Preparation methods for and uses of theanine powder, finishing agent and gel for textiles

Abstract

Preparation methods for and the uses of a theanine powder, finishing agent and gel for textiles, relating to the field of textiles. The preparation method for a theanine powder for textiles comprises the following steps: 1) preliminarily obtaining a tea leaf tissue fluid; 2) collecting a tea leaf supernatant; 3) obtaining tea leaf tissue; 4) obtaining a high-purity tea leaf extract; and 5) obtaining the theanine powder. The preparation method for a theanine finishing agent for textiles comprises the following steps: a) obtaining 98% purified theanine powder; and b) obtaining a full-bio-based theanine finishing agent. The obtained theanine powder can be used for preparing the theanine finishing agent or a theanine gel. The theanine finishing agent or theanine gel can be attached to textile fibers or textile fabrics, thereby endowing the textile fibers or the textile fabrics with an antibacterial effect.

Description

Preparation method and application of theanine powder, finishing agent and gel for textiles Technical Field

[0001] The present invention relates to the field of new materials, in particular to textile raw materials. Background Art

[0002] Theanine has antibacterial and antimicrobial effects. If it can be used in the textile field, the textile fabrics prepared with it will surely solve the existing problem of preventing fabrics from easily growing bacteria and producing odors.

[0003] Summary of the Invention

[0004] In order to solve the above-mentioned problems of the prior art, the present invention provides a method for preparing theanine powder for textile use and its application; the present invention also aims to provide a method for preparing theanine finishing agent for textile use and its application; the present invention also aims to provide a method for preparing theanine gel for textile use and its application.

[0005] In order to achieve the above-mentioned purpose, the present invention adopts the following technical solutions:

[0006] A method for preparing theanine powder for textile use, characterized in that it comprises the following steps:

[0007] 1) Preliminary acquisition of tea tissue fluid:

[0008] Putting tea buds and diatomaceous earth into a high-speed stirring barrel in a proportion and stirring at high speed to obtain tea tissue fluid; wherein the mass percentage of tea buds and diatomaceous earth is 90wt%-95wt%:5wt%-10wt%;

[0009] 2) Collecting tea supernatant:

[0010] The tea tissue fluid obtained in step 1) is allowed to stand, and the upper translucent liquid is collected as the tea supernatant;

[0011] 3) Obtaining tea tissue:

[0012] Filtering the tea tissue fluid obtained from the upper translucent liquid in step 2) to remove diatomaceous earth powder precipitate in the tea tissue fluid to obtain tea tissue;

[0013] 4) Obtaining high-purity tea extract:

[0014] injecting ultra-low temperature liquid nitrogen into the tea leaves obtained in step 3), reacting for a period of time, centrifuging, collecting the supernatant, filtering, and concentrating to obtain a high-purity tea leaf extract;

[0015] 5) Obtain theanine powder:

[0016] The high-purity tea extract obtained in step 4) is added with basic copper carbonate, and then extracted, separated and filtered to obtain theanine powder.

[0017] A method for preparing a theanine finishing agent for textiles, characterized by comprising the following steps: a) obtaining 98% purified theanine powder;

[0018] Sulfuric acid is added to theanine powder to adjust the pH of the theanine powder to 4-6, the sulfuric acid reacts with basic copper carbonate to obtain copper theanine salt, and hydrogen sulfide is added to react and precipitate to remove copper ions and reduce theanine powder to obtain 98% purified theanine powder;

[0019] b) Obtaining a fully bio-based theanine finishing agent:

[0020] The tea supernatant and 98% purified theanine powder are mixed and placed in a high-speed stirring barrel for stirring to obtain a fully bio-based theanine finishing agent; wherein the mass percentages of the tea supernatant and the 98% purified theanine powder are 80wt%-90wt% and 10wt%-20wt%.

[0021] A method for preparing theanine gel for textile use, characterized by comprising the following steps:

[0022] First, emulsify 2%-5% ethyl acetate by mass under stirring at 2000-4000 r / min for 20-50 minutes to obtain a solution as the oil phase;

[0023] Then, the seaweed polysaccharide is dissolved in a 1%-1.5% by mass glacial acetic acid solution to prepare a 4%-6% by mass seaweed polysaccharide acetic acid solution, and then a 3%-5% by mass hyaluronic acid solution is added and stirred evenly to form the deionized water phase;

[0024] Then, the deionized water phase is added dropwise into the oil phase, and the emulsification is continued for 20-50 minutes under stirring at 2000-4000 r / min to obtain a deionized water-in-oil emulsion;

[0025] Then, under stirring at 500-800 r / min, the solution containing theanine powder is added dropwise into the deionized water-in-oil emulsion, and reacted at 40-60° C. for 1-2 hours to obtain solution 1;

[0026] Then, the pH value of solution 1 is adjusted to 5-7 with a deionized aqueous sodium carbonate solution with a mass fraction of 1%-2%, solidified for 20-50 minutes, and the precipitate is collected and washed 3-5 times with ethanol without deionized water, and vacuum dried to obtain theanine gel.

[0027] Directions:

[0028] The theanine powder obtained by the invention can be used to prepare theanine finishing agent or theanine gel.

[0029] The theanine finishing agent obtained by the invention can be used to finish textile fibers or textile fabrics, so that the textile fibers or textile fabrics contain theanine and have an antibacterial effect.

[0030] The theanine gel obtained by the invention can be used to repair, fill, and seal gaps or fiber depressions on textile fibers or textile fabrics, thereby preventing theanine on the textile fibers or textile fabrics from falling off easily. DETAILED DESCRIPTION

[0031] In order to better explain the present invention and facilitate understanding, the present invention is described in detail below through specific implementation methods in conjunction with the accompanying drawings.

[0032] The present invention will be further described below by way of examples, the purpose of which is merely to provide a better understanding of the present invention. Therefore, the examples given do not limit the scope of protection of the present invention.

[0033] Example 1:

[0034] The preparation method of theanine finishing agent for textiles comprises the following steps:

[0035] 1) Initially obtain green tea leaf tissue fluid:

[0036] Green tea tree buds and diatomaceous earth are selected, and the two are placed in a high-speed stirring barrel in proportion for high-speed stirring. The mass percentage of the two is 90wt%:10wt%, the net moisture content of the green tea tree buds is between 0.5% and 2%, the stirring speed is 500r / min, the stirring time is 2h, and the stirring temperature is 35°C to obtain tea tissue fluid.

[0037] 2) Collecting tea supernatant:

[0038] The tea tissue fluid obtained in step 1) was allowed to stand for 24 hours at a temperature of 26° C. and a humidity of 95%, and the upper translucent liquid was collected as the tea supernatant;

[0039] 3) Obtaining tea tissue:

[0040] Filtering the tea tissue fluid obtained from the upper translucent liquid in step 2) to remove diatomaceous earth powder precipitate in the tea tissue fluid to obtain tea tissue;

[0041] 4) Obtaining high-purity tea extract:

[0042] The tea leaves obtained in step 3) are injected into ultra-low temperature liquid nitrogen at -100°C at a rate of 10ml / min-20ml / min. After a period of reaction, the tea leaves are concentrated 5 times to obtain a high-purity tea extract.

[0043] 5) Obtain theanine powder:

[0044] Basic copper carbonate is added to the high-purity tea extract obtained in step 4), with the weight ratio of tea extract to basic copper carbonate being 1:5. A 6-stage microchannel fluid separation system processor is then used for extraction and separation. The extraction temperature is 50°C and the extraction time is 120 minutes. After extraction, the extract is filtered using a microfiltration membrane with a pore size of 0.1um-0.5um to obtain theanine powder. The microchannel fluid separation system processor has a multi-stage adsorption flow microchannel, which is treated with different fluid media to adsorb and flow different components in the extract through the fluid microchannel, thereby separating theanine powder. Because tea contains a variety of water-soluble components, the use of multi-stage fluid microchannel separation technology can ensure the effective removal of impurities on the basis of high separation efficiency without contaminating the active ingredient, thereby obtaining highly purified active substances.

[0045] 6) Obtaining 98% purified theanine powder:

[0046] Sulfuric acid is added to the theanine powder obtained in step 5), the pH of the theanine powder is adjusted to 4-6, the temperature is adjusted to 40°C, the sulfuric acid reacts with basic copper carbonate to obtain copper theanine salt, and hydrogen sulfide is then added to react and precipitate to remove copper ions and reduce to obtain 98% purified theanine powder;

[0047] 7) Obtaining a fully bio-based theanine finishing agent:

[0048] The tea supernatant obtained in step 2) and the 98% purified theanine powder obtained in step 6) are mixed and placed in a high-speed stirring barrel and stirred to obtain a fully bio-based theanine finishing agent; wherein the mass percentage of the tea supernatant and the 98% purified theanine powder is 80wt%:20wt%, the stirring speed is 1000r / min, and the stirring time is 30min, thereby obtaining a fully bio-based theanine finishing agent.

[0049] Example 2

[0050] The preparation method of theanine finishing agent for textiles comprises the following steps:

[0051] 1) Initially obtain green tea leaf tissue fluid:

[0052] Green tea buds and diatomaceous earth are placed in a high-speed stirring barrel and stirred at a ratio of 95 wt% to 5 wt% (mass percentage), with the net moisture content of the green tea buds between 0.5% and 2%. The stirring speed is 1000 r / min, the stirring time is 4 hours, and the stirring temperature is 25°C to obtain tea tissue fluid. The tea buds are preferably grown at an altitude of 500 to 800 meters. The diatomaceous earth is produced from Changbai Mountain and has a D90 particle size of 2 to 10 μm.

[0053] 2) Collecting tea supernatant:

[0054] The tea tissue fluid obtained in step 1) was allowed to stand for 24 hours at a temperature of 26° C. and a humidity of 95%, and the upper translucent liquid was collected as the tea supernatant;

[0055] 3) Obtaining tea tissue:

[0056] Filtering the tea tissue fluid obtained from the upper translucent liquid in step 2) to remove diatomaceous earth powder precipitate in the tea tissue fluid to obtain tea tissue;

[0057] 4) Obtaining high-purity tea extract:

[0058] Injecting the tea leaves obtained in step 3) into ultra-low temperature liquid nitrogen at -100°C at an injection rate of 10ml / min-20ml / min to obtain a high-purity tea extract;

[0059] 5) Obtain theanine powder:

[0060] Basic copper carbonate is added to the high-purity tea extract obtained in step 4), with the weight ratio of tea extract to basic copper carbonate being 1:15. The mixture is then separated and extracted using a 10-stage microchannel fluid separation system processor, and subjected to countercurrent turbulent extraction in a separation adsorption microchannel with a stage number of 6-10. The extraction temperature is 100°C, the extraction time is 60 minutes, and after extraction, the mixture is filtered using a microfiltration membrane with a pore size of 0.1um-0.5um to obtain theanine powder. Compared to Example 1, the microchannel fluid separation system processor in Example 2 has increased the number of stages and higher purity. Multiple stages are opened for extraction to increase the processing speed.

[0061] 6) Obtaining 98% purified theanine powder:

[0062] Sulfuric acid is added to the theanine powder obtained in step 5), the pH of the theanine powder is adjusted to 4-6, the temperature is adjusted to 50° C., the sulfuric acid reacts with basic copper carbonate to obtain copper theanine salt, and hydrogen sulfide is then added to react and precipitate to remove copper ions and reduce to obtain 98% purified theanine powder;

[0063] 7) Obtaining a fully bio-based theanine finishing agent:

[0064] The tea supernatant from step 2) and the 98% purified theanine powder from step 6) were mixed in a ratio of 90 wt% to 10 wt% and placed in a high-speed stirring barrel with stirring at a speed of 1000 rpm for 30 min to obtain a fully bio-based theanine finishing agent.

[0065] Compared with Example 1 and Example 2, the content of diatomaceous earth powder added in Example 1 is greater than that in Example 2. The stirring time of Example 1 is 2 hours, while the stirring time of Example 2 is 4 hours. The stirring time of Example 1 is half of that of Example 2, and the stirring efficiency is greatly improved.

[0066] How to use theanine finishing agent for textiles 1:

[0067] During the impregnation or padding finishing process of textile fabrics, 20wt%-50wt% of a fully bio-based theanine finishing agent is added. The fully bio-based theanine finishing agent adheres to the surface of the textile fabric during the impregnation process. After subsequent drying, curing and balancing treatment of the fabric, the theanine is mixed into the interior and surface of the textile fabric. Since theanine is a pure natural substance with bactericidal properties, the obtained fabric has antibacterial properties. The preparation process is green and environmentally friendly, reduces chemicals, and improves the safety and comfort of textile use.

[0068] Method 2 for using theanine finishing agent for textiles: adopt a spraying treatment process, the conditions of which are that the weight ratio of silicone oil to water is 6-10:90-94, the weight ratio of theanine finishing agent to silicone oil solution is 1-2:98-99, the spinning speed is 180m / min, and then drying is carried out at a drying temperature of 120-170℃; finally, setting treatment is carried out at 180℃ for 30-40 seconds, and then the theanine antibacterial fiber is obtained through packaging and other processes.

[0069] Table 1 is a table showing the antibacterial properties of the control group and the fabric impregnated with the all-biobased theanine finishing agent provided by the present invention (i.e., usage method 1) against various bacterial species after initial use and after washing 30 times.

[0070] Table 1

[0071] The control group used antibacterial fabrics synthesized by curing chemical substances. The example used fabrics treated with the fully bio-based theanine finish prepared by the above-described method. The results are as follows. Antibacterial efficacy evaluation showed an antibacterial activity of greater than 90% against Escherichia coli and Candida albicans, and greater than 89% against Staphylococcus aureus.

[0072] The preparation method of theanine gel for textile use comprises the following steps:

[0073] S1, placing 2%-5% by mass of ethyl acetate in a stirring device and stirring and emulsifying for 20-50 minutes, the stirring device is set to a speed of 2000-4000 r / min, to obtain a solution as the oil phase; by stirring, the emulsification speed is accelerated, the time for preparing theanine gel is shortened, and work efficiency is improved.

[0074] S2, dissolving seaweed polysaccharide in 1%-1.5% by mass glacial acetic acid solution to prepare 4%-6% by mass seaweed polysaccharide acetic acid solution, and then adding 3%-5% by mass hyaluronic acid solution, stirring evenly, as the deionized water phase; hyaluronic acid can absorb a large amount of water and has high water retention. Adding hyaluronic acid solution to the deionized water phase can make the subsequently prepared theanine gel have moisturizing function, and the hyaluronic acid contained in the theanine gel can be transferred to human skin to form a film suitable for human skin, which has good moisturizing properties and alleviates the effects of irritants on the skin.

[0075] S3, adding the deionized water phase prepared in S2 dropwise into the oil phase prepared in S1, and continuing stirring and emulsifying in a stirring device for 20-50 minutes, with the stirring device set to a speed of 2000-4000 r / min, to obtain a deionized water-in-oil emulsion;

[0076] In step S4, the stirring speed is adjusted to 500-800 rpm. The fully bio-based theanine solution is added dropwise to the deionized water-in-oil emulsion prepared in step S3. The mixture is reacted at 40-60°C for 1-2 hours to obtain a mixed solution. A 1%-2% by weight sodium carbonate deionized water solution is added to the mixed solution, the pH is adjusted to 5-7, and the mixture is cured for 20-50 minutes. The precipitate is collected and washed 3-5 times with deionized water-free ethanol. After vacuum drying, the theanine gel is obtained. By utilizing the fluid properties of hyaluronic acid and seaweed polysaccharides, the fully bio-based theanine solution is organically integrated into a composite fluid with a certain viscosity, thereby obtaining a stable gel-state of theanine. This can reduce material loss during subsequent processing and more easily form a homogeneous coating layer on the fiber surface.

[0077] How to use theanine gel for textiles:

[0078] The fiber is rotated in the theanine gel in the form of a monofilament, so that the fiber is coated with the theanine gel. The fiber coated with the theanine gel can be dried at room temperature, or the fiber coated with the theanine gel can be dried at 120-170°C.

[0079] Theanine gel and theanine finishing agent can be used in combination: coating with theanine gel first, followed by finishing with theanine finishing agent. This strengthens the bond between theanine and the fiber, thereby enhancing the durability of the antimicrobial effect. The finishing agent can also fill vacant sites created during the coating process. Alternatively, the fiber can be treated with theanine gel and the textile can be treated with theanine finishing agent.

[0080] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, they indicate the presence of features, steps, operations, devices, components and / or combinations thereof.

[0081] Unless otherwise specifically stated, the relative arrangement of the parts and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present application. At the same time, it should be understood that, for ease of description, the sizes of the various parts shown in the drawings are not drawn according to actual proportional relationships. The techniques, methods and equipment known to those of ordinary skill in the relevant art may not be discussed in detail, but where appropriate, the techniques, methods and equipment should be considered as part of the authorized specification. In all examples shown and discussed here, any specific values ​​should be interpreted as being merely exemplary, rather than as limitations. Therefore, other examples of the exemplary embodiments may have different values. It should be noted that similar numbers and letters represent similar items in the following figures, and therefore, once an item is defined in one figure, it does not need to be further discussed in subsequent figures.

[0082] The above description is only a preferred embodiment of the present invention. All equivalent changes and modifications made according to the scope of the patent application of the present invention should fall within the scope of the present invention.

Claims

1. A method for preparing theanine powder for textile use, characterized in that: The steps include: 1) Preliminary acquisition of tea tissue fluid: Put tea tree buds and diatomaceous earth into a high-speed stirring barrel according to a certain proportion and stir at a high speed to obtain tea tissue fluid; wherein the mass percentage of tea tree buds and diatomaceous earth is 90wt%-95wt%:5wt%-10wt%; 2) Collecting tea supernatant: The tea tissue fluid obtained in step 1) is allowed to stand, and the upper translucent liquid is taken as the tea supernatant; 3) Obtain tea tissue: Filtering the tea tissue fluid obtained from the upper layer of the translucent liquid in step 2) to remove the diatomaceous earth powder precipitate in the tea tissue fluid to obtain tea tissue; 4) Obtaining high-purity tea extract: Injecting ultra-low temperature liquid nitrogen into the tea tissue obtained in step 3), reacting for a period of time, centrifuging, collecting the supernatant, filtering, and concentrating to obtain a high-purity tea extract; 5) Obtain theanine powder: Adding basic copper carbonate to the high-purity tea extract obtained in step 4) and then leaching, separating and filtering to obtain theanine powder.

2. The method for preparing theanine powder for textile use according to claim 1, characterized in that: In the step 1), the net moisture content of the tea tree buds is between 0.5% and 2%.

3. The method for preparing theanine powder for textile use according to claim 1, characterized in that: In the step 1), the stirring speed is 500 r / min-1000 r / min, the stirring time is 2 h-4 h, and the stirring temperature is 25° C.-35° C.

4. A method for preparing a theanine finishing agent for textiles, characterized in that: The steps include: a) Obtaining 98% purified theanine powder: Sulfuric acid is added to theanine powder to adjust the pH of theanine powder to 4-6, the sulfuric acid reacts with basic copper carbonate to obtain theanine copper salt, and then hydrogen sulfide is added to react and precipitate to remove copper ions and reduce to obtain 98% purified theanine powder; b) Obtaining a fully bio-based theanine finishing agent: The tea supernatant and 98% purified theanine powder are mixed, placed in a high-speed stirring barrel and stirred to obtain a fully bio-based theanine finishing agent; wherein the mass percentages of the tea supernatant and the 98% purified theanine powder are 80wt%-90wt%: 10wt%-20wt%.

5. The use of theanine finishing agent for textiles prepared according to claim 4, characterized in that: During the impregnation or padding finishing process of textile fabrics, 20wt%-50wt% of theanine finishing agent is added. The bio-based theanine finishing agent adheres to the surface of the textile fabric during the impregnation process. After subsequent fabric drying, curing and balancing treatment, theanine is mixed into the interior and surface of the textile fabric.

6. The use of theanine finishing agent for textiles prepared according to claim 4, characterized in that: The textile fibers are sprayed, the weight ratio of silicone oil to water in the spray liquid is 6-10:90-94, and the weight ratio of theanine finishing agent to silicone oil solution is 1-2:98-99; the spinning speed is 180m / min, and then drying is performed at a drying temperature of 120-170°C; finally, a shaping treatment is performed at 180°C for 30-40 seconds to make the textile fibers contain theanine.

7. A method for preparing theanine gel for textile use, characterized in that: The steps include: First, 2% to 5% by mass of ethyl acetate is emulsified for 20 to 50 minutes under stirring at 2000 to 4000 r / min to obtain a solution as the oil phase; Then, the seaweed polysaccharide is dissolved in a glacial acetic acid solution with a mass fraction of 1%-1.5% to prepare a seaweed polysaccharide acetic acid solution with a mass fraction of 4%-6%, and then a hyaluronic acid solution with a mass fraction of 3%-5% is added and stirred evenly to form a deionized water phase; Then, the deionized water phase is added dropwise into the oil phase, and the emulsification is continued for 20-50 minutes under stirring at 2000-4000 r / min to obtain a deionized water-in-oil emulsion; Then, under stirring at 500-800 r / min, a solution containing theanine powder prepared according to claim 1 is dripped into the deionized water-in-oil emulsion dropwise, and reacted at 40-60° C. for 1-2 hours. Solution 1 is obtained; Then, the pH value of solution 1 is adjusted to 5-7 with a mass fraction of 1%-2% sodium carbonate deionized water solution, solidified for 20-50 minutes, the precipitate is collected, washed with ethanol without deionized water for 3-5 times, and vacuum dried to obtain theanine gel.

8. The use of theanine gel for textiles prepared according to claim 5, characterized in that: The fiber is rotated in the theanine gel in the form of a monofilament, so that the theanine gel is wrapped outside the fiber.

9. The use of theanine gel for textile use as claimed in claim 8, characterized in that: The fibers coated with theanine gel were left to dry at room temperature.

10. The use of theanine gel for textile use according to claim 8, characterized in that: The fiber coated with theanine gel is dried at 120-170°C.

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