Plant fiber containing a peppermint extract and a process for the preparation thereof

Abstract

The present application provides a kind of plant fiber containing mint extract and its preparation process, the plant fiber is after washing 50 times, the inhibition rate of staphylococcus aureus, escherichia coli, klebsiella pneumoniae, candida albicans is all ≥95%, the killing rate of influenza virus H3N2, H1N1 is all ≥99%, with excellent cool feeling function, the average contact cool feeling coefficient is higher than 0.19J / cm 2 The biomass component A is combined with the biomass component B into the biomass component C by gas deposition method, on the one hand, the biomass component B is used as a tubular substrate, and a rhizome plant is calcined to form a porous carbon structure skeleton as a solid for gas deposition; the solution gas molecular weight of the biomass component A is small, and after the solution is vaporized, the biomass component A is captured by the porous structure of the biomass component B and uniformly filled into the pores of the biomass component B, so as to ensure the durability of the plant function and play a protective role at high temperature. The biomass component C is blended with a polymer slice and then subjected to subsequent spinning, so as to reduce the loss of the biomass component A in the preparation of the fiber.

Description

Technical Field

[0001] This invention belongs to the field of plant fiber technology, specifically relating to a plant fiber containing peppermint extract and its preparation process. Background Technology

[0002] Synthetic fibers are fibers made from high molecular weight compounds, including polyester, nylon, and acrylic fibers. Synthetic fibers have good abrasion resistance, high strength, and are more durable, but most synthetic fibers, such as polyester and nylon, have poor moisture absorption and antistatic properties. Adding plant components to synthetic fibers not only increases the number of hydrophilic functional groups such as -OH, -NH2, and -COOH, improving the moisture regain and absorption, but also ensures good cell compatibility, preventing allergic reactions and providing antibacterial and antiviral functions. This endows synthetic fibers with natural antibacterial properties, aligning better with modern people's green and health-conscious lifestyle.

[0003] The patent, titled "Preparation Method of Polyester Fiber Containing Honeysuckle Herbal Antibacterial and Antioxidant Skin Care," with patent number "CN202111519624.0," involves purifying honeysuckle and other traditional Chinese medicines, adding them to PET chips to form masterbatch, and then melt-extruding them into polyester fibers. However, this method requires high temperatures for the melt spinning process of synthetic fibers, such as 230℃ for PP and 270℃ for PET. At these temperatures, plant components will carbonize, gelatinize, and turn black, damaging or deactivating the effective ingredients, wasting plant resources, and increasing production costs. Summary of the Invention

[0004] To address the problems existing in the prior art, this invention provides a plant fiber containing peppermint extract and its preparation process, thereby achieving the invention objective of endowing synthetic fibers with natural cooling, antibacterial, and antiviral properties.

[0005] To solve the above technical problems, the present invention adopts the following technical solution:

[0006] A process for preparing plant fiber containing peppermint extract includes the following steps:

[0007] S1, Preparation of biomass component C

[0008] The solution containing biomass component A is heated to boiling. Nitrogen gas is used to propel the gas generated after boiling and continuously introduce it into biomass component B. After reacting for a period of time, the solution is cooled to room temperature. Biomass component C is obtained by filtration, purification, and grinding.

[0009] Preferably, in the solution containing biomass component A, the mass ratio of biomass component A to solvent is 0.5 to 2:1.

[0010] Furthermore, the solvent is one or more of methanol, ethanol, diethyl ether, acetone, and petroleum ether.

[0011] Preferably, the nitrogen flow rate is 0.1–1 m / s; and the reaction time is 4–8 h.

[0012] Preferably, the purification is carried out by one of rotary evaporation, vacuum decompression, or static evaporation.

[0013] Preferably, the preparation method of biomass component A is as follows: the plant components are pulverized to 1-10 μm and then immersed in liquid, followed by low-temperature extraction with an extraction solvent to extract the phenolic polymers in the plant components. The product obtained after filtration, separation, and low-temperature drying is biomass component A.

[0014] Preferably, the plant ingredient is one or more of peppermint, tea, grape, chili, and oats.

[0015] Preferably, the liquid is one or more of methanol, ethanol, acetone, and water.

[0016] More preferably, the liquid is ethanol and water in a mass ratio of 8:2.

[0017] Preferably, the extraction solvent is one or more of n-hexane, n-butanol, and ethyl acetate.

[0018] Preferably, the low-temperature extraction temperature is 0–40°C, the extraction time is 3–4 h, and the flow rate of the extraction solvent is 1–2 L / h.

[0019] Preferably, the low-temperature drying is drying at 45°C or infrared drying at room temperature.

[0020] Preferably, the preparation method of biomass component B is as follows: the root and rhizome plants are dried, crushed, calcined, washed, and filtered to form a powder, namely biomass component B.

[0021] Preferably, the rhizome plant is one or more of tea stems, wheat stems, isatis root, mugwort stems, and mint stems.

[0022] Preferably, the particle size of the pulverized material is 1–10 μm; the calcination temperature is 800–1500 °C, and the time is 3–6 h.

[0023] Preferably, the biomass component B is a plant vascular bundle-like carbonized material with a specific surface area of ​​300–800 m². 2 / g.

[0024] Preferably, the mass ratio of biomass component A to biomass component B is 2.8 to 3.5:1.

[0025] Preferably, the particle size of the biomass component C is 200 nm to 1 μm.

[0026] Using vapor deposition, biomass component A and biomass component B are combined. On the one hand, biomass component B serves as a tubular substrate, forming a porous carbon structure framework after the rhizomes are calcined. As a solid in the vapor deposition, the gas molecules in the solution containing biomass component A have small molecular weights. After vaporization with the solution, they are captured by the porous structure of biomass component B and uniformly filled into the pores of biomass component B, ensuring the durability of plant functions and providing protection at high temperatures.

[0027] S2. Preparation of biomass masterbatch

[0028] Biomass component C is blended and polymerized with polymer chips at high temperature to prepare biomass masterbatch.

[0029] Preferably, the polymer chips are one or more of polyethylene terephthalate, polybutylene terephthalate, polycaprolactam, polyhexamethylene adipamide, polypropylene, polyurethane, polyethylene, polyacrylic acid, polystyrene, and polyacrylonitrile.

[0030] Preferably, the mass ratio of the biomass component C to the polymer chips in the high-temperature blend is 0.01 to 0.2:1.

[0031] Preferably, the high temperature is 160–350°C.

[0032] S3, spinning

[0033] Plant fibers are produced by blending biomass masterbatch with fiber spinning raw materials, followed by melting, extrusion, traction, shaping, and cutting.

[0034] Preferably, the fiber spinning raw material is one of polyester, nylon, polypropylene, chlorofiber, spandex, acrylic fiber, etc.

[0035] Preferably, the blending mass ratio of the biomass masterbatch to the fiber spinning raw material is 0.01 to 0.2:1; and the melting temperature is 160 to 350°C.

[0036] By adopting the above technical solution, the technical effect achieved by the present invention is as follows:

[0037] 1. The fiber prepared by this invention exhibits minimal loss of functional active ingredients during washing. After 50 washes, it maintains an inhibition rate of ≥95% against Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae, and Candida albicans (tested according to GB / T 20944.3-2007), and a kill rate of ≥99% against influenza viruses H3N2 and H1N1 (tested according to ISO18184:2014). The fiber prepared by this invention also exhibits a removal rate of ≥90% against ammonia, acetic acid, isovaleric acid, and nonenal odors (determined according to GB / T 33610.3-2019).

[0038] 2. Biomass component B has a wide range of sources, is easy to process, is a pure natural material with good cell compatibility, and is harmless to both the human body and the environment.

[0039] 3. The plant fiber containing peppermint extract prepared by this invention has excellent cooling properties, with an average contact cooling coefficient higher than 0.19 J / cm. 2 •s (tested according to GB / T 35263-2017).

[0040] 4. The fiber prepared by this invention has a fiber fineness of 0.8 dtex to 6.0 dtex; biomass component A is a cross-linked phenolic polymer and is an unsaturated compound. The cross-linked phenolic polymer is rich in -OH, which can increase the moisture regain of the fiber. The moisture regain of the fiber is 4 to 8%.

[0041] 5. The cross-structured phenolic polymers in biomass component A can effectively increase the stability of the fiber backbone, raise the glass transition temperature, and improve the dimensional stability of the fabric woven from the fiber. Therefore, the fiber has low shrinkage and better dimensional stability.

[0042] 6. The fiber prepared by this invention has a biodegradability rate of over 60% after 180 days (measured according to GB / T19277.1-2011), while ordinary fibers only have a biodegradability of 20-30%.

[0043] 7. The fiber density prepared by this invention is about 30% lower than that of ordinary fibers, making it lighter and more comfortable to wear.

[0044] 8. The preparation process provided by this invention results in less loss of plant components during fiber preparation, reducing the waste of plant resources. The loss rate of biomass component A during fiber preparation is less than 5%. Detailed Implementation

[0045] The present invention will be further illustrated below with reference to specific embodiments.

[0046] Example 1

[0047] S1, Preparation of biomass component C

[0048] The solution containing biomass component A is heated to boiling. Nitrogen gas is used to propel the gas generated after boiling and continuously introduce it into biomass component B. After reacting for a period of time, the solution is cooled to room temperature, filtered, allowed to stand and evaporate, and then ground to obtain biomass component C.

[0049] In the solution containing biomass component A, the mass ratio of biomass component A to solvent methanol is 1:1.

[0050] The nitrogen flow rate is 0.5 m / s; the reaction time is 6 hours.

[0051] The preparation method of biomass component A is as follows: the plant components are crushed to 1μm and then immersed in liquid. The phenolic polymers in the plant components are extracted by low-temperature extraction with an extraction solvent. The product obtained after filtration, separation and low-temperature drying is biomass component A.

[0052] The plant ingredients are peppermint and tea in a 1:1 mass ratio.

[0053] The liquid is ethanol and water in a mass ratio of 8:2, and the extraction solvent is n-hexane.

[0054] The low-temperature extraction was performed at a temperature of 10°C for 4 hours, with a solvent flow rate of 1.5 L / h; the low-temperature drying was performed at 45°C.

[0055] The preparation method of biomass component B is as follows: the root and rhizome plants are dried, crushed, calcined, washed and filtered to form a powder, which is biomass component B.

[0056] The root and rhizome plants are Isatis root, Artemisia stem, and peppermint stem in a mass ratio of 1:1:1.

[0057] The particle size of the pulverized material is 1 μm; the calcination temperature is 1100℃ and the time is 3 h.

[0058] The biomass component B is a carbonized material in the form of plant vascular bundles, with a specific surface area of ​​600 m². 2 / g.

[0059] The mass ratio of biomass component A to biomass component B is 3.3:1.

[0060] The particle size of the biomass component C is 200 nm.

[0061] S2. Preparation of biomass masterbatch

[0062] Biomass component C is blended and polymerized with polymer chips at high temperature to prepare biomass masterbatch.

[0063] The polymer chips are polyethylene terephthalate, and the mass ratio of the biomass component C to the polymer chips in the high-temperature blend is 0.1:1.

[0064] The high temperature is defined as follows: Zone 1 temperature is 305℃, Zone 2 temperature is 315℃, Zone 3 temperature is 305℃, and Zone 4 temperature is 295℃.

[0065] S3, spinning

[0066] Plant fibers are produced by blending biomass masterbatch with fiber spinning raw materials, followed by melting, extrusion, traction, shaping, and cutting.

[0067] The fiber spinning raw material is polyester chips.

[0068] The blending mass ratio of the biomass masterbatch to the fiber spinning raw material is 0.08:1; the melting temperature is 305℃ in zone one, 315℃ in zone two, 305℃ in zone three, and 300℃ in zone four.

[0069] Example 2

[0070] S1, Preparation of biomass component C

[0071] The solution containing biomass component A is heated to boiling. Nitrogen gas is used to propel the gas generated after boiling and continuously introduce it into biomass component B. After reacting for a period of time, the solution is cooled to room temperature, filtered, rotary evaporated, and ground to obtain biomass component C.

[0072] In the solution containing biomass component A, the mass ratio of biomass component A to ethanol is 0.5:1.

[0073] The nitrogen flow rate is 0.1 m / s; the reaction time is 8 hours.

[0074] The preparation method of biomass component A is as follows: the plant components are crushed to 10μm and then immersed in liquid. The phenolic polymers in the plant components are extracted by low-temperature extraction with an extraction solvent. The product obtained after filtration, separation and low-temperature drying is biomass component A.

[0075] The plant ingredients are peppermint, tea, and grapes in a mass ratio of 1:1:1.

[0076] The liquid is ethanol and water in a mass ratio of 8:2, and the extraction solvent is n-hexane.

[0077] The low-temperature extraction was performed at a temperature of 40°C for 4 hours, with a solvent flow rate of 2 L / h.

[0078] Low-temperature drying is infrared drying at room temperature.

[0079] The preparation method of biomass component B is as follows: the root and rhizome plants are dried, crushed, calcined, washed and filtered to form a powder, which is biomass component B.

[0080] The root and rhizome plants are Artemisia argyi stems and peppermint stems in a mass ratio of 1:1.

[0081] The particle size of the pulverized material is 10 μm; the calcination temperature is 800℃ and the time is 3 hours.

[0082] The biomass component B is a carbonized material in the form of plant vascular bundles, with a specific surface area of ​​300 m². 2 / g.

[0083] The mass ratio of biomass component A to biomass component B is 2.8:1.

[0084] The particle size of the biomass component C is 1 μm.

[0085] S2. Preparation of biomass masterbatch

[0086] Biomass component C is blended and polymerized with polymer chips at high temperature to prepare biomass masterbatch.

[0087] The polymer chips are polyethylene terephthalate.

[0088] The mass ratio of the biomass component C to the polymer chips in the high-temperature blend is 0.01:1.

[0089] The high temperature is defined as follows: Zone 1 temperature is 305℃, Zone 2 temperature is 315℃, Zone 3 temperature is 305℃, and Zone 4 temperature is 295℃.

[0090] S3, spinning

[0091] Plant fibers are produced by blending biomass masterbatch with fiber spinning raw materials, followed by melting, extrusion, traction, shaping, and cutting.

[0092] The fiber spinning raw material is polyester chips.

[0093] The blending mass ratio of the biomass masterbatch to the fiber spinning raw material is 0.01:1; the melting temperature is 305℃ in zone one, 315℃ in zone two, 305℃ in zone three, and 300℃ in zone four.

[0094] Example 3

[0095] S1, Preparation of biomass component C

[0096] The solution containing biomass component A is heated to boiling. Nitrogen gas is used to propel the gas generated after boiling and continuously introduce it into biomass component B. After reacting for a period of time, the solution is cooled to room temperature, filtered, vacuum depressurized, and ground to obtain biomass component C.

[0097] In the solution containing biomass component A, the mass ratio of biomass component A to methanol is 2:1.

[0098] The nitrogen flow rate is 1 m / s; the reaction time is 4 h.

[0099] The preparation method of biomass component A is as follows: the plant components are crushed to 5μm and then immersed in liquid. The phenolic polymers in the plant components are extracted by low-temperature extraction with an extraction solvent. The product obtained after filtration, separation and low-temperature drying is biomass component A.

[0100] The plant ingredients are peppermint and tea in a 1:1 mass ratio.

[0101] The liquid is ethanol and water in a mass ratio of 8:2; the extraction solvent is n-hexane.

[0102] The low-temperature extraction was performed at a temperature of 0°C for 3 hours, with a solvent flow rate of 1 L / h.

[0103] The low-temperature drying is drying at 45°C.

[0104] The preparation method of biomass component B is as follows: the root and rhizome plants are dried, crushed, calcined, washed and filtered to form a powder, which is biomass component B.

[0105] The root and rhizome plants are wheat stems, mugwort stems, and mint stems in a mass ratio of 1:1:1.

[0106] The particle size of the pulverized material is 5 μm; the calcination temperature is 1500℃ and the time is 6 h.

[0107] The biomass component B is a carbonized material in the form of plant vascular bundles, with a specific surface area of ​​800 m². 2 / g.

[0108] The mass ratio of biomass component A to biomass component B is 3.5:1.

[0109] The particle size of the biomass component C is 400 nm.

[0110] S2. Preparation of biomass masterbatch

[0111] Biomass component C is blended and polymerized with polymer chips at high temperature to prepare biomass masterbatch.

[0112] The polymer chips are polyethylene terephthalate.

[0113] The biomass component C and the polymer chips are blended at high temperature in a mass ratio of 0.2:1.

[0114] The high temperature is defined as follows: Zone 1 temperature is 305℃, Zone 2 temperature is 315℃, Zone 3 temperature is 305℃, and Zone 4 temperature is 295℃.

[0115] S3, spinning

[0116] Plant fibers are produced by blending biomass masterbatch with fiber spinning raw materials, followed by melting, extrusion, traction, shaping, and cutting.

[0117] The fiber spinning raw material is polyester chips.

[0118] The blending mass ratio of the biomass masterbatch to the fiber spinning raw material is 0.2:1; the melting temperature is 305℃ in zone one, 315℃ in zone two, 305℃ in zone three, and 300℃ in zone four.

[0119] Comparative Example 1

[0120] In Example 1, a representative example was selected. Instead of heating the solution containing biomass component A to boiling, the solution containing biomass component A was directly added to biomass component B. All other aspects were the same as in Example 1. This example served as Comparative Example 1.

[0121] Comparative Example 2

[0122] Example 1, a representative example, was selected. Biomass component B was not calcined, while all other aspects were the same as in Example 1. This example serves as Comparative Example 2.

[0123] Comparative Example 3

[0124] Example 1, a representative example, was selected. Biomass component C was removed, and an equal amount of biomass component A was directly blended and polymerized with polymer chips at high temperature. All other aspects were the same as in Example 1. This was used as Comparative Example 3.

[0125] Comparative Example 4

[0126] Example 1, a representative example, was selected. Biomass component C was removed, and an equal amount of biomass component B was directly blended and polymerized with polymer chips at high temperature. All other aspects were the same as in Example 1. This example was used as Comparative Example 3.

[0127] The changes in biomass component B in Examples 1-3 and Comparative Examples 1-2 were compared with the fiber density, as shown in Table 1.

[0128] Table 1

[0129]

[0130] Table 1 shows that by using vapor deposition to combine biomass component A and biomass component B, biomass component B serves as a tubular substrate. The calcined rhizomes form a porous carbon structure framework, which acts as a solid in the vapor phase. The gas molecules in the solution containing biomass component A have small molecular weights and are captured by the porous structure of biomass component B after vaporization, uniformly filling the pores of biomass component B. Failure to heat and vaporize the solution containing biomass component A or failure to calcine biomass component B will affect the adsorption capacity of biomass component B, ultimately impacting the properties of the resulting biomass component C and plant fibers.

[0131] The antibacterial, antiviral, and cooling effects of Examples 1-3 and Comparative Examples 1-4 after 50 washes are compared, as detailed in Table 2.

[0132] Table 2

[0133]

[0134]

[0135] As shown in Table 2, biomass component A plays a major functional role. Biomass component B, produced by calcination, serves as a tubular substrate for biomass component A, resulting in better adsorption and protection of biomass component A. This ensures the durability of the antibacterial and antiviral effects of the fiber after washing, while also providing protection at high temperatures and reducing the loss of biomass component A during fiber preparation.

[0136] The fiber properties of Examples 1-3 and ordinary fibers are compared, as shown in Table 3.

[0137] Table 3

[0138]

[0139] Table 3 shows that the phenolic polymers in biomass component A can replace some alcohols and undergo condensation reactions, mostly in the main chain, such as polyester / terephthalic acid alcohols, so their biodegradability is better than that of ordinary fibers; the cross-structured phenols can effectively increase the stability of the fiber main chain, increase the glass transition temperature, and improve the dimensional stability of the fabric woven from the fibers.

[0140] Unless otherwise specified, all proportions and percentages mentioned in this invention are mass proportions and mass percentages; all raw materials are commercially available.

[0141] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A plant fiber containing peppermint extract, characterized in that, The plant fiber includes biomass component C; The preparation process of the plant fiber includes the preparation of biomass component C, the preparation of biomass masterbatch, and spinning; The preparation of biomass component C involves heating a solution containing biomass component A to boiling, using nitrogen to propel the gas generated after boiling and continuously introducing it into biomass component B, reacting for a period of time, cooling to room temperature, and then filtering, purifying, and grinding to obtain biomass component C. The preparation method of biomass component A is as follows: after pulverizing the plant components to 1~10μm, immersing them in liquid, and then extracting them at low temperature with an extraction solvent to extract the phenolic polymers in the plant components, the product obtained after filtration, separation, and low-temperature drying is biomass component A. The plant ingredients are one or more of peppermint, tea, grape, chili, and oats; The liquid is one or more of methanol, ethanol, acetone, and water; The preparation method of biomass component B is as follows: the root and rhizome plants are dried, crushed, calcined, washed and filtered to form a powder, which is biomass component B; The rhizome plants are one or more of the following: tea stems, wheat stems, isatis root, mugwort stems, and mint stems.

2. The plant fiber containing peppermint extract according to claim 1, characterized in that, In the solution containing biomass component A, the mass ratio of biomass component A to solvent is 0.5~2:1; The solvent is one or more selected from methanol, ethanol, diethyl ether, acetone, and petroleum ether; The nitrogen flow rate is 0.1~1m / s; the reaction time is 4~8h.

3. The plant fiber containing peppermint extract according to claim 1, characterized in that, The extraction solvent is one or more selected from n-hexane, n-butanol, and ethyl acetate; The low-temperature extraction temperature is 0~40℃, the extraction time is 3~4h, and the flow rate of the extraction solvent is 1~2L / h; The low-temperature drying is drying at 45°C or infrared drying at room temperature.

4. The plant fiber containing peppermint extract according to claim 1, characterized in that, The particle size of the pulverized material is 1~10μm; the calcination temperature is 800~1500℃ and the time is 3~6h; The biomass component B is a carbonized material in the form of plant vascular bundles, with a specific surface area of ​​300-800 m². 2 / g.

5. The plant fiber containing peppermint extract according to claim 1, characterized in that, The mass ratio of biomass component A to biomass component B is 2.8~3.5:1; The particle size of the biomass component C is 200 nm to 1 μm.

6. The plant fiber containing peppermint extract according to claim 1, characterized in that, The preparation of biomass masterbatch involves high-temperature blending of biomass component C with polymer chips to prepare biomass masterbatch. The polymer chips are one or more of the following: polyethylene terephthalate, polybutylene terephthalate, polycaprolactam, polyhexamethylene adipamide, polypropylene, polyurethane, polyethylene, polyacrylic acid, polystyrene, and polyacrylonitrile.

7. The plant fiber containing peppermint extract according to claim 6, characterized in that, The mass ratio of the biomass component C to the polymer chips during high-temperature blending is 0.01~0.2:1; The high temperature is 160~350℃.

8. The plant fiber containing peppermint extract according to claim 1, characterized in that, The spinning process involves blending biomass masterbatch with fiber spinning raw materials, followed by melting, extrusion, traction, shaping, and cutting to produce plant fibers. The fiber spinning raw material is one of polyester, nylon, polypropylene, chlorofiber, spandex, and acrylic fiber; the blending mass ratio of the biomass masterbatch to the fiber spinning raw material is 0.01~0.2:1; and the melting temperature is 160~350℃.

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