered and the fabric is taken out, washed with water, soaped, and dried.
[0071] The results of dyeing synthetic fiber fabrics with the mixed pigment of β,β-dimethylacryloylshikonin and L-shikonin are shown in Table 6.
[0072] Table 6 Synthetic fiber fabrics dyed with mixed pigments of β,β-dimethylacryloylshikonin and L-shikonin
[0073]
[0074] Embodiment 6:
[0075] (1) Weigh 40 g of dried Xinjiang lithospermum officinale, crush it into powder using a high-speed grinder, put it into 95% ethanol at a solid-liquid ratio of 1:20, and extract it at a constant temperature of 50° C. for 120 min. Then filter it, evaporate it under reduced pressure, and freeze-dry it to obtain an extract powder to be stored for later use.
[0076] (2) Weigh an appropriate amount of silica gel (200-300 mesh), add an appropriate amount of petroleum ether and stir evenly, fill it into a chromatographic column with a diameter of 25mm*300mm, control the column height to be 25cm, rinse the silica gel column with elution solvent under pressure for about 10min, and then equilibrate the silica gel column under normal pressure for 2h. Take 2g of the extract powder, concentrate and dry it, add 4ml of dichloromethane solvent to dissolve it, load the sample, wait for the sample to penetrate into the silica gel, and elute it with a petroleum ether / ethyl acetate elution system. The solvent ratio is shown in Table 1 above.
[0077] (3) Prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate, and formic acid as a developing solvent in a ratio of 5:5:0.6:0.1, spot the sample using a capillary tube, spot the sample in a volume of 2 μL, and irradiate with white light to obtain R f Value result. Merge R f The pigment solutions with values of 0.65 and 0.38 were subjected to rotary evaporation and freeze drying to obtain pigment solid powder.
[0078] (4) After the synthetic fiber fabric is wetted at room temperature, it is put into a 2% (owf) lithospermum pigment dye solution at a bath ratio of 1:50, the pH value is adjusted to 5, the temperature is raised to 130° C. at 1° C. / min, and then the temperature is kept for 60 min. After the temperature is lowered and the fabric is taken out, washed with water, soaped, and dried.
[0079] The results of dyeing synthetic fiber fabrics with the mixed pigment of acetylshikonin and L-shikonin are shown in Table 7.
[0080] Table 7 Synthetic fiber fabric dyed with acetylshikonin and L-shikonin mixed pigment
[0081]
[0082] The synthetic fiber fabrics dyed with plant dyes described in Examples 1, 2, 3, 4, 5 and 6 were tested.
[0083] K / S value: SF600X Datacolor colorimetric spectrometer was used to test the K / S value of the fabric under D65 light source.
[0084] Fastness test: Refer to GB / T 8427-2008 "Textiles - Tests for color fastness - Color fastness to artificial light: Xenon arc fading lamp" to determine the light fastness of dyed samples; refer to GB / T 3921-2019 "Textiles - Tests for color fastness - Color fastness to washing with soap" method, and use the grey sample card to evaluate the color change of the sample and the color fastness to the adjacent fabric.
[0085] In the present invention, the pigment of Xinjiang lithospermum is extracted by ethanol extraction, the Xinjiang lithospermum extract is separated into a single pigment by column chromatography, and the high performance liquid chromatography is used for qualitative and quantitative measurement to obtain β,β-dimethylacryloylshikonin, acetylshikonin and L-shikonin plant dyes and two-by-two mixed pigments. By direct dyeing method, the K / S value of β,β-dimethylacryloylshikonin plant dye directly dyed polyester is the highest and the soap fastness and light fastness are the best; the K / S value of acetylshikonin and L-shikonin mixed pigment dyed nylon fabric is the highest; the fastness of β,β-dimethylacryloylshikonin and acetylshikonin mixed pigment dyed nylon fabric is the best; the K / S value of β,β-dimethylacryloylshikonin directly dyed polylactic acid fabric is the highest, and the soap fastness and light fastness of β,β-dimethylacryloylshikonin and acetylshikonin mixed pigment dyed polylactic acid fabric is the best. Therefore, the polyester fabric dyeing and finishing technology of the present invention has broad application prospects.
[0086] The above are only specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent replacements or modifications made based on the present invention to solve basically the same technical problems and achieve basically the same technical effects are all included in the protection scope of the present invention.
Claims
1. A method for preparing a plant dye capable of dyeing synthetic fibers, characterized in that The steps include: (1) weighing Xinjiang lithospermum officinale, and extracting it to obtain lithospermum officinale extract powder; (2) using column chromatography, dissolving the lithospermum extract powder in dichloromethane, and loading the lithospermum dichloromethane phase into a silica gel column by wet column loading for separation; (3) eluting with a petroleum ether / ethyl acetate elution system of different volume ratios and an ethyl acetate / isopropanol elution system of different volume ratios, and collecting the eluents; (4) Thin layer chromatography was used to prepare a mixed solution of petroleum ether, carbon tetrachloride, ethyl acetate and formic acid as a developing solvent to identify the eluent, and the R f The eluent with the same value can obtain a high-purity single-substance pigment solution; (5) using high performance liquid chromatography to qualitatively and quantitatively detect the separated elemental pigment solution; (6) The obtained high-purity single substance pigment solution is subjected to rotary evaporation and freeze-drying to obtain a pigment solid powder.
2. The method for preparing a plant dye capable of dyeing synthetic fibers according to claim 1, characterized in that: The step (1) comprises the following steps: weighing Xinjiang sclerophyll powder, placing it in 50-95% ethanol at a solid-liquid ratio of 1:10-1:30, extracting at a constant temperature of 40-60°C for 60-120 minutes, filtering, vacuum rotary evaporation and freeze drying to obtain sclerophyll extract powder for storage.
3. The method for preparing a plant dye capable of dyeing synthetic fibers according to claim 1, characterized in that: The step (2) comprises the following steps: weighing silica gel, adding petroleum ether and stirring evenly, filling the silica gel column in a chromatography column, washing the silica gel column with an eluting solvent under pressure for 10 minutes, and balancing the silica gel column under normal pressure for 2 hours; taking the extract powder, concentrating and drying it, adding dichloromethane solvent to dissolve it, loading the sample, and waiting for the lithospermum dichloromethane phase to penetrate into the silica gel.
4. The method for preparing a plant dye capable of dyeing synthetic fibers according to claim 1, characterized in that: In the step (3), the volume ratio of the petroleum ether / ethyl acetate elution system comprises: a. Petroleum ether: ethyl acetate is 100:0, and the elution time is 20 min; b. Petroleum ether: ethyl acetate: 30:1, elution time: 120 min; c. Petroleum ether: ethyl acetate is 20:1, and the elution time is 60 min; d. Petroleum ether: ethyl acetate is 15:1, and the elution time is 60 min; e. Petroleum ether: ethyl acetate is 10:1, and the elution time is 30 min; f. Petroleum ether: ethyl acetate: 5:1, elution time: 60 min; g, petroleum ether: ethyl acetate is 0:100, and the elution time is 30 min.
5. The method for preparing a plant dye capable of dyeing synthetic fibers according to claim 1, characterized in that: In the step (3), the volume ratio of the ethyl acetate / isopropanol elution system comprises: a. Ethyl acetate: isopropanol ratio is 10:1, and the elution time is 30 min; b. Ethyl acetate: isopropanol is 0:1, and the elution time is 20 min.
6. The method for preparing a plant dye capable of dyeing synthetic fibers according to claim 1, characterized in that: In the step (4), the ratio of petroleum ether: carbon tetrachloride: ethyl acetate: formic acid is prepared to be 5:5:0.6:0.
1.
7. The method for preparing a plant dye capable of dyeing synthetic fibers according to claim 1, characterized in that: In the step (5), the chromatographic conditions of the high performance liquid chromatography are as follows: the high performance liquid chromatograph is LC-20ADXR, the chromatographic column condition is Shim-pack GIS C18 (250mm×4.6mm, 5μm); PAD detector; the mobile phase is acetonitrile and 0.05% formic acid aqueous solution, and the gradient elution program is as follows: the initial acetonitrile concentration is 66%, the acetonitrile concentration is 66% to 70% at 0-5min; the acetonitrile concentration is 70% to 80% at 5-20min; the acetonitrile concentration is 80% to 85% at 20-25min; the acetonitrile concentration is 85% at 25-38min; the acetonitrile concentration is 85% to 66% at 38-40min; the acetonitrile concentration is 66% at 40-50min; the detection wavelength is 275nm; the flow rate is 1mL / min; the column temperature is 30°C; the injection volume is 10μL; The standard reference substances were β,β-dimethylacryloylshikonin, acetylshikonin, and L-shikonin.
8. The method for dyeing synthetic fibers with a plant dye as claimed in claim 1, characterized in that: The pigment solid powder is prepared into a dye solution, the synthetic fiber fabric is wetted and put into the dye solution at room temperature; the pH value is adjusted and the synthetic fiber is dyed by a direct dyeing process; After dyeing, take out the synthetic fiber fabric, wash it with clean water, soap it, and dry it.
9. The method for dyeing synthetic fibers with a plant dye according to claim 8, characterized in that: The dyeing solution is prepared at 2% (owf) and a bath ratio of 1:40-60; the synthetic fiber fabric is polyester fabric, nylon fabric or polylactic acid fabric. During the dyeing process, the pH value is adjusted to 4-8, the dyeing temperature is slowly increased to 100-130°C at a heating rate of 1°C / min and kept warm for 40-80min, and then taken out after being cooled to 30°C at a rate of 2°C / min.
10. The method for dyeing synthetic fibers with plant dyes according to claim 8, characterized in that: The process conditions for soap washing are: water is added at a bath ratio of 1:20, soap flakes are added at 2g / L, and soap washing is carried out at 60°C for 20 minutes.