High temperature antioxidant textile fiber adjunct

Abstract

The application relates to the field of textile fiber treatment, in particular to a high-temperature antioxidant textile fiber auxiliary agent; the textile fiber auxiliary agent comprises the following components in parts by weight: 50-75 parts by weight of a basic auxiliary agent, 15-35 parts by weight of a first mixed additive and 20-35 parts by weight of a second mixed additive; the first mixed additive comprises 5-10 parts by weight of an antioxidant, 5-10 parts by weight of an ultraviolet absorber, 2-5 parts by weight of a light stabilizer and 3-10 parts by weight of an antistatic agent; and the second mixed additive comprises 5-10 parts by weight of a defoaming agent, 10-20 parts by weight of a dispersing agent, 1-5 parts by weight of a leveling agent and 3-7 parts by weight of a surface tension auxiliary agent. The prepared textile fiber auxiliary agent can make the textile fabric have better antioxidant effect at a higher temperature, and also has the effect of long-acting anti-ultraviolet aging.

Description

Technical Field

[0001] This invention relates to the field of textile fiber treatment, specifically to a high-temperature antioxidant textile fiber auxiliary agent. Background Technology

[0002] Textile auxiliaries are essential chemicals in the production and processing of textiles. They play an indispensable role in improving the quality and added value of textile products. They not only endow textiles with various special functions and styles, such as softness, wrinkle resistance, shrinkage resistance, water resistance, antibacterial properties, antistatic properties, and flame retardancy, but also improve dyeing and finishing processes, saving energy and reducing processing costs. Textile auxiliaries are crucial for improving the overall level of the textile industry and their role in the textile supply chain. Existing textile auxiliaries mainly include scouring agents, dyeing agents, leveling agents, softeners, wool effect enhancers, polyester low-temperature dyeing carriers, alkali substitutes, CT powder, chemical fiber oils, high-efficiency desiccant powder, hydrogen peroxide stabilizers, silicone removers, foaming agents, raising agents, and color-fixing agents. However, the effects of existing textile auxiliaries are relatively limited.

[0003] Therefore, a high-temperature antioxidant textile fiber auxiliary agent is proposed. Products treated with this agent have good antioxidant effects at higher temperatures and also have anti-ultraviolet aging effects. Summary of the Invention

[0004] This invention provides a high-temperature antioxidant textile fiber auxiliary agent to address the shortcomings of related technologies.

[0005] To achieve the above objectives, the present invention provides the following technical solution:

[0006] According to a first aspect of the present disclosure, a high-temperature antioxidant textile fiber auxiliary agent is provided, the textile fiber auxiliary agent comprising the following components in parts by weight:

[0007] 50-75 parts by weight of basic additive, 15-35 parts by weight of first mixed additive and 20-35 parts by weight of second mixed additive.

[0008] In one aspect of this disclosure, preferably, the textile fiber auxiliary agent comprises the following components in parts by weight:

[0009] 55-65 parts by weight of basic additive, 18-22 parts by weight of first mixed additive and 22-28 parts by weight of second mixed additive.

[0010] In one aspect of this disclosure, the textile fiber auxiliary agent specifically comprises the following components in parts by weight:

[0011] 55 parts by weight of the base additive, 20 parts by weight of the first mixed additive and 25 parts by weight of the second mixed additive.

[0012] In one aspect of this disclosure, the first mixed additive comprises the following components in parts by weight:

[0013] 5-10 parts by weight of antioxidant, 5-10 parts by weight of UV absorber, 2-5 parts by weight of light stabilizer and 3-10 parts by weight of antistatic agent.

[0014] In one aspect of this disclosure, specifically, the first mixed additive comprises the following components in parts by weight:

[0015] 6 parts by weight of antioxidant, 6 parts by weight of UV absorber, 3 parts by weight of light stabilizer and 5 parts by weight of antistatic agent.

[0016] In one aspect of the present disclosure, the base adjuvant is selected from at least one of isooctyl palmitate, isooctyl stearate, and isooctyl oleate.

[0017] In one aspect of the embodiments of this disclosure, the base adjuvant comprises isooctyl palmitate, isooctyl stearate, and isooctyl oleate.

[0018] In one aspect of the embodiments of this disclosure, preferably, the base adjuvant comprises 30-40 parts by weight of isooctyl palmitate, 10-15 parts by weight of isooctyl stearate and 10-20 parts by weight of isooctyl oleate.

[0019] In one aspect of the embodiments of this disclosure, specifically, the base adjuvant comprises 32 parts by weight of isooctyl palmitate, 12 parts by weight of isooctyl stearate and 11 parts by weight of isooctyl oleate.

[0020] In one aspect of this disclosure, the antioxidant comprises resveratrol extract and at least one plant oligosaccharide.

[0021] In one aspect of this disclosure, the plant oligosaccharide is selected from osmanthus leaf oligosaccharide, yam oligosaccharide, or soybean oligosaccharide.

[0022] In one aspect of this disclosure, preferably, the plant oligosaccharide is selected from osmanthus leaf oligosaccharide.

[0023] In one aspect of this disclosure, the resveratrol extract is selected from 15%-25% by mass based on the total mass of the antioxidants, with the remainder being plant oligosaccharides.

[0024] In one aspect of this disclosure, the resveratrol extract is prepared by the following steps:

[0025] Step 1-a: Provide grape pomace raw material; wash and dry the grape pomace, then pass it through a 40-60 mesh sieve to obtain grape pomace dry powder;

[0026] Step 2-a: Add the grape pomace powder to a 60% ethanol aqueous solution, then add cellulase, adjust the pH to 4.5-5.5, heat to 50℃-60℃ and sonicate for 1-1.5h to obtain a mixed solution;

[0027] Step 3-a: After centrifuging the mixed solution obtained in step 2-a, take the supernatant. After evaporating and concentrating the supernatant, obtain a solid. Then dissolve the solid in methanol and purify it through an organic filter membrane. After evaporating and concentrating again, obtain the resveratrol extract.

[0028] In one aspect of this disclosure, specifically, the resveratrol extract is prepared by the following steps:

[0029] Step 1-a: Provide grape pomace raw material; wash and dry the grape pomace, then pass it through a 60-mesh sieve to obtain grape pomace dry powder;

[0030] Step 2-a: Add the grape pomace powder to 5 times its mass of 60% ethanol aqueous solution, then add cellulase, adjust the pH to 4.8, and then add to an ultrasonic water bath. Heat to 50°C and sonicate for 1.5 hours (ultrasonic power: 40kHz) to obtain a mixed solution; the mass of the added cellulase is 0.25%-0.5% of the mass of the grape pomace powder.

[0031] Step 3-a: After centrifuging the mixed solution obtained in step 2-a (4000 r / min, 5 min), the supernatant is collected. The supernatant is then evaporated and concentrated at 60 °C to obtain a solid. The solid is then dissolved in 4 times its mass of methanol and purified through an organic filter membrane (0.22 μm). After further evaporation and concentration at 60 °C, the resveratrol extract is obtained.

[0032] In one aspect of this disclosure, the plant oligosaccharide is selected from osmanthus leaf oligosaccharide; the osmanthus leaf oligosaccharide is prepared through the following steps:

[0033] Step 1-b: Provide osmanthus leaf raw material; wash and dry the osmanthus leaf raw material, and then pass it through an 80-100 mesh sieve to obtain osmanthus leaf powder;

[0034] Step 2-b: The dried osmanthus leaf powder is subjected to defatting and deproteinization processes to obtain defatted and deproteinized osmanthus leaf extract;

[0035] Step 3-b: Add the defatted and deproteinized osmanthus leaf extract to 8-12 times its weight of 80% ethanol aqueous solution for reflux extraction. The reflux extraction temperature is selected from 60℃-70℃, the reflux extraction time is selected from 1.5-2h, and the number of reflux extractions is selected from 2-3 times. After the reflux extraction is completed, collect the solid.

[0036] Step 4-b: Add 5-8 times the mass of water to the solid obtained in step 3-b and decoct for extraction. The decoction temperature is selected from 90℃-100℃, the decoction time is selected from 1-2 hours, and the number of decoctions is selected from 2-3 times. After the decoction is completed, filter and collect the aqueous extract.

[0037] Step 5-b: Concentrate the aqueous extract obtained in step 4-b to 1 / 3 of its original volume, then add 80% ethanol until the ethanol concentration in the mixed solution is 60%. After centrifugation, the resulting mixed solution is used to obtain a precipitate and a supernatant. The precipitate is collected and washed to obtain Osmanthus leaf polysaccharide.

[0038] Step 6-b: Dissolve the osmanthus leaf polysaccharide in water, add a compound enzyme for enzymatic hydrolysis, and after the enzymatic hydrolysis process is completed, collect the precipitate after enzyme inactivation, concentration, alcohol precipitation, and centrifugation to obtain the osmanthus leaf oligosaccharide; wherein, the compound enzyme includes cellulase and glucanase.

[0039] In one aspect of the embodiments of this disclosure, in step 2-b, the defatting process is as follows: the dried osmanthus leaf powder is wrapped in filter paper, placed in a Soxhlet extractor, petroleum ether is added, and the mixture is refluxed at 50℃-60℃ for 2-4 hours to obtain defatted osmanthus leaf extract.

[0040] In one aspect of this disclosure, in step 2-b, the deproteinization process is as follows: the defatted osmanthus leaf extract is added to water, the pH is adjusted to 5-6, then papain is added, and deproteinization is carried out at 55℃-65℃. After deproteinization, the enzyme is inactivated to obtain the defatted and deproteinized osmanthus leaf extract; wherein, the deproteinization time is selected from 1-2 hours, and the amount of papain used is 50-150 U / mg.

[0041] In one aspect of this disclosure, specifically, the osmanthus leaf oligosaccharide is prepared by the following steps:

[0042] Step 1-b: Provide osmanthus leaf raw material; wash and dry the osmanthus leaf raw material, and then pass it through an 80-mesh sieve to obtain osmanthus leaf powder;

[0043] Step 2-b: Wrap the dried osmanthus leaf powder in filter paper, place it in a Soxhlet extractor, add petroleum ether, and reflux at 60°C for 3 hours to obtain defatted osmanthus leaf extract; add the defatted osmanthus leaf extract to water, adjust the pH to 5.2, then add papain, and deproteinize at 60°C. After deproteinization, inactivate the enzyme to obtain defatted and deproteinized osmanthus leaf extract; wherein, the deproteinization time is 1.5 hours, and the amount of papain used is 120 U / mg;

[0044] Step 3-b: Add the defatted and deproteinized osmanthus leaf extract to 10 times its weight of 80% ethanol aqueous solution and reflux extract. The reflux extraction temperature is selected from 65℃, the reflux extraction time is selected from 1.8h, and the reflux extraction is performed 3 times. After the reflux extraction is completed, collect the solid.

[0045] Step 4-b: Add 6 times the mass of water to the solid obtained in step 3-b and decoct for extraction. The decoction temperature is 98℃, the decoction time is 1.2h, and the number of decoctions is 2. After the decoction is completed, filter and collect the aqueous extract.

[0046] Step 5-b: Concentrate the aqueous extract obtained in step 4-b to 1 / 3 of its original volume, then add 80% ethanol until the ethanol concentration in the mixed solution is 60%. After centrifugation, the resulting mixed solution is used to obtain a precipitate and a supernatant. The precipitate is collected and washed to obtain Osmanthus leaf polysaccharide.

[0047] Step 6-b: Dissolve the osmanthus leaf polysaccharide in water, add a compound enzyme for enzymatic hydrolysis, and after the enzymatic hydrolysis process is completed, collect the precipitate after enzyme inactivation, concentration, alcohol precipitation, and centrifugation to obtain the osmanthus leaf oligosaccharide; wherein, the compound enzyme includes cellulase and glucanase, the mass ratio of cellulase to glucanase is 1:1, and the amount of compound enzyme used is 100U / mg.

[0048] In one aspect of this disclosure, the ultraviolet absorber is prepared by the following steps:

[0049] Step 1-c: Prepare compound 1, the structural formula of which is shown below:

[0050]

[0051] Step 2-c: Dissolve compound 1 in an organic solvent, protect it with an inert gas, then add polyethyleneimine, and react at 70℃-80℃ for 5-7 hours to obtain the ultraviolet absorber.

[0052] In one aspect of this disclosure, the organic solvent is DMF.

[0053] In one aspect of this disclosure, compound 1 is prepared by the following steps:

[0054] Step 1-d: Epichlorohydrin is prepared by Finkelstein reaction using epichlorohydrin as a raw material;

[0055]

[0056] Step 2-d: Using 2,3,3-trimethyl-3H-indole as a starting material, intermediate product 1 is generated through an N-alkylation reaction;

[0057]

[0058] Step 3-d: Intermediate 1 and 2,5-dihydroxybenzaldehyde were reacted under reflux in anhydrous ethanol in the presence of triethylamine to prepare compound 1;

[0059]

[0060] In one aspect of this disclosure, in step 2-c, polyethyleneimine undergoes a grafting reaction with compound 1 to obtain an ultraviolet absorber having the following structure:

[0061] .

[0062] In one aspect of the embodiments of this disclosure, the light stabilizer is selected from N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phenylenediamide, dimethyl succinate and a polymer of 4-hydroxy-2,2,6,6-tetramethyl-1-piperidinol or [[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methyl]butylmalonate di(1,2,2,6,6-pentamethyl-4-piperidinyl) ester.

[0063] In one aspect of this disclosure, specifically, the light stabilizer is selected from N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phenylenediamide, which has the following structural formula:

[0064]

[0065] In one aspect of this disclosure, the antistatic agent is selected from at least one of phosphate esters, polyethylene glycol esters, polyols, quaternary ammonium compounds, polysiloxanes, polyol amines, and polyvinyl chloride derivatives.

[0066] In one aspect of this disclosure, specifically, the antistatic agent is selected from hexadecyltrimethylammonium chloride.

[0067] In one aspect of this disclosure, the second mixed additive comprises at least two of an antifoaming agent, a dispersant, a leveling agent, and a surface tension enhancer.

[0068] In one aspect of the embodiments of this disclosure, preferably, the second mixed additive comprises an antifoaming agent, a dispersant, a leveling agent, and a surface tension enhancer; more preferably, the second mixed additive comprises 5-10 parts by weight of an antifoaming agent, 10-20 parts by weight of a dispersant, 1-5 parts by weight of a leveling agent, and 3-7 parts by weight of a surface tension enhancer.

[0069] In one aspect of the embodiments of this disclosure, specifically, the second mixed additive comprises 7 parts by weight of defoamer, 12 parts by weight of dispersant, 2 parts by weight of leveling agent and 4 parts by weight of surface tension enhancer.

[0070] In one aspect of the embodiments of this disclosure, the defoamer is selected from one or more of tributyl phosphate, defoamer Deqian 3100, and defoamer BYK088; but is not limited thereto. Specifically, the defoamer is selected from tributyl phosphate.

[0071] In one aspect of this disclosure, the dispersant is selected from polycarboxylate dispersant 5040 or sodium hexametaphosphate; however, it is not limited thereto. Specifically, the dispersant is selected from sodium hexametaphosphate.

[0072] In one aspect of this disclosure, the leveling agent is selected from leveling agent BYK-333 or silicone leveling agent HY-5030; however, it is not limited thereto. Specifically, the leveling agent is selected from BYK-333.

[0073] In one aspect of this disclosure, the surface tension aid is selected from polysiloxane-polyalkoxy polyether copolymers.

[0074] Compared with the prior art, the beneficial effects of the present invention are: a textile fiber auxiliary agent that can enable textiles to have good antioxidant effect at higher temperatures and also has a long-lasting anti-ultraviolet aging effect. Detailed Implementation

[0075] To make the objectives, technical solutions, and advantages of this application clearer, the technical solutions of this application will be clearly and completely described below in conjunction with embodiments. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. The embodiments described herein are illustrative in nature and are used to provide a basic understanding of this application. The embodiments of this application should not be construed as limiting this application.

[0076] For the sake of brevity, this article only discloses a few specific numerical ranges. However, any lower limit can be combined with any upper limit to form an unspecified range; and any lower limit can be combined with other lower limits to form an unspecified range, just as any upper limit can be combined with any other upper limit to form an unspecified range. Furthermore, each individually disclosed point or single value can itself serve as a lower or upper limit and be combined with any other point or single value or with other lower or upper limits to form an unspecified range.

[0077] In this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0078] In this description, unless otherwise stated, "above" and "below" include the stated number.

[0079] Unless otherwise stated, the terms used in this disclosure have their common meanings as commonly understood by those skilled in the art. Unless otherwise stated, the values ​​of the parameters mentioned in this disclosure can be measured using various measurement methods commonly used in the art (e.g., they can be tested according to the methods given in the embodiments of this disclosure).

[0080] The term "about" is used to describe and indicate small variations. When used in conjunction with an event or situation, the term may refer to examples in which the event or situation occurred precisely or in examples in which the event or situation occurred very approximately. For example, when used in conjunction with numerical values, the term may refer to a range of variation 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 in range format herein. It should be understood that such range format is for convenience and brevity and should be interpreted flexibly to include not only numerical values ​​explicitly specified as range limits but also all individual numerical values ​​or subranges covered within the range, as if each numerical value and subrange were explicitly specified.

[0081] The list of items connected by the terms "at least one of," "at least one of," "at least one of," or other similar terms can mean any combination of the listed items. For example, if items A and B are listed, then the phrase "at least one of A and B" means only A; only B; or A and B. In another instance, if items A, B, and C are listed, then 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 may contain a single component or multiple components. Item B may contain a single component or multiple components. Item C may contain a single component or multiple components.

[0082] The present disclosure is further illustrated below with reference to embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the disclosure.

[0083] Examples and comparative examples:

[0084] Example 1

[0085] Example 1 includes the following steps:

[0086] 1. Compound 1 was prepared according to the method described above:

[0087]

[0088] Add 50g of KI and 300mL of acetone to a round-bottom flask, then add an appropriate amount of boiling chips; weigh out 18.5g (200mmol) of epichlorohydrin for later use, then set up a reflux condenser, using an oil bath as a heat source and connecting it to cooling water; turn on the oil bath and set the temperature to 50℃. When the oil bath temperature stabilizes at around 50℃, add epichlorohydrin to the end of the dropping funnel, then open the dropping funnel and slowly add epichlorohydrin dropwise to the reaction mixture. After the addition is complete, continue the reflux reaction operation, maintaining the temperature at around 50℃, and continue the reaction for 2 hours. Then, after washing, extraction, and rotary evaporation, the obtained product, epichlorohydrin, is directly used in the next reaction step.

[0089] Weigh 120 mmol of the previously prepared epichlorohydrin and 100 mmol of 2,3,3-trimethyl-3H-indole. First, add 2,3,3-trimethyl-3H-indole and 3.6 g of sodium hydroxide to a three-necked flask, then add 200 mL of methanol and stir until homogeneous. Then, fix the three-necked flask on an electric stirrer, install the condenser and dropping funnel, turn on the electric stirrer, and heat the reaction mixture to 40 °C. Then, add the epichlorohydrin to the dropping funnel and slowly add it dropwise to the reaction mixture. After the addition is complete, continue the reflux reaction for 3.5 h. Then, after washing, extraction, rotary evaporation and purification, collect the obtained intermediate product 1 and use it for the next reaction.

[0090] 100 mmol of 2,5-dihydroxybenzaldehyde was weighed into a round-bottom flask. 150 mL of anhydrous ethanol and 15 mL of triethylamine were added. 80 mmol of the intermediate product 1 prepared earlier was weighed and added to the reaction mixture under stirring. The reaction was allowed to proceed for 2 h to obtain compound 1. ¹H NMR: δ 1.26–1.36 (6H, 1.31 (s), 1.31 (s)), 3.06 (2H,dd, J = 7.9, 4.3 Hz), 3.17–3.35 (3H, 3.22 (d, J = 5.1 Hz), 3.27 (ddt, J = 8.1, 7.7, 5.1 Hz)), 6.30 (1H, d, J = 9.7 Hz), 6.52–6.86 (4H, 6.58 (td, J = 7.6, 1.1 Hz), 6.60 (ddd, J = 7.8, 1.1, 0.4 Hz), 6.72 (dd, J = 8.6, 0.5 Hz), 6.80 (dd, J = 8.6, 2.9 Hz)), 6.87-7.25 (4H, 6.95 (ddd, J = 7.8, 7.6, 1.5 Hz), 7.00 (ddd, J = 7.6, 1.5, 0.4 Hz), 7.11 (dd, J = 2.9, 0.5 Hz), 7.19 (d, J =9.7 Hz)).

[0091] 2. Preparation of ultraviolet absorbers:

[0092] 50 mmol of compound 1 was weighed into 150 mL of DMF and protected with an inert gas. Then 25 mL of polyethyleneimine was added, and the mixture was reacted at 75 °C for 6 h. After separation and purification, the UV absorber of Example 1 was obtained.

[0093] 3. Preparation of antioxidants:

[0094] Grape pomace raw material is provided; the grape pomace is washed, dried, and then passed through a 60-mesh sieve to obtain grape pomace dry powder; the grape pomace dry powder is added to 5 times its mass of 60% ethanol aqueous solution, then cellulase is added, the pH is adjusted to 4.8, and then added to an ultrasonic water bath, heated to 50℃ and ultrasonicated for 1.5h (ultrasonic power: 40kHz) to obtain a mixed solution; the mass of cellulase added is 0.25%-0.5% of the mass of grape pomace dry powder; the obtained mixed solution is centrifuged (4000r / min, 5min), and the supernatant is collected. The supernatant is evaporated and concentrated at 60℃ to obtain a solid, then the solid is dissolved in 4 times its mass of methanol and purified through an organic filter membrane (0.22μm), and then evaporated and concentrated at 60℃ to obtain resveratrol extract.

[0095] Osmanthus leaf raw material is provided; the osmanthus leaf raw material is washed, dried, and then passed through an 80-mesh sieve to obtain osmanthus leaf powder; the osmanthus leaf powder is wrapped in filter paper, placed in a Soxhlet extractor, petroleum ether is added, and the mixture is refluxed at 60℃ for 3 hours to obtain defatted osmanthus leaf extract; the defatted osmanthus leaf extract is added to water, the pH is adjusted to 5.2, then papain is added, and deproteinization is carried out at 60℃. After deproteinization, the enzyme is inactivated to obtain defatted and deproteinized osmanthus leaf extract; the deproteinization time is 1.5 hours, and the amount of papain used is 120 U / mg; the defatted and deproteinized osmanthus leaf extract is added to 10 times its weight of 80% ethanol aqueous solution, and refluxed for extraction. The reflux extraction temperature is selected from 65℃, the reflux extraction time is selected from 1.8 hours, and the reflux extraction is carried out 3 times; reflux extraction is performed. After extraction, the solid was collected. Six times the mass of water was added to the solid for decoction extraction at 98℃ for 1.2 hours, repeated twice. After extraction, the aqueous extract was collected by filtration. The aqueous extract was concentrated to 1 / 3 of its original volume, and then 80% ethanol was added until the ethanol concentration in the mixed solution was 60%. The mixed solution was then centrifuged to obtain a precipitate and supernatant. The precipitate was collected, washed, and then Osmanthus leaf polysaccharide was obtained. The Osmanthus leaf polysaccharide was dissolved in water, and a complex enzyme (complex enzymes including cellulase and glucanase, with a mass ratio of 1:1 and a dosage of 100 U / mg) was added for enzymatic hydrolysis. After hydrolysis, the enzyme was inactivated, concentrated, precipitated with alcohol, centrifuged, and the precipitate was collected to obtain Osmanthus leaf oligosaccharide.

[0096] The obtained resveratrol extract and osmanthus leaf oligosaccharide were formulated into the antioxidant of Example 1 at a mass ratio of 15:85.

[0097] 4. Preparation of textile fiber auxiliaries:

[0098] Weigh 32 parts by weight of isooctyl palmitate, 12 parts by weight of isooctyl stearate, and 11 parts by weight of isooctyl oleate as basic additives; weigh 6 parts by weight of the antioxidant prepared above, 6 parts by weight of the ultraviolet absorber prepared above, 3 parts by weight of the light stabilizer N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phenylenediamide, 5 parts by weight of the antistatic agent hexadecyltrimethylammonium chloride, 7 parts by weight of the defoamer tributyl phosphate, 12 parts by weight of the dispersant sodium hexametaphosphate, 2 parts by weight of the leveling agent BYK-333, and 4 parts by weight of the surface tension enhancer polysiloxane-polyalkoxy polyether copolymer; mix all the above compounds thoroughly to obtain the product of Example 1.

[0099] Example 2

[0100] The steps in Example 2 are the same as in Example 1, except that 5-hydroxy-2-nitrobenzaldehyde is used in Example 2 instead of 2,5-dihydroxybenzaldehyde used in Example 1; and the compound obtained in Example 2 is compound 2 having the following structure instead of compound 1:

[0101]

[0102] Example 3

[0103] The steps in Example 3 are the same as those in Example 1. The difference is that in Example 3, polyethyleneimine is not used to perform a grafting reaction with compound 1. Instead, compound 1 is used directly as an ultraviolet absorber.

[0104] Example 4

[0105] The steps in Example 4 are the same as those in Example 1, except that Example 4 does not include the step of preparing resveratrol extract, but instead uses 5 parts by weight of osmanthus leaf oligosaccharide as an antioxidant.

[0106] Example 5

[0107] The steps in Example 5 are the same as those in Example 1, except that Example 5 does not include the step of preparing osmanthus leaf oligosaccharides, but instead uses 1 part by weight of resveratrol extract as an antioxidant.

[0108] Comparative Example 1

[0109] In Comparative Example 1, 32 parts by weight of isooctyl palmitate, 12 parts by weight of isooctyl stearate, and 11 parts by weight of isooctyl oleate were weighed as basic additives; 3 parts by weight of light stabilizer N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phenylenediamide, 5 parts by weight of antistatic agent cetyltrimethylammonium chloride, 7 parts by weight of defoamer tributyl phosphate, 12 parts by weight of dispersant sodium hexametaphosphate, 2 parts by weight of leveling agent BYK-333, and 4 parts by weight of surface tension enhancer polysiloxane-polyalkoxy polyether copolymer were weighed; all the above compounds were thoroughly mixed to obtain the product of Comparative Example 1.

[0110] Comparative Example 1 does not contain the antioxidants and UV absorbers prepared in Example 1.

[0111] High-temperature antioxidant performance and long-lasting UV absorption performance test:

[0112] High-temperature anti-DPPH free radical performance test: Weigh 1 mg of DPPH and dissolve it in 10 mL of ethanol solvent. Store at room temperature in the dark for 60-120 minutes. The optimal absorbance of the solution at 517 nm is 1.2-1.3, which is the DPPH stock solution.

[0113] The products of Examples 1 to 5 and Comparative Example 1 of equal mass were dissolved in an equal volume of ethanol solvent and sealed and stored at 40°C for 24 hours to obtain samples of Examples 1 to 5 and Comparative Example 1 after high-temperature treatment.

[0114] Then, the samples from Examples 1 to 5 and Comparative Example 1, after high-temperature treatment, were mixed with equal masses of DPPH stock solution. After reacting in the dark for 30 minutes, the absorbance of the resulting solution was measured at 517 nm. An equal volume of ethanol solvent was used instead of the product, and the reaction time was the same for the same duration; the absorbance measured was the absorbance of the control group. DPPH free radical scavenging rate (%) = (Absorbance of control group / Absorbance of experimental group) / Absorbance of control group.

[0115] The test results are shown in Table 1 below.

[0116] Long-lasting UV absorption performance test: The products of Examples 1 to 5 and Comparative Example 1 were coated onto aramid 1414 fiber sample fabric at a rate of 50g per square meter. After drying, the UV resistance of the sample fabric after product treatment was tested using a UV-2000F UV transmittance analyzer. Five points were tested, and the instrument automatically calculated the UVA and UVB transmittance of the aramid fiber sample fabric. The sample fabric was then stored indoors for 30 days, and the UVA and UVB transmittance of the aramid fiber sample fabric was tested again. The test results are shown in Table 1 below.

[0117] Table 1:

[0118]

[0119] As can be seen from Table 1, both resveratrol extract and osmanthus leaf oligosaccharides have antioxidant capabilities. By comparing Examples 1 and 4 / 5, it can be seen that the combination of resveratrol extract and osmanthus leaf oligosaccharides is more effective than using them alone. This is because plant oligosaccharides not only have the effect of directly scavenging free radicals, but they are also stable and not easily decomposed or degraded. Furthermore, they can combine with resveratrol extract and protect it at higher temperatures, thus achieving the goal of better combined use.

[0120] Furthermore, since plant oligosaccharides are rich in hydroxyl, aldehyde, and ketone groups, and compound 1 grafted with polyethyleneimine is rich in amine groups, the two cross-link and combine with each other, thereby giving it long-term stability. Therefore, compared with Example 3 without amine grafting and Example 5 without the use of plant oligosaccharides, Example 1 (and Example 4) exhibits excellent long-term UV protection.

[0121] In this disclosure, the principle of the UV protection ability of compound 1 (and the UV absorber obtained through compound 1) is as follows: Under UV irradiation, compound 1 undergoes the following reversible structural change:

[0122]

[0123] This process not only absorbs ultraviolet light, but the hydroquinone group on its right side also has an anti-ultraviolet effect, which is why the ultraviolet absorption capacity of Example 1 is better than that of Example 2.

[0124] Other embodiments of this disclosure will readily occur to those skilled in the art upon consideration of the specification and practice of the disclosure herein. This disclosure is intended to cover any variations, uses, or adaptations of this disclosure that follow the general principles of this disclosure and include common knowledge or customary techniques in the art not disclosed herein.

Claims

1. A high-temperature antioxidant textile fiber auxiliary agent, characterized in that, The textile fiber auxiliary agent comprises the following components in parts by weight: 50-75 parts by weight of basic additives, 15-35 parts by weight of first mixed additives and 20-35 parts by weight of second mixed additives; The first mixed additive comprises the following components in parts by weight: 5-10 parts by weight of antioxidant, 5-10 parts by weight of ultraviolet absorber, 2-5 parts by weight of light stabilizer and 3-10 parts by weight of antistatic agent; The ultraviolet absorber is prepared by the following steps: Step 1-c: Prepare compound 1, the structural formula of which is shown below: Step 2-c: Dissolve compound 1 in an organic solvent, protect it with an inert gas, then add polyethyleneimine, and react at 70℃-80℃ for 5-7 hours to obtain the ultraviolet absorber; The second mixed additive comprises at least two of an antifoaming agent, a dispersant, a leveling agent, and a surface tension enhancer; The basic adjuvant is selected from at least one of isooctyl palmitate, isooctyl stearate, and isooctyl oleate.

2. The high-temperature antioxidant textile fiber auxiliary agent according to claim 1, characterized in that, The antioxidant contains resveratrol extract and at least one plant oligosaccharide.

3. The high-temperature antioxidant textile fiber auxiliary agent according to claim 2, characterized in that, The resveratrol extract was prepared by the following steps: Step 1-a: Provide grape pomace raw material; wash and dry the grape pomace, then pass it through a 40-60 mesh sieve to obtain grape pomace dry powder; Step 2-a: Add the grape pomace powder to a 60% ethanol aqueous solution, then add cellulase, adjust the pH to 4.5-5.5, heat to 50℃-60℃ and sonicate for 1-1.5h to obtain a mixed solution; Step 3-a: After centrifuging the mixed solution obtained in step 2-a, take the supernatant. After evaporating and concentrating the supernatant, obtain a solid. Then dissolve the solid in methanol and purify it through an organic filter membrane. After evaporating and concentrating again, obtain the resveratrol extract.

4. The high-temperature antioxidant textile fiber auxiliary agent according to claim 2, characterized in that, The plant oligosaccharide is selected from osmanthus leaf oligosaccharide; the osmanthus leaf oligosaccharide is prepared through the following steps: Step 1-b: Provide osmanthus leaf raw material; wash and dry the osmanthus leaf raw material, and then pass it through an 80-100 mesh sieve to obtain osmanthus leaf powder; Step 2-b: The dried osmanthus leaf powder is subjected to defatting and deproteinization processes to obtain defatted and deproteinized osmanthus leaf extract; Step 3-b: Add the defatted and deproteinized osmanthus leaf extract to 8-12 times its weight of 80% ethanol aqueous solution for reflux extraction. The reflux extraction temperature is selected from 60℃-70℃, the reflux extraction time is selected from 1.5-2h, and the number of reflux extractions is selected from 2-3 times. After the reflux extraction is completed, collect the solid. Step 4-b: Add 5-8 times the mass of water to the solid obtained in step 3-b and decoct for extraction. The decoction temperature is selected from 90℃-100℃, the decoction time is selected from 1-2 hours, and the number of decoctions is selected from 2-3 times. After the decoction is completed, filter and collect the aqueous extract. Step 5-b: Concentrate the aqueous extract obtained in step 4-b to 1 / 3 of its original volume, then add 80% ethanol until the ethanol concentration in the mixed solution is 60%. After centrifugation, the resulting mixed solution is used to obtain a precipitate and a supernatant. The precipitate is collected and washed to obtain Osmanthus leaf polysaccharide. Step 6-b: Dissolve the osmanthus leaf polysaccharide in water, add a compound enzyme for enzymatic hydrolysis, and after the enzymatic hydrolysis process is completed, collect the precipitate after enzyme inactivation, concentration, alcohol precipitation, and centrifugation to obtain the osmanthus leaf oligosaccharide; wherein, the compound enzyme includes cellulase and glucanase.

5. The high-temperature antioxidant textile fiber auxiliary agent according to claim 1, characterized in that, The light stabilizer is selected from a polymer of N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-phenylenediamide, dimethyl succinate and 4-hydroxy-2,2,6,6-tetramethyl-1-piperidinol or [[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methyl]butylmalonate di(1,2,2,6,6-pentamethyl-4-piperidinyl) ester.

6. The high-temperature antioxidant textile fiber auxiliary agent according to claim 1, characterized in that, The antistatic agent is selected from at least one of phosphate esters, polyethylene glycol esters, polyols, quaternary ammonium compounds, polysiloxanes, polyol amines, and polyvinyl chloride derivatives.

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