Ultralow-pollution environment-friendly liquid disperse dye

Abstract

The invention relates to the technical field of textile printing and dyeing, in particular to an environment-friendly liquid disperse dye with ultralow pollution. The environment-friendly liquid disperse dye is prepared by the following steps: preparing a caragana microphylla extract, dissolving the caragana microphylla extract in an acid solution, and mixing with aluminum hydroxide; preparing a ginkgo biloba extract, dissolving the ginkgo biloba extract in an acidic solution, and mixing with aluminum hydroxide; mixing the two substances with a complexing agent and a stabilizer in a sodium bicarbonate aqueous solution, drying to obtain a solid, and finally reacting the solid with polyethyleneimine to obtain the environment-friendly orange dye with good dispersity.

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 Since the end of the 19th century, due to the rapid development of synthetic dyes, natural dyes have basically withdrawn from the field of fabric dyeing.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 stem epidermis and flowers of dicotyledonous plants, 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: Step 1: preparing a first plant tannin extract; Step 2: dissolving the first plant tannin extract in water, adding acid and / or anhydride to control the pH value to 2-3, keeping stirring, adding aluminum hydroxide thereto, continuing to stir for 0.5-1 h after the addition is completed, and obtaining a first mixed solution; Step 3: preparing a second plant orange ketone extract; Step 4: dissolving the second plant tannin extract in water, adding acid and / or anhydride, adjusting the pH value to 4-5, keeping stirring, adding aluminum hydroxide thereto, continuing stirring for 0.5-1 h after the addition is completed, to obtain a second mixed solution; Step 5: providing an aqueous sodium bicarbonate 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 in which polyethyleneimine is dissolved, under the protection of nitrogen, adding the intermediate product solid, reacting at 60-70℃ for 4-6 h, and then washing, rotary evaporation and drying, to obtain an environmentally friendly liquid disperse dye solid.

[0008] In an aspect of the embodiments of the present disclosure, the first plant tannin extract is selected from a Caragana jubata extract; and the second plant flavone extract is selected from a Ginkgo biloba extract.

[0009] In the present disclosure, the environmentally friendly liquid disperse dye prepared is an orange dye.

[0010] In an aspect of the embodiments of the present disclosure, the Caragana jubata extract is prepared by the following steps: Step 1-1: providing Caragana jubata; washing, drying and sieving the Caragana jubata to obtain Caragana jubata powder; Step 1-2: preparing an aqueous acetone 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, adding the Caragana jubata powder into the aqueous acetone solution, and then refluxing extraction at 60-70℃ for 2-3 h, repeating the extraction for 2-4 times, to obtain an aqueous Caragana jubata extract; Step 1-3: filtering, concentrating and freeze-drying the aqueous Caragana jubata extract, to obtain the Caragana jubata extract.

[0011] In an aspect of the embodiments of the present disclosure, the Caragana jubata extract is prepared by the following steps: Step 1-1: providing Caragana jubata; washing, drying and sieving the Caragana jubata to obtain Caragana jubata powder; 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, adding the Caragana jubata powder into the aqueous acetone solution, and then refluxing extraction at 65℃ for 2.5 h, repeating the extraction for 3 times, to obtain an aqueous Caragana jubata extract; Step 1-3: filtering, concentrating and freeze-drying the aqueous Caragana jubata extract, to obtain the Caragana jubata extract.

[0012] In an aspect of the embodiments of the present disclosure, the ginkgo leaf extract is prepared by the following steps: Step 3-1: providing ginkgo leaves; the ginkgo leaves are washed, dried and sieved to obtain ginkgo leaf powder; Step 3-2: preparing a deep eutectic solvent; the deep eutectic solvent comprises acetylcholine and urea, wherein the molar ratio of the acetylcholine and the urea is selected from 1-2:1; the mass percentage of the mass sum of the acetylcholine and the lactic acid in the total mass of the deep eutectic solvent is selected from 25%-50%; Step 3-3: adding the ginkgo leaf powder into the deep eutectic solvent, heating and stirring at 40-50°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.

[0013] In an aspect of the embodiments of the present disclosure, the ginkgo leaf extract is prepared by the following steps: Step 3-1: providing ginkgo leaves; the ginkgo leaves are washed, dried and sieved to obtain ginkgo leaf powder; Step 3-2: preparing a deep eutectic solvent; the deep eutectic solvent comprises acetylcholine and urea, wherein the molar ratio of the acetylcholine and the urea is selected from 1.5:1; the mass percentage of the mass sum of the acetylcholine and the lactic acid in the total mass of the deep eutectic solvent is selected from 30%; Step 3-3: adding the ginkgo leaf powder into the deep eutectic solvent, heating and stirring at 45°C for 4h 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.

[0014] In an aspect of the embodiments of the present disclosure, step 2 comprises: 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 solution of step 2-1; Step 2-2: keeping the solution of step 2-1 in a stirring state, 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 liquid; wherein the mass ratio of the caragana extract and the aluminum hydroxide is selected from 1:(0.25-0.5).

[0015] In an aspect of the embodiments of the present disclosure, step 2 comprises: Step 2-1: Dissolve the Caragana extract in 16 times the mass of water, add glacial acetic acid to adjust the pH value to 2.6; obtain the solution of step 2-1; 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 stirring for 45 min after the addition is completed, obtain a first mixed solution; wherein the mass ratio of the Caragana extract and aluminum hydroxide is selected from 1:0.35.

[0016] In an aspect of the embodiments of the present disclosure, step 4 comprises: Step 4-1: Dissolve the Ginkgo biloba extract in 20-30 times the mass of water, add maleic anhydride to 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, 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).

[0017] In an aspect of the embodiments of the present disclosure, step 4 comprises: Step 4-1: Dissolve the Ginkgo biloba extract in 25 times the mass of water, add maleic anhydride to adjust 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; Step 4-2: Keep the solution of step 4-1 in a stirring state, the stirring rate is selected from 500 r / min, add aluminum hydroxide thereto, continue stirring for 45 min after the addition is completed, obtain a second mixed solution; wherein the mass ratio of the Ginkgo biloba extract and aluminum hydroxide is selected from 1:0.2.

[0018] 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.

[0019] In an aspect of the embodiments of the present disclosure, step 5 comprises: 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.

[0020] In one 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.

[0021] In one 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.

[0022] The technical solutions provided by the embodiments of the present disclosure can have the following beneficial effects: As can be seen from the above embodiments, the orange dye prepared by the present disclosure has stable color, good dispersibility, and does not use high-pollution and high-toxicity raw materials in the preparation process.

[0023] It should be understood that the foregoing general description and the following detailed description are only exemplary and explanatory, and are not limiting to the present disclosure. DETAILED DESCRIPTION

[0024] 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 only a 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 to the present application.

[0025] For the sake of brevity, only some numerical ranges are specifically disclosed herein. However, any lower limit can be combined with any upper limit to form a range not explicitly recited; and any lower limit can be combined with any other lower limit to form a range not explicitly recited, and likewise any upper limit can be combined with any other upper limit to form a range not explicitly recited. Further, each individual disclosed point or singular number can be combined as a lower limit or an upper limit with any other point or singular number or with other lower limits or upper limits to form a range not explicitly recited.

[0026] In this document, the terms "comprises", "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 include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without more limitations, an element defined by an "comprising" statement does not exclude the existence of additional identical elements in the process, method, article, or apparatus that includes the element.

[0027] In the description herein, "above," "below," contain the number, unless otherwise stated.

[0028] 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 numerical values of the various parameters set forth in the present application can be measured using any of the various measuring methods commonly used in the art (e.g., can be tested according to the methods given in the examples of the present application).

[0029] 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 that is less than or equal to ±10% of the numerical 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 taken as a literal disclosure of all individual values and subranges falling within the range. Any numerical value, however, can inherently contain uncertainty and these include the ± 2 sigma values inherent in the measurement process.

[0030] The phrase "at least one of," "at least one of," "at least one of," or other similar phrases connected to a list of items 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; or 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.

[0031] The present application is further illustrated by the following examples. It is to be understood that these examples are only for the purpose of illustration and are not intended to limit the scope of the present application.

[0032] Examples and Comparative Examples: Example One Comprising the following steps: 1. Preparation of a Hippophae rhamnoides extract: Providing Caragana, washing Caragana with water, drying Caragana at 60℃, and sieving Caragana through a 50-mesh sieve to obtain Caragana powder; preparing an aqueous solution of acetone, 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 solution of acetone, and then refluxing extraction at 65℃ for 2.5h, repeating extraction for 3 times to obtain an aqueous solution of Caragana extract; filtering, concentrating, and freeze-drying the aqueous solution of Caragana to obtain Caragana extract. The above steps are appropriately repeated to obtain sufficient product for the following reaction.

[0033] 2. Preparation of Ginkgo biloba extract: Providing Ginkgo biloba; washing Ginkgo biloba with water, drying Ginkgo biloba at 60℃, and sieving Ginkgo biloba 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 sum of the mass of acetylcholine and the mass of 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 solution of Ginkgo biloba extract; filtering, concentrating, and freeze-drying the aqueous solution of Ginkgo biloba extract to obtain Ginkgo biloba extract. The above steps are appropriately repeated to obtain sufficient product for the following reaction.

[0034] 3. Preparation of dye: Taking 100 parts by weight of Caragana extract, dissolving it in 1600 parts by weight of water, adding glacial acetic acid to adjust the pH value to 2.6 to obtain solution A-1; keeping solution A-1 in a stirring state (500r / min), adding 35 parts by weight of aluminum hydroxide thereto, continuing to stir for 45min after the addition is completed to obtain solution A-2; Taking 25 parts by weight of Ginkgo biloba extract, dissolving it in 625 parts by weight of water, adding maleic anhydride to adjust the pH value to 4.3 to obtain solution B-1; keeping solution B-1 in a stirring state (500r / min), adding 5 parts by weight of aluminum hydroxide thereto, continuing to stir for 45min after the addition is completed to obtain solution B-2; Providing 3000 parts by weight of 5% concentration of sodium bicarbonate aqueous solution, keeping stirring (500r / min), adding solution A-2, 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; Concentrating and drying the intermediate product solution to obtain 113 parts by weight of intermediate product solid; dissolving 36 parts by weight of polyethyleneimine in 200 parts by weight of DMF, adding the aforementioned intermediate product solid under the protection of nitrogen, reacting at 70℃ for 5h, and then washing, rotary evaporation and drying to obtain the environmentally friendly liquid disperse dye solid of example one.

[0035] Example two comprising the steps of: 1. Preparing a Caragana extract: Providing Caragana, washing the Caragana with water, drying the Caragana at 60°C, and sieving the Caragana to obtain Caragana powder; preparing an acetone aqueous solution, wherein the volume fraction of acetone is selected from 50%; adding the Caragana powder to the acetone aqueous solution under the condition that the solid-liquid ratio is selected from 25:1, and then refluxing and extracting the Caragana powder at 65°C for 2.5h, repeating the extraction for 3 times to obtain a Caragana extract aqueous solution; filtering, concentrating, and freeze-drying the Caragana extract aqueous solution to obtain the Caragana extract. The above steps are appropriately repeated to obtain sufficient product for the following reaction.

[0036] 2. Preparing a Ginkgo biloba leaf extract: Providing Ginkgo biloba leaves; washing the Ginkgo biloba leaves with water, drying the Ginkgo biloba leaves at 60°C, and sieving the Ginkgo biloba leaves to obtain Ginkgo biloba leaf powder; preparing a deep eutectic solvent (the deep eutectic solvent contains 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%); adding the Ginkgo biloba leaf powder to the deep eutectic solvent, and heating and stirring at 45°C for 4h to obtain a Ginkgo biloba extract aqueous solution; filtering, concentrating, and freeze-drying the Ginkgo biloba extract aqueous solution to obtain the Ginkgo biloba extract. The above steps are appropriately repeated to obtain sufficient product for the following reaction.

[0037] 3. Preparing a dye: Taking 100 parts by weight of the Caragana extract, dissolving the Caragana extract 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 a stirring state (500r / min), and then adding 35 parts by weight of aluminum hydroxide to solution A-1, and continuing to stir for 45min after the addition is completed to obtain solution A-2; Taking 75 parts by weight of the Ginkgo biloba extract, dissolving the Ginkgo biloba extract in 625 parts by weight of water, adding maleic anhydride to control the pH value to 4.3 to obtain solution B-1; keeping solution B-1 in a stirring state (500r / min), and then adding 15 parts by weight of aluminum hydroxide to solution B-1, and continuing to stir for 45min after the addition is completed to obtain solution B-2; Providing 3000 parts by weight of a 5% concentration sodium bicarbonate aqueous solution, keeping the sodium bicarbonate aqueous solution in a stirring state (500r / min), and then adding 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 to obtain an intermediate product solution; The intermediate product solution was concentrated and dried to obtain 163 parts by weight of intermediate product solids; 45 parts by weight of polyethyleneimine was dissolved in 300 parts by weight of DMF, and the aforementioned intermediate product solids were added under the protection of nitrogen, and reacted at 70°C for 5h, and then washed, rotary evaporated and dried to obtain the environmentally friendly liquid disperse dye solid of Example Two.

[0038] Comparative Example One comprising the following steps: 1. Preparation of Caragana Extract: Caragana was provided, and the Caragana was washed with water, dried at 60°C, and sieved through a 50 mesh sieve to obtain Caragana powder; an aqueous acetone solution was prepared, wherein the volume fraction of acetone was selected from 50%; the Caragana powder was added to the aqueous acetone solution under the condition that the solid-liquid ratio was selected from 25:1, and then refluxed at 65°C for 2.5h, and the extraction was repeated for 3 times to obtain an aqueous Caragana extract solution; the aqueous Caragana extract solution was filtered, concentrated, and freeze-dried to obtain the Caragana extract. The above steps were appropriately repeated to obtain sufficient product for the following reaction.

[0039] 2. Preparation of Dye: 100 parts by weight of Caragana extract was weighed and dissolved in 1600 parts by weight of water, and glacial acetic acid was added to adjust the pH value to 2.6 to obtain solution A-1; solution A-1 was kept under stirring (500r / min), and 35 parts by weight of aluminum hydroxide was added thereto, and after the addition was completed, the stirring was continued for 45min to obtain solution A-2; 3000 parts by weight of a 5% concentration aqueous sodium bicarbonate solution was provided and kept under stirring (500r / min), and solution A-2, 15 parts by weight of complexing agent potassium sodium tartrate, and 6 parts by weight of stabilizer ammonium acetate were added to obtain an intermediate product solution; The intermediate product solution was concentrated and dried to obtain 87 parts by weight of intermediate product solids; 18 parts by weight of polyethyleneimine was dissolved in 120 parts by weight of DMF, and the aforementioned intermediate product solids were added under the protection of nitrogen, and reacted at 70°C for 5h, and then washed, rotary evaporated and dried to obtain the environmentally friendly liquid disperse dye solid of Comparative Example One.

[0040] Comparative Example Two comprising the following steps: 1. Preparation of Ginkgo Biloba Leaf Extract: Ginkgo biloba leaves are provided; the Ginkgo biloba leaves are washed with water, dried at 60°C, and passed through a 30-mesh sieve to obtain Ginkgo biloba leaf powder; a deep eutectic solvent (the deep eutectic solvent contains 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 4 h 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.

[0041] 2. Preparation of a dye: 25 parts by weight of the Ginkgo biloba extract are weighed into 625 parts by weight of water, maleic anhydride is added, and the pH is adjusted to 4.3 to obtain solution B-1; solution B-1 is kept under stirring (500 r / min), 5 parts by weight of aluminum hydroxide is added thereto, and stirring is continued for 45 min after the addition is completed to obtain solution B-2; 3000 parts by weight of a 5% concentration sodium bicarbonate aqueous solution is provided and kept under stirring (500 r / min), solution B-2, 15 parts by weight of a complexing agent potassium sodium tartrate, and 6 parts by weight of a stabilizing agent ammonium acetate are added to obtain an intermediate product solution; The intermediate product solution is concentrated and dried to obtain 21 parts by weight of an intermediate product solid; 12 parts by weight of polyethyleneimine is dissolved in 50 parts by weight of DMF, the aforementioned intermediate product solid is added under the protection of nitrogen, and reaction is carried out at 70°C for 5 h, followed by washing, rotary evaporation, and drying to obtain the environmentally friendly liquid disperse dye solid of Comparative Example Two.

[0042] Color characteristic value test: The products of Examples One to Two and Comparative Examples One to Two are formulated into solutions, which are placed in a dye vat, 5 g of cotton fabric is accurately weighed into the dye liquor, and dyeing is carried out at a dyeing depth of 2% (omf).

[0043] The color fastness to washing, rubbing, and sunlight of the dyed cotton fabric is determined according to GB / T 3920-2008 “Textiles-Color Fastness to Rubbing”, GB / T 3921-2008 “Textiles-Color Fastness to Washing”, and AATCC 16.3-2012 “Color Fastness to Light: Xenon Arc Lamp”, respectively; wherein the color fastness to washing, rubbing, and sunlight of Example One are all Grade 4.

[0044] The color data (CIE Lab values, lightness value L*, red-green color light a*, and blue-yellow color light b*) of the dyed fabric is determined by a Datacolor SF600 colorimeter. , red-green color light , yellow-blue light , saturation , hue angle h°). The test light source was D65, the field of view angle was 10°, the dyed cotton fabric was measured 4 times, and the average value was taken. The specific values are shown in Table 1 below.

[0045] Table 1 As can be seen from Table 1, Comparative Example 1 and Comparative Example 2 cannot form orange dyes, while Example 1 and Example 2 can form orange color with high saturation.

[0046] 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 the true scope and spirit of the application being indicated by the following claims.

Claims

1. An ultra-low pollution environmentally friendly liquid disperse dye, characterized in that, The environmentally friendly liquid disperse dye is prepared through the following steps: Step 1: Preparation of the first plant tannin extract; Step 2: Dissolve the first plant tannin extract in water, add acid and / or acid anhydride to adjust the pH to 2-3, keep stirring, add aluminum hydroxide, and continue stirring for 0.5-1 h after the addition is complete to obtain the first mixture; Step 3: Prepare the second plant citron extract; 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; 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; Step 6: The intermediate product solution is concentrated and dried to obtain the intermediate product solid; 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.

2. The environmentally friendly liquid disperse dye according to claim 1, characterized in that, The first plant tannin extract is selected from Litsea cubeba extract; the second plant orange ketone extract is selected from Ginkgo biloba extract.

3. The environmentally friendly liquid disperse dye according to claim 2, characterized in that, The Caragana extract was prepared through the following steps: Step 1-1: Provide lemon twigs; wash, dry, and sieve the lemon twigs to obtain lemon twig powder; 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. Steps 1-3: The aqueous solution of *Leonurus japonicus* is filtered, concentrated, and freeze-dried to obtain the *Leonurus japonicus* extract.

4. The environmentally friendly liquid disperse dye according to claim 2, characterized in that, The Ginkgo biloba extract was prepared by the following steps: Step 3-1: Provide ginkgo leaves; after washing, drying and sieving the ginkgo leaves, obtain ginkgo leaf powder; Step 3-2: Prepare a eutectic solvent; the eutectic solvent contains acetylcholine and urea, wherein the molar ratio of acetylcholine to urea is selected from (1-2):1; based on the total mass of the eutectic solvent, the mass percentage of acetylcholine and lactic acid is selected from 25%-50%; Step 3-3: Add the ginkgo leaf powder to the eutectic solvent and heat and stir at 40℃-50℃ for 3-5 hours to obtain an aqueous solution of ginkgo leaf extract; Steps 3-4: The aqueous solution of the ginkgo leaf extract is filtered, concentrated, and freeze-dried to obtain the ginkgo leaf extract.

5. The environmentally friendly liquid disperse dye according to claim 2, characterized in that, Step 2 includes: Step 2-1: Dissolve the Caragana korshinskii extract in 15-20 times its weight of water, add glacial acetic acid, and adjust the pH to 2.2-2.7; to obtain the solution from Step 2-1; Step 2-2: Keep the solution from Step 2-1 under stirring at a speed of 200-600 r / min. Add aluminum hydroxide to the solution and continue stirring for 30-45 min after the addition is complete to obtain the first mixture. The mass ratio of the Caragana korshinskii extract to aluminum hydroxide is selected as 1:(0.25-0.5).

6. The environmentally friendly liquid disperse dye according to claim 1 or 5, characterized in that, Step 4 includes: Step 4-1: Dissolve the ginkgo leaf extract in 20-30 times its weight of water, add maleic anhydride, and adjust the pH to 4.2-4.7; to obtain the solution of Step 4-1; wherein, the mass ratio of the ginkgo leaf extract to the caragana extract used in Step 2-1 is selected as (0.15-0.2):1; Step 4-2: Keep the solution from Step 4-1 under stirring at a speed of 200-600 r / min. Add aluminum hydroxide to the solution and continue stirring for 30-45 min after the addition is complete to obtain a second mixture. The mass ratio of the ginkgo leaf extract to aluminum hydroxide is selected as 1:(0.15-0.35).

7. The environmentally friendly liquid disperse 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 sodium potassium tartrate, ethylenediaminetetraacetic acid, sodium polyphosphate, or sodium citrate.

8. The environmentally friendly liquid disperse dye according to claim 6, characterized in that, Step 5 includes: Step 5-1: Provide a 5% sodium bicarbonate aqueous solution, keep stirring at a speed of 200-600 r / min, add the first mixture, the second mixture, the complexing agent, and the stabilizer to obtain an intermediate product solution.

9. The environmentally friendly liquid disperse dye according to claim 5 or 7, characterized in that, The stabilizer is selected from 5%-20% of the Caragana korshinskii extract; the complexing agent is selected from 10%-20% of the Caragana korshinskii extract.

10. The environmentally friendly liquid disperse dye according to claim 1, characterized in that, The mass ratio of the polyethyleneimine to the intermediate solid is selected from (0.15-0.35):1.

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