An ultra-low pollution environment-friendly liquid disperse dye

Abstract

The present disclosure relates to the field of textile printing and dyeing technology, and particularly relates to an environmentally-friendly liquid dispersion dye with ultra-low pollution; the environmentally-friendly liquid dispersion dye is prepared by the following steps: preparing a Hippophae rhamnoides extract, dissolving the Hippophae rhamnoides extract in an acid solution and mixing with aluminum hydroxide; preparing a Ginkgo biloba extract, dissolving the Ginkgo biloba extract in an acid solution and mixing with aluminum hydroxide; then mixing the two in a sodium bicarbonate aqueous solution with a complexing agent and a stabilizer, drying to obtain a solid, and finally reacting the solid with polyethyleneimine to obtain an environmentally-friendly orange dye with good dispersibility.

Description

TECHNICAL FIELD

[0001] The present disclosure relates to the technical field of textile printing and dyeing, and particularly relates to an environmentally-friendly liquid dispersion dye with ultra-low pollution. BACKGROUND

[0002] In the history of mankind, natural dyes have made indelible contributions to beautifying people's lives. Since the end of the 19th century, due to the rapid development of synthetic dyes, natural dyes have basically withdrawn from the field of fabric dyeing. With the continuous enhancement of human environmental protection consciousness and the increasing concern for their own health, the harm of some synthetic dyes to human health and ecological environment has attracted more and more attention. Under the global green revolution wave, natural dyes have begun to be valued by people again. Among the natural dyes, animal and plant dyes are extracted from biological bodies, and have good environmental compatibility and can be biodegraded.

[0003] Caragana is a perennial shrub of Leguminosae, Caragana plant, also known as Mao Tiao and Bai Ningtiao. The leaf stalk has thorns, and the growth form shows single or cluster. The flower stalk has joints, the main root penetrates into the soil about 40.0-70.0 cm, and the highest can grow to about 2 m. Caragana has many excellent properties, such as drought resistance, heat resistance, cold resistance, and strong salt and alkali resistance. The tender branches, leaves, flowers, fruits and seeds of Caragana contain rich nutrients and rich tannin. Tannin, also known as tannic acid, tannin and tannic acid, is rich in the epidermis of dicotyledonous plants and flowers, especially in the trees and shrubs growing in subtropical and tropical regions.

[0004] Ginkgo biloba, also known as white fruit and Gong Sun tree, is a relic plant of Ginkgoaceae and Ginkgo biloba, and is known as "living fossil". The main chemical components in Ginkgo biloba leaves are orange ketone and rutin.

[0005] At present, there is an urgent need for a method for preparing dyes by effectively utilizing abundant plant resources as raw materials. SUMMARY

[0006] The present disclosure provides an environmentally-friendly liquid dispersion dye with ultra-low pollution to solve the problems in the prior art.

[0007] According to a first aspect of an embodiment of the present disclosure, an environmentally-friendly liquid dispersion dye with ultra-low pollution is provided, which is prepared by the following steps:

[0008] Step 1: preparing a first plant tannin extract;

[0009] Step 2: dissolving the first plant tannin extract in water, adding acid and / or anhydride, adjusting the pH value to 2-3, keeping stirring, adding aluminum hydroxide thereto, continuing stirring for 0.5-1 h after the addition is completed, and obtaining a first mixed solution;

[0010] Step 3: Prepare the second plant citron extract;

[0011] Step 4: Dissolve the second plant tannin extract in water, add acid and / or acid anhydride to adjust the pH to 4-5, keep stirring, add aluminum hydroxide, and continue stirring for 0.5-1 h after the addition is complete to obtain the second mixture;

[0012] Step 5: Provide an aqueous solution of sodium bicarbonate, keep stirring, add the first mixture, the second mixture, the complexing agent and the stabilizer to obtain an intermediate product solution;

[0013] Step 6: The intermediate product solution is concentrated and dried to obtain the intermediate product solid;

[0014] Step 7: Provide an organic solution containing polyethyleneimine, add the intermediate solid under nitrogen protection, react at 60℃-70℃ for 4-6 hours, and then wash, rotary evaporate and dry to obtain an environmentally friendly liquid disperse dye solid.

[0015] In one aspect of this disclosure, the first plant tannin extract is selected from *Caragana korshinskii* extract; the second plant citronella extract is selected from *Ginkgo biloba* leaf extract.

[0016] In this disclosure, the environmentally friendly liquid disperse dye prepared is an orange dye.

[0017] In one aspect of this disclosure, the Caragana korshinskii extract is prepared by the following steps:

[0018] Step 1-1: Provide lemon twigs; wash, dry, and sieve the lemon twigs to obtain lemon twig powder;

[0019] Steps 1-2: Prepare an acetone aqueous solution, wherein the volume fraction of acetone is selected from 30%-60%; under the condition that the material-liquid ratio is selected from (20-30):1, add the Caragana korshinskii powder to the acetone aqueous solution, and then reflux extract at 60℃-70℃ for 2-3 hours, repeat the extraction 2-4 times to obtain Caragana korshinskii extract aqueous solution.

[0020] Steps 1-3: The aqueous solution of *Leonurus japonicus* is filtered, concentrated, and freeze-dried to obtain the *Leonurus japonicus* extract.

[0021] In one aspect of this disclosure, the Caragana korshinskii extract is prepared by the following steps:

[0022] Step 1-1: Provide lemon twigs; wash, dry, and sieve the lemon twigs to obtain lemon twig powder;

[0023] Step 1-2: preparing an aqueous acetone solution, wherein the volume fraction of acetone is selected from 50%; under the condition that the solid-liquid ratio is selected from 25:1, the caragana powder is added into the aqueous acetone solution, and then reflux extraction is carried out at 65℃ for 2.5h, and the extraction is repeated for 3 times to obtain an aqueous caragana extract solution;

[0024] Step 1-3: filtering, concentrating and freeze-drying the aqueous caragana solution to obtain the caragana extract.

[0025] In an aspect of the embodiments of the present disclosure, the ginkgo leaf extract is prepared by the following steps:

[0026] Step 3-1: providing ginkgo leaves; washing, drying and sieving the ginkgo leaves to obtain ginkgo leaf powder;

[0027] Step 3-2: preparing a deep eutectic solvent; the deep eutectic solvent comprises acetylcholine and urea, wherein the molar ratio of the acetylcholine and urea is selected from 1-2:1; and the mass percentage of the mass sum of the acetylcholine and lactic acid in the total mass of the deep eutectic solvent is selected from 25%-50%;

[0028] Step 3-3: adding the ginkgo leaf powder into the deep eutectic solvent, heating and stirring at 40-50℃ for 3-5h to obtain an aqueous ginkgo leaf extract solution;

[0029] Step 3-4: filtering, concentrating and freeze-drying the aqueous ginkgo leaf extract solution to obtain the ginkgo leaf extract.

[0030] In an aspect of the embodiments of the present disclosure, the ginkgo leaf extract is prepared by the following steps:

[0031] Step 3-1: providing ginkgo leaves; washing, drying and sieving the ginkgo leaves to obtain ginkgo leaf powder;

[0032] Step 3-2: preparing a deep eutectic solvent; the deep eutectic solvent comprises acetylcholine and urea, wherein the molar ratio of the acetylcholine and urea is selected from 1.5:1; and the mass percentage of the mass sum of the acetylcholine and lactic acid in the total mass of the deep eutectic solvent is selected from 30%;

[0033] Step 3-3: adding the ginkgo leaf powder into the deep eutectic solvent, heating and stirring at 45℃ for 4h to obtain an aqueous ginkgo leaf extract solution;

[0034] Step 3-4: filtering, concentrating and freeze-drying the aqueous ginkgo leaf extract solution to obtain the ginkgo leaf extract.

[0035] In an aspect of the embodiments of the present disclosure, step 2 comprises:

[0036] Step 2-1: Dissolve the Caragana extract in 15-20 times the mass of water, add glacial acetic acid to regulate the pH value to 2.2-2.7; obtain the solution of step 2-1;

[0037] Step 2-2: Keep the solution of step 2-1 in a stirring state, the stirring rate is selected from 200-600 r / min, add aluminum hydroxide thereto, continue to stir for 30-45 min after the addition is completed, to obtain a first mixed solution; wherein the mass ratio of the Caragana extract and aluminum hydroxide is selected from 1:(0.25-0.5).

[0038] In an aspect of the embodiment of the present disclosure, step 2 comprises:

[0039] Step 2-1: Dissolve the Caragana extract in 16 times the mass of water, add glacial acetic acid to regulate the pH value to 2.6; obtain the solution of step 2-1;

[0040] Step 2-2: Keep the solution of step 2-1 in a stirring state, the stirring rate is selected from 500 r / min, add aluminum hydroxide thereto, continue to stir for 45 min after the addition is completed, to obtain a first mixed solution; wherein the mass ratio of the Caragana extract and aluminum hydroxide is selected from 1:0.35.

[0041] In an aspect of the embodiment of the present disclosure, step 4 comprises:

[0042] Step 4-1: Dissolve the Ginkgo biloba extract in 20-30 times the mass of water, add maleic anhydride to regulate the pH value to 4.2-4.7; obtain the solution of step 4-1; wherein the mass ratio of the Ginkgo biloba extract and the Caragana extract used in step 2-1 is selected from (0.15-0.2):1;

[0043] Step 4-2: Keep the solution of step 4-1 in a stirring state, the stirring rate is selected from 200-600 r / min, add aluminum hydroxide thereto, continue to stir for 30-45 min after the addition is completed, to obtain a second mixed solution; wherein the mass ratio of the Ginkgo biloba extract and aluminum hydroxide is selected from 1:(0.15-0.35).

[0044] In an aspect of the embodiment of the present disclosure, step 4 comprises:

[0045] Step 4-1: Dissolve the Ginkgo biloba extract in 25 times the mass of water, add maleic anhydride to regulate the pH value to 4.3; obtain the solution of step 4-1; wherein the mass ratio of the Ginkgo biloba extract and the Caragana extract used in step 2-1 is selected from 0.25:1;

[0046] Step 4-2: keep the solution of step 4-1 under stirring, the stirring rate is selected from 500 r / min, add aluminum hydroxide into the solution, continue stirring for 45 min after the addition is completed, to obtain a second mixed solution; wherein, the mass ratio of the ginkgo biloba extract and the aluminum hydroxide is selected from 1:0.2.

[0047] In an aspect of the embodiments of the present disclosure, the stabilizer is selected from boric acid, ammonium acetate, tartaric acid or potassium hydrogen phthalate; the complexing agent is selected from potassium sodium tartrate, ethylenediaminetetraacetic acid, sodium polyphosphate or sodium citrate; preferably, the stabilizer is selected from ammonium acetate, and the complexing agent is selected from potassium sodium tartrate.

[0048] In an aspect of the embodiments of the present disclosure, step 5 comprises:

[0049] Step 5-1: provide a 5% concentration of sodium bicarbonate aqueous solution, keep stirring, the stirring rate is selected from 200-600 r / min, add the first mixed solution, the second mixed solution, the complexing agent and the stabilizer, to obtain an intermediate product solution.

[0050] In an aspect of the embodiments of the present disclosure, the mass of the stabilizer is selected from 5%-20% of the caragana extract; the mass of the complexing agent is selected from 10%-20% of the caragana extract; preferably, the mass of the stabilizer is selected from 5%-8% of the caragana extract; the mass of the complexing agent is selected from 12%-16% of the caragana extract.

[0051] In an aspect of the embodiments of the present disclosure, the mass ratio of the polyethyleneimine and the intermediate product solid is selected from (0.15-0.35):1.

[0052] The technical solutions provided by the embodiments of the present disclosure can include the following beneficial effects:

[0053] As can be seen from the above embodiments, the present disclosure prepares an orange dye which is stable in color, good in dispersibility and does not use high-pollution and high-toxicity raw materials in the preparation process.

[0054] It should be understood that the foregoing general description and the following detailed description are only exemplary and explanatory, and cannot limit the present disclosure. DETAILED DESCRIPTION

[0055] In order to make the objects, technical solutions and advantages of the present application clearer, the technical solutions of the present application will be described clearly and completely below in conjunction with embodiments. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. The embodiments described herein are illustrative in nature and are used to provide a basic understanding of the present application. The embodiments of the present application should not be interpreted as a limitation of the present application.

[0056] For the sake of brevity, only some numerical ranges are specifically disclosed herein. However, any upper limit can be combined with any lower limit to create a range not explicitly recited; and, any lower limit can be combined with any other lower limit to create a range not explicitly recited, as well as any upper limit can be combined with any other upper limit to create a range not explicitly recited. Further, each individual disclosed point or singular value can be combined with any other point or singular value as a lower limit or upper limit to create a range not explicitly recited.

[0057] In this document, the terms "comprise", "comprising", or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can also include other elements not expressly listed or inherent to such process, method, article, or apparatus. An element proceeded by "comprises... a" does not, without more constraints, exclude the presence of additional identical elements in the process, method, article, or apparatus that comprises the element.

[0058] In the description herein, "above", "below" include the number itself, unless otherwise indicated.

[0059] Unless otherwise indicated, the terms used in the present application have the meanings commonly understood by a person of ordinary skill in the art. Unless otherwise indicated, the values of the parameters mentioned in the present application can be measured using the various measuring methods commonly used in the art (for example, tests can be performed according to the methods given in the examples of the present application).

[0060] The term "about" is used to describe and account for small variations. When used in connection with an event or circumstance, the term can refer to instances where the event or circumstance occurs exactly, as well as instances where the event or circumstance occurs with a close approximation. For example, when used in connection with a numerical value, the term can refer to a range of variation less than or equal to ±10% of that value, such as less than or equal to ±5%, less than or equal to ±4%, less than or equal to ±3%, less than or equal to ±2%, less than or equal to ±1%, less than or equal to ±0.5%, less than or equal to ±0.1%, or less than or equal to ±0.05%. Additionally, quantities, ratios and other numerical values are sometimes presented herein in a range format. It is to be understood that such range format is used for convenience and brevity and should be understood as having been preceeded by the word "about". Also, a number of different aspects are presented in this detailed description by expressing their quantitative limitations in a single format. Each expression is specifically disclosed in this format; however, it is to be understood that each expression so disclosed also describes every combination of such expressions in that format expressed otherwise.

[0061] The list of items connected by "at least one of," "one or more of," or other similar phrases can mean any combination of the listed items. For example, if items A and B are listed, the phrase "at least one of A and B" means only A; only B; or A and B. In another example, if items A, B, and C are listed, the phrase "at least one of A, B, and C" means only A; only B; only C; A and B (excluding C); A and C (excluding B); B and C (excluding A); or all of A, B, and C. Item A can include a single component or multiple components. Item B can include a single component or multiple components. Item C can include a single component or multiple components.

[0062] The present application is further illustrated by the following examples. It is to be understood that these examples are merely illustrative of the present application and do not limit the scope of the application.

[0063] Examples and Comparative Examples:

[0064] Example One

[0065] comprising the following steps:

[0066] 1. Preparation of a Caragana extract:

[0067] Caragana is provided, washed with water, dried at 60°C, and sieved through a 50 mesh screen to obtain a Caragana powder. An aqueous acetone solution is prepared, wherein the volume fraction of acetone is selected from 50%. The Caragana powder is added to the aqueous acetone solution under the condition that the solid-liquid ratio is selected from 25:1, and then refluxed at 65°C for 2.5 hours, repeated for 3 times to obtain an aqueous Caragana extract solution. The aqueous Caragana extract solution is filtered, concentrated, and freeze-dried to obtain the Caragana extract. The above steps are repeated as appropriate to obtain sufficient product for use in the following reactions.

[0068] 2. Preparation of a Ginkgo biloba leaf extract:

[0069] Ginkgo biloba leaves are provided, washed with water, dried at 60°C, and sieved through a 30 mesh screen to obtain a Ginkgo biloba leaf powder. A deep eutectic solvent (the deep eutectic solvent comprises acetylcholine and urea, wherein the molar ratio of acetylcholine and urea is selected from 1.5:1; the mass percentage of the sum of the mass of acetylcholine and lactic acid based on the total mass of the deep eutectic solvent is selected from 30%) is prepared. The Ginkgo biloba leaf powder is added to the deep eutectic solvent, heated and stirred at 45°C for 4 hours to obtain an aqueous Ginkgo biloba leaf extract solution. The aqueous Ginkgo biloba leaf extract solution is filtered, concentrated, and freeze-dried to obtain the Ginkgo biloba leaf extract. The above steps are repeated as appropriate to obtain sufficient product for use in the following reactions.

[0070] 3. Preparation of a dye:

[0071] Take 100 parts by weight of the Caragana extract, dissolved in 1600 parts by weight of water, add glacial acetic acid, adjust the pH value to 2.6, to obtain solution A-1; keep solution A-1 in the state of stirring (500 r / min), add 35 parts by weight of aluminum hydroxide to it, continue stirring for 45 min after the addition is completed, to obtain solution A-2;

[0072] Take 25 parts by weight of the Ginkgo biloba extract, dissolved in 625 parts by weight of water, add maleic anhydride, adjust the pH value to 4.3, to obtain solution B-1; keep solution B-1 in the state of stirring (500 r / min), add 5 parts by weight of aluminum hydroxide to it, continue stirring for 45 min after the addition is completed, to obtain solution B-2;

[0073] Provide 3000 parts by weight of a 5% concentration of sodium bicarbonate aqueous solution, keep stirring (500 r / min), add solution A-2, solution B-2, 15 parts by weight of the complexing agent potassium sodium tartrate, 6 parts by weight of the stabilizer ammonium acetate, to obtain an intermediate product solution;

[0074] Concentrate and dry the intermediate product solution to obtain 113 parts by weight of an intermediate product solid; dissolve 36 parts by weight of polyethyleneimine in 200 parts by weight of DMF, under the protection of nitrogen, add the aforementioned intermediate product solid, react at 70°C for 5 h, then wash, rotary evaporate and dry, to obtain the environmentally friendly liquid disperse dye solid of Example One.

[0075] Example Two

[0076] Comprising the following steps:

[0077] 1. Preparation of Caragana extract:

[0078] Provide Caragana, wash the Caragana with water, dry at 60°C, pass through a 50-mesh sieve to obtain Caragana powder; prepare an aqueous acetone solution, wherein the volume fraction of acetone is selected from 50%; under the condition that the solid-liquid ratio is selected from 25:1, add the Caragana powder to the aqueous acetone solution, then reflux extract at 65°C for 2.5 h, repeat the extraction for 3 times, to obtain an aqueous Caragana extract solution; filter, concentrate, freeze-dry the aqueous Caragana solution, to obtain the Caragana extract. Appropriately repeat the above steps to obtain sufficient product for the following reaction.

[0079] 2. Preparation of Ginkgo biloba extract:

[0080] Ginkgo biloba leaves are provided; the Ginkgo biloba leaves are washed with water, dried at 60°C, and passed through a 30-mesh screen to obtain Ginkgo biloba leaf powder; a deep eutectic solvent (the deep eutectic solvent comprises acetylcholine and urea, wherein the molar ratio of acetylcholine to urea is selected from 1.5:1; the mass percentage of the sum of the mass of acetylcholine and the mass of lactic acid based on the total mass of the deep eutectic solvent is selected from 30%) is prepared; the Ginkgo biloba leaf powder is added to the deep eutectic solvent, heated and stirred at 45°C for 4h to obtain a Ginkgo biloba extract aqueous solution; the Ginkgo biloba extract aqueous solution is filtered, concentrated, and freeze-dried to obtain a Ginkgo biloba extract. The above steps are appropriately repeated to obtain a sufficient amount of product for the following reaction.

[0081] 3. Preparation of a dye:

[0082] 100 parts by weight of Caragana extract are weighed out, dissolved in 1600 parts by weight of water, and ice acetic acid is added to adjust the pH value to 2.6 to obtain solution A-1; solution A-1 is kept under stirring (500 r / min), and 35 parts by weight of aluminum hydroxide is added thereto, and after the addition is completed, stirring is continued for 45 min to obtain solution A-2;

[0083] 75 parts by weight of Ginkgo biloba extract are weighed out, dissolved in 625 parts by weight of water, and maleic anhydride is added to adjust the pH value to 4.3 to obtain solution B-1; solution B-1 is kept under stirring (500 r / min), and 15 parts by weight of aluminum hydroxide is added thereto, and after the addition is completed, stirring is continued for 45 min to obtain solution B-2;

[0084] 3000 parts by weight of a 5% concentration sodium bicarbonate aqueous solution are provided, and stirring (500 r / min) is kept, and solution A-2, solution B-2, 15 parts by weight of a complexing agent potassium sodium tartrate, and 6 parts by weight of a stabilizer ammonium acetate are added to obtain an intermediate product solution;

[0085] The intermediate product solution is concentrated and dried to obtain 163 parts by weight of an intermediate product solid; 45 parts by weight of polyethyleneimine is dissolved in 300 parts by weight of DMF, and the aforementioned intermediate product solid is added under the protection of nitrogen, and reaction is carried out at 70°C for 5h, and then washing, rotary evaporation, and drying are carried out to obtain the environmentally friendly liquid disperse dye solid of Example Two.

[0086] Comparative Example One

[0087] comprising the following steps:

[0088] 1. Preparation of Caragana extract:

[0089] Providing Caragana, washing Caragana with water, drying at 60℃, passing through a 50-mesh sieve to obtain Caragana powder; preparing an aqueous acetone solution, wherein the volume fraction of acetone is selected from 50%; under the condition that the solid-liquid ratio is selected from 25:1, adding Caragana powder into the aqueous acetone solution, then refluxing at 65℃ for 2.5h, repeating the extraction for 3 times to obtain an aqueous Caragana extract solution; filtering, concentrating, freeze-drying the aqueous Caragana extract solution to obtain Caragana extract. The above steps are appropriately repeated to obtain sufficient product for the following reaction.

[0090] 2. Preparation of dye:

[0091] Taking 100 parts by weight of Caragana extract, dissolving in 1600 parts by weight of water, adding glacial acetic acid to control the pH value to 2.6 to obtain solution A-1; keeping solution A-1 in stirring state (500 r / min), adding 35 parts by weight of aluminum hydroxide, continuing to stir for 45 min after the completion of addition to obtain solution A-2;

[0092] Providing 3000 parts by weight of 5% concentration of sodium bicarbonate aqueous solution, keeping stirring (500 r / min), adding solution A-2, 15 parts by weight of complexing agent potassium sodium tartrate, 6 parts by weight of stabilizer ammonium acetate to obtain intermediate product solution;

[0093] Concentrating and drying the intermediate product solution to obtain 87 parts by weight of intermediate product solid; dissolving 18 parts by weight of polyethyleneimine in 120 parts by weight of DMF, adding the aforementioned intermediate product solid under the protection of nitrogen, reacting at 70℃ for 5h, then washing, rotary evaporation and drying to obtain the solid of the environmentally friendly liquid disperse dye of Comparative Example One.

[0094] Comparative Example Two

[0095] Comprising the following steps:

[0096] 1. Preparation of Ginkgo biloba extract:

[0097] Providing Ginkgo biloba; washing Ginkgo biloba with water, drying at 60℃, passing through a 30-mesh sieve to obtain Ginkgo biloba powder; preparing a eutectic solvent (the eutectic solvent contains acetylcholine and urea, wherein the molar ratio of acetylcholine and urea is selected from 1.5:1; the mass percentage of the mass sum of acetylcholine and lactic acid based on the total mass of the eutectic solvent is selected from 30%); adding Ginkgo biloba powder into the eutectic solvent, heating and stirring at 45℃ for 4h to obtain an aqueous Ginkgo biloba extract solution; filtering, concentrating, freeze-drying the aqueous Ginkgo biloba extract solution to obtain Ginkgo biloba extract. The above steps are appropriately repeated to obtain sufficient product for the following reaction.

[0098] 2. Preparation of dye:

[0099] Take 25 parts by weight of Ginkgo biloba extract, dissolve in 625 parts by weight of water, add maleic anhydride, adjust the pH value to 4.3, to obtain solution B-1; keep solution B-1 in stirring state (500 r / min), add 5 parts by weight of aluminum hydroxide to it, continue stirring for 45 min after the addition is completed, to obtain solution B-2;

[0100] Provide 3000 parts by weight of 5% concentration sodium bicarbonate aqueous solution, keep stirring (500 r / min), add solution B-2, 15 parts by weight of complexing agent potassium sodium tartrate, 6 parts by weight of stabilizer ammonium acetate, to obtain intermediate product solution;

[0101] Concentrate and dry the intermediate product solution to obtain 21 parts by weight of intermediate product solid; dissolve 12 parts by weight of polyethyleneimine in 50 parts by weight of DMF, under the protection of nitrogen, add the aforementioned intermediate product solid, react at 70°C for 5 h, then wash, rotary evaporate and dry to obtain the environmental-friendly liquid disperse dye solid of Comparative Example Two.

[0102] Color characteristic value test:

[0103] Prepare solutions of the products of Examples One to Two and Comparative Examples One to Two, put them into dyeing kettles, accurately take 5 g of cotton fabric into the dyeing liquor, and dye according to a dyeing depth of 2% (omf).

[0104] Determine the rubbing fastness of the dyed cotton fabric according to GB / T 3920-2008 "Textiles-Color Fastness Tests-Rubbing Color Fastness"; determine the washing fastness of the dyed cotton fabric according to GB / T 3921-2008 "Textiles-Color Fastness Tests-Soaping Color Fastness"; determine the light fastness of the dyed cotton fabric according to AATCC 16.3-2012 "Light Fastness: Xenon Arc Lamp"; wherein the washing fastness, rubbing fastness and light fastness of Example One are all grade 4.

[0105] Determine the color data (CIE Lab values, lightness value , red-green color light , yellow-blue color light , saturation , hue angle h°) of the dyed fabric by Datacolor SF600 colorimeter. The test light source is D 65, and the field angle is 10°. The dyed cotton fabric is measured 4 times, and the average value is taken. The specific values are shown in Table 1.

[0106] Table 1

[0107]

[0108] As can be seen from Table 1, Comparative Example 1 and Comparative Example 2 do not form orange dyes, while Example 1 and Example 2 form orange shades with high saturation.

[0109] Other embodiments of the application will be apparent to those skilled in the art from consideration of the specification and practice of the application disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the application being indicated by the following claims.

Claims

1. An ultra-low pollution, environment-friendly orange dye, characterized in that, The environment-friendly orange dye is prepared by the following steps: Step 1: preparing a caragana extract; The caragana extract is prepared by the following steps: Step 1-1: providing caragana; after washing, drying and sieving, caragana powder is obtained; Step 1-2: preparing an acetone aqueous solution, wherein the volume fraction of acetone is selected from 30%-60%; under the condition that the solid-liquid ratio is selected from (20-30):1, the caragana powder is added to the acetone aqueous solution, and then reflux extraction is carried out at 60-70 DEG C for 2-3h, and the extraction is repeated for 2-4 times to obtain a caragana extract aqueous solution; Step 1-3: the caragana aqueous solution is filtered, concentrated and freeze-dried to obtain the caragana extract; Step 2: dissolving the caragana extract in water, adding glacial acetic acid to control the pH value to 2-3, keeping stirring, adding aluminum hydroxide thereto, continuing to stir for 0.5-1h after the addition is completed to obtain a first mixed solution; Step 3: preparing a ginkgo leaf extract; The ginkgo leaf extract is prepared by the following steps: Step 3-1: providing ginkgo leaves; after washing, drying and sieving, ginkgo leaf powder is obtained; Step 3-2: preparing a deep eutectic solvent; the deep eutectic solvent contains acetylcholine and urea, wherein the molar ratio of the acetylcholine and urea is selected from (1-2):1; the mass percentage of the mass sum of the acetylcholine and lactic acid in the total mass of the deep eutectic solvent is selected from 25%-50%; Step 3-3: adding the ginkgo leaf powder to the deep eutectic solvent, heating and stirring at 40-50 DEG C for 3-5h to obtain a ginkgo leaf extract aqueous solution; Step 3-4: filtering, concentrating and freeze-drying the ginkgo leaf extract aqueous solution to obtain the ginkgo leaf extract; Step 4: dissolving the ginkgo leaf extract in water, adding maleic anhydride to control the pH value to 4-5, keeping stirring, adding aluminum hydroxide thereto, continuing to stir for 0.5-1h after the addition is completed to obtain a second mixed solution; Step 5: providing a sodium bicarbonate aqueous solution, keeping stirring, adding the first mixed solution, the second mixed solution, a complexing agent and a stabilizer to obtain an intermediate product solution; Step 6: concentrating and drying the intermediate product solution to obtain an intermediate product solid; Step 7: providing an organic solution containing polyethyleneimine, under the protection of nitrogen, adding the intermediate product solid, reacting at 60-70 DEG C for 4-6h, and then washing, rotary evaporating and drying to obtain an environment-friendly orange dye solid.

2. The environment-friendly orange dye according to claim 1, characterized in that, Step 2 includes: Step 2-1: dissolving the caragana extract in 15-20 times the mass of water, adding glacial acetic acid to control the pH value to 2.2-2.7; obtaining a step 2-1 solution; Step 2-2: keeping the step 2-1 solution under stirring, the stirring rate is selected from 200-600r / min, adding aluminum hydroxide thereto, continuing to stir for 30-45min after the addition is completed to obtain a first mixed solution; wherein the mass ratio of the caragana extract and aluminum hydroxide is selected from 1:(0.25-0.5).

3. The environment-friendly orange dye according to claim 2, characterized in that, Step 4 includes: Step 4-1: dissolve the ginkgo biloba extract in 20-30 times mass of water, add maleic anhydride, and adjust the pH value to 4.2-4.7; obtain the solution of step 4-1; wherein the mass ratio of the ginkgo biloba extract and the caragana extract used in step 2-1 is selected from (0.15-0.2):1; Step 4-2: keep the solution of step 4-1 in a stirring state, the stirring rate is selected from 200-600 r / min, add aluminum hydroxide thereto, continue stirring for 30-45 min after the addition is completed, and obtain a second mixed solution; wherein the mass ratio of the ginkgo biloba extract and the aluminum hydroxide is selected from 1:(0.15-0.35).

4. The environment-friendly orange dye according to claim 1, characterized in that, The stabilizer is selected from boric acid, ammonium acetate, tartaric acid or potassium hydrogen phthalate; the complexing agent is selected from potassium sodium tartrate, ethylenediaminetetraacetic acid, sodium polyphosphate or sodium citrate.

5. The environment-friendly orange dye according to claim 3, characterized in that, Step 5 includes: Step 5-1: provide a 5% concentration of sodium bicarbonate aqueous solution, keep stirring, the stirring rate is selected from 200-600 r / min, add the first mixed solution, the second mixed solution, the complexing agent and the stabilizer, and obtain an intermediate product solution.

6. The environment-friendly orange dye according to claim 2 or 4, characterized in that, The mass of the stabilizer is selected from 5%-20% of the caragana extract; the mass of the complexing agent is selected from 10%-20% of the caragana extract.

7. The environment-friendly orange dye according to claim 1, characterized in that, The mass ratio of the polyethyleneimine and the intermediate product solid is selected from (0.15-0.35):1.

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