Polyamide-6 master batch with long-acting jasmine fragrance, polyamide-6 fiber and preparation method of polyamide-6 master batch and polyamide-6 fiber

Abstract

The invention discloses a chinlon 6 master batch with long-acting jasmine fragrance, a chinlon 6 fiber and a preparation method of the chinlon 6 master batch and the chinlon 6 fiber, and belongs to the technical field of aromatic functional fibers. Jasmine oil and jasmonone are prepared into a high-concentration aqueous solution according to a specific proportion, PA6 powder is fully soaked in the aqueous solution, then the aqueous solution, PA6 slices and a dispersing agent are subjected to low-temperature melting granulation to prepare aromatic master batches, and the polyamide 6 fiber with long-acting jasmine fragrance is prepared through melt spinning. The stability of the aromatic in high-temperature processing is enhanced by utilizing the intermolecular hydrogen-bond interaction among the jasmine oil, the jasmonone and the nylon matrix, the slow and continuous release is realized, and meanwhile, the aroma synergistic effect is formed due to the volatilization rate difference of the jasmine oil and the jasmonone, so that the fiber has good mechanical properties and a long-acting aroma retaining function, and the long-acting aroma retaining function is realized. The technical problems that a traditional fiber jasmine aromatic is easy to volatilize and difficult to keep fragrance in the high-temperature master batch manufacturing and spinning process are solved, and the jasmine aromatic has good application prospects in the fields of spinning, clothes and the like.

Description

Technical Field

[0001] This invention belongs to the field of aromatic functional fiber technology, specifically relating to a nylon 6 masterbatch with a long-lasting jasmine fragrance, nylon 6 fiber and its preparation method. Background Technology

[0002] Polyamide 6 (PA6), also known as nylon 6, is a synthetic fiber material with excellent comprehensive properties. Its high strength, high abrasion resistance, excellent elastic recovery, and good processing adaptability make it widely used in apparel textiles, home furnishing fabrics, and industrial fabrics. With the increasing demand from the consumer market for functional, personalized, and sensory-experience-enhancing textiles, traditional single-performance polyamide 6 is no longer sufficient for high-end applications. Therefore, endowing polyamide 6 fibers with a pleasant and lasting fragrance has become an important research and development direction for enhancing product added value and user experience. Among these, jasmine fragrance, due to its fresh, elegant, and widely loved qualities, has become a popular choice for fragrance fiber development.

[0003] Introducing fragrance into chemical fibers traditionally falls into two main categories: direct addition and microencapsulation. Direct addition is the most straightforward approach, involving the direct mixing of fragrance agents into the spinning melt or pre-spinning raw materials. This method is simple and relatively low-cost. However, the main fragrance components of jasmine-scented fragrances are organic compounds with small molecular weights and low boiling points, while the melt processing temperature of PA6 is generally between 220°C and 280°C. During this high-temperature, high-shear-force preparation process, the directly added fragrance molecules are highly susceptible to volatilization, thermal oxidative decomposition, or structural isomerization, resulting in significant loss of effective fragrance components during the production stage. Even if a small amount remains inside the fiber, it will quickly dissipate during subsequent storage, transportation, or use, failing to achieve long-lasting fragrance retention.

[0004] To overcome the problems of volatile and easily decomposed fragrances, microencapsulation technology has been widely studied and applied to the development of aromatic fibers. This technology encapsulates fragrances within tiny capsules formed by polymer wall materials (such as melamine resin and polyurea), creating a core-shell structure. These microcapsules can withstand high-temperature processing to a certain extent, protecting the fragrances inside. However, the core drawback of microencapsulation technology lies in its passive release mechanism, which relies on physical rupture. This "high-temperature protection - mechanical rupture release" mode leads to discontinuous, uncontrollable, and unpredictable fragrance release. The intensity of the fragrance depends entirely on the frequency and intensity of external forces, making it impossible to achieve a stable, smooth, and long-lasting release effect, resulting in significant fluctuations in the user experience. Furthermore, the introduction of microcapsule wall materials may affect the mechanical properties, transparency, or processing flowability of polyamide 6 fibers, and some wall materials may pose environmental and safety concerns regarding residual monomers.

[0005] For example, Chinese patent CN115434026A, filed on August 23, 2022, discloses a bamboo-scented viscose fiber and its preparation method. The method involves diluting a bamboo-scented microcapsule slurry mother liquor with an effective content of 40% using deionized water to obtain a bamboo-scented microcapsule diluent; thoroughly mixing the bamboo-scented microcapsule diluent with the viscose stock solution to obtain a bamboo-scented spinning stock solution; regenerating and shaping the bamboo-scented spinning stock solution through a spinneret in a coagulation bath; and finally, cutting, desulfurizing, washing, bleaching, oiling, and drying to obtain the bamboo-scented viscose fiber. The resulting bamboo-scented viscose fiber maintains excellent physical and mechanical properties while possessing the advantages of long-lasting fragrance and water resistance, with a fragrance retention time of up to 80 seconds. 150 days. This preparation uses a wet spinning process, where the temperature of the spinning solution and coagulation bath is usually between room temperature and below 100°C. This low-temperature environment requires much lower thermal stability for the fragrance microcapsules than the melt spinning process of PA6, and therefore is not suitable for the high-temperature melt granulation and spinning process of PA6.

[0006] Chinese patent CN115573072A, filed on November 2, 2022, discloses an aromatic antibacterial composite yarn, its preparation method, and its application. This invention prepares hollow fibers and, during the preparation process, injects fragrance-containing nanocapsules into the cavities of the hollow fibers. The temperature of the hollow fibers produced by melt spinning melts and disperses the nanocapsules into the cavities and micropores of the hollow fibers. After cooling, aromatic fiber filament bundles are obtained. These aromatic fiber filament bundles and antibacterial fiber filament bundles are then blended to obtain the aromatic antibacterial composite yarn. Because the jasmine fragrance nanocapsules are injected into the hollow fibers, the fragrance has a longer retention time and greater stability than that of conventional mixed hollow fibers. However, this physical encapsulation method may still lead to rapid diffusion or leakage of the fragrance through the micropores when the fibers are subjected to significant deformation or high temperatures. The stability and durability of the released fragrance are greatly affected by the microstructure of the fibers. The mechanism of its long-lasting fragrance is still the slow diffusion after physical barrier, rather than the strong binding and slow release based on chemical interaction as in this invention.

[0007] In summary, there is an urgent need in this field for an innovative technical solution, particularly tailored to the characteristics of polyamide 6 materials and jasmine fragrance, that can minimize the loss of volatile fragrances during high-temperature masterbatch manufacturing and spinning processes, while avoiding reliance on mechanical breakage mechanisms, thereby achieving long-lasting and stable release of fragrance in fibers. Summary of the Invention

[0008] To address the problems existing in the prior art, this invention provides a nylon 6 masterbatch with a long-lasting jasmine fragrance, nylon 6 fiber, and its preparation method. The nylon 6 fiber has both good mechanical properties and long-lasting fragrance retention, solving the technical problems of easy volatilization and difficulty in retaining fragrance in traditional fiber jasmine fragrance during high-temperature masterbatch manufacturing and spinning.

[0009] The technical solution of the present invention is as follows: One objective of this invention is to provide a method for preparing nylon 6 masterbatch with a long-lasting jasmine fragrance, comprising the following steps: S11. Weigh the following components according to the formula: 2-4 parts of jasmine oil and 2-8 parts of jasmine ketone mixed evenly to form a high-concentration aqueous solution, 18-45 parts of nylon 6 powder impregnated in the high-concentration aqueous solution, 1-2 parts of dispersant, and 44-77 parts of bright nylon 6 chips. S12. Mix the components weighed in S11 and feed them into a twin-screw extruder to melt and form a melt strip. S13. The extruded strip from step S12 is water-cooled and plasticized, and then pelletized to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0010] Furthermore, the jasmine oil is 1-[2-trans-2-buten-1-yl]-2-methylcyclopentane, with the chemical formula C2. 10 H 16 The CAS number is 8022-96-6, and the structural formula is shown in Figure I: (I). Furthermore, the jasmone is 3-methyl-2-(2-pentenyl)-2-cyclopenten-1-one, with the chemical formula C. 15 H 26 O3, CAS number 158474-72-7, structural formula is shown in II: (II).

[0011] Furthermore, the nylon 6 powder is immersed in a high-concentration aqueous solution at a temperature of 25-35℃ for 5-15 min; the dispersant is 330 dispersant, which can maintain a stable dispersion state during the melting process, optimize the stability of the masterbatch dispersion, and improve the quality and performance of the final masterbatch.

[0012] Furthermore, the temperatures of the twin-screw extruder in zones 1-9 are 210-230℃, 210-230℃, 210-230℃, 205-215℃, 205-205℃, 195-205℃, 185-195℃, 175-185℃, and 165-180℃, respectively, and the die head temperature is 220-230℃.

[0013] The second objective of this invention is to provide a nylon 6 masterbatch with a long-lasting jasmine fragrance.

[0014] The third objective of this invention is to provide a method for preparing nylon 6 fiber with a long-lasting jasmine fragrance, comprising the following steps: S21. Weigh 5 portions of nylon 6 masterbatch with long-lasting jasmine aroma and 95 portions of nylon 6 semi-glossy chips, and dry them separately. S22. Feed semi-dull nylon 6 chips into the main feed port, and put nylon 6 masterbatch with long-lasting jasmine aroma into the buffer bin. After being placed into the hopper, it is spirally stirred evenly and fed into the side feed port. After being mixed evenly, it is compounded and melted in a twin-screw extruder to obtain a composite melt. The composite melt obtained in steps S23 and S21 is metered by a metering pump and then enters the spinning box. The composite filament is obtained by spinning through the component. Then, it undergoes slow cooling, monomer suction, side blowing cooling, bundle oiling, secondary cooling in the channel, stretching and shaping, and winding to obtain the nylon 6 fiber with long-lasting jasmine fragrance.

[0015] Furthermore, the temperature zones of the twin-screw extruder are 240-250℃, 245-255℃, 245-255℃, 245-255℃, and 245-255℃, with the die head temperature being 245-255℃.

[0016] The fourth objective of this invention is to provide a nylon 6 fiber with a long-lasting jasmine fragrance.

[0017] Furthermore, the nylon 6 fiber has a specification of 85D / 24F.

[0018] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention abandons traditional methods of direct addition or microencapsulation, and for the first time designs a novel nylon 6 masterbatch with a long-lasting jasmine aroma based on a synergistic strategy of pretreatment and low-temperature processing using molecular interactions. This invention fully utilizes the different volatility characteristics of jasmine oil and jasmine ketone, two fragrance agents. The jasmine oil component volatilizes quickly, providing the initial bright aroma, while the jasmine ketone component volatilizes slowly, responsible for the long-lasting aroma. The two components complement and synergize in release kinetics, jointly ensuring the stability and longevity of the jasmine aroma. Simultaneously, strong intermolecular hydrogen bonds can form between the hydrogen donors in the jasmine oil and jasmine ketone molecules and the H, O, and N atoms on the terminal amino and carboxyl groups at the end of the PA6 molecular chain. This not only promotes the effective adsorption and binding of the fragrance agent on the PA6 powder during the impregnation stage, but also plays an anchoring and protective role in the subsequent masterbatch melting and granulation process, significantly reducing volatilization and heat loss at high temperatures, laying a chemical foundation for the long-lasting sustained release of aroma in the fiber.

[0019] 2. The nylon 6 fiber disclosed in this invention not only possesses a long-lasting jasmine fragrance but also retains the inherent excellent physical and mechanical properties of nylon 6 fiber. Example data shows that the prepared 85D / 24F POY fiber exhibits a breaking strength of 4.4-4.54 cN / dtex, a breaking elongation of 76.06-77.74%, and key indicators such as evenness and oil content are at the same level as conventional nylon 6 fiber without added fragrance, showing no significant difference. Thermogravimetric analysis (TGA) further confirms that the nylon 6 masterbatch exhibits good thermal stability near the spinning temperature, with a weight loss of only 3.08%. In the temperature range where the PA6 matrix begins to decompose, the weight loss curve of the nylon 6 masterbatch shows a continuous and gentle characteristic, indirectly confirming the stable bond between the fragrance and the matrix. In infrared spectroscopy analysis, the amide II absorption peak undergoes a blue shift and a change in peak shape, providing direct evidence for the existence of hydrogen bonds. The above physicochemical property tests collectively demonstrate that the technical solution of the present invention successfully introduces a lasting jasmine fragrance without adversely affecting the quality of nylon 6 fiber.

[0020] 3. The innovative nylon 6 fiber with long-lasting jasmine fragrance of this invention exhibits significant advantages in application, especially in its long-lasting fragrance retention. When the fiber yarn obtained in the examples was woven into socks and simulated in use, its fragrance retention effect far exceeded that of conventional aromatic fibers that rely on physical rupture for release. Test results show that the fragrance release of products made from the innovative nylon 6 fiber of this invention is the most persistent and stable: the fragrance is strong one week after washing, remains noticeable until the third week, and is still perceptible until the sixth and seventh weeks. Thanks to the regulation of hydrogen bonding forces and the synergistic effect of the volatilization of jasmine oil and jasmine ketone in this invention, the fragrance release process is smooth and continuous, achieving a natural and controllable slow release without relying on external friction. This not only solves the technical problem of fragrance loss during high-temperature processing but also achieves long-lasting and stable fragrance release throughout the product's lifespan, enhancing the sensory value and user experience of textiles, and has broad application prospects in high-end apparel, home textiles, and other fields. Attached Figure Description

[0021] Figure 1 This is a comparison of the thermogravimetric curves of the nylon 6 masterbatch with long-lasting jasmine fragrance prepared in Example 1 of the performance test of the present invention and ordinary nylon 6 chips. Figure 2 The infrared spectra of the nylon 6 masterbatch with long-lasting jasmine aroma and ordinary nylon 6 chips prepared in Example 1 of the performance test of the present invention are shown. Detailed Implementation

[0022] The present invention will be further described below with reference to preferred embodiments. The endpoints and any values ​​of the ranges disclosed in the present invention are not limited to the precise ranges or values. These ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be regarded as specifically disclosed herein. Unless otherwise specified, the experimental methods in the following embodiments are conventional methods, performed in accordance with the techniques or conditions described in the literature in this field or in accordance with the product instructions.

[0023] Unless otherwise specified, all materials and reagents used in the following examples are commercially available.

[0024] Example 1 This embodiment provides a nylon 6 masterbatch with a long-lasting jasmine fragrance, the preparation method of which includes the following steps: (1) Weigh each component of the jasmine masterbatch according to the following formula: 2 parts jasmine oil and 8 parts jasmine ketone are mixed evenly to prepare a high-concentration aqueous solution, 45 parts nylon 6 powder impregnated in the high-concentration aqueous solution, 1 part dispersant, and 44 parts bright nylon 6 chips; (2) Mix the components weighed in step (1) and impregnate them at an ambient temperature of 30°C for 10 min. Then feed them into a twin-screw extruder to melt and form a melt strip. The temperatures of the twin-screw extruder in zones 1-9 are 210℃, 210℃, 210℃, 205℃, 205℃, 195℃, 185℃, 175℃, and 165℃, respectively, and the die head temperature is 220℃. (3) The extruded strip from step (2) is water-cooled and plasticized, and then granulated to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0025] Example 2 This embodiment provides a nylon 6 masterbatch with a long-lasting jasmine fragrance, the preparation method of which includes the following steps: (1) Weigh the components of the jasmine masterbatch according to the following formula: 2 parts jasmine oil and 6 parts jasmine ketone are mixed evenly to prepare a high-concentration aqueous solution, 45 parts nylon 6 powder impregnated in the high-concentration aqueous solution, 1 part dispersant, and 46 parts bright nylon 6 chips. (2) Mix the components weighed in step (1) and impregnate them at an ambient temperature of 30°C for 10 min. Then feed them into a twin-screw extruder to melt and form a melt strip. The temperatures of the twin-screw extruder in zones 1-9 are 210℃, 210℃, 210℃, 205℃, 205℃, 195℃, 185℃, 175℃, and 165℃, respectively, and the die head temperature is 220℃. (3) The extruded strip from step (2) is water-cooled and plasticized, and then granulated to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0026] Example 3 This embodiment provides a method for preparing nylon 6 masterbatch with a long-lasting jasmine fragrance, comprising the following steps: (1) Weigh the components of the jasmine masterbatch according to the following formula: 4 parts jasmine oil and 8 parts jasmine ketone are mixed evenly to prepare a high-concentration aqueous solution, 45 parts nylon 6 powder impregnated in the high-concentration aqueous solution, 1 part dispersant, and 42 parts bright nylon 6 chips. (2) Mix the components weighed in step (1) and impregnate them at an ambient temperature of 30°C for 10 min. Then feed them into a twin-screw extruder to melt and form a melt strip. The temperatures of the twin-screw extruder in zones 1-9 are 210℃, 210℃, 210℃, 205℃, 205℃, 195℃, 185℃, 175℃, and 165℃, respectively, and the die head temperature is 220℃. (3) The extruded strip from step (2) is water-cooled and plasticized, and then granulated to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0027] Example 4 This embodiment provides a method for preparing nylon 6 masterbatch with a long-lasting jasmine fragrance, comprising the following steps: (1) Weigh the components of the jasmine masterbatch according to the following formula: 2 parts jasmine oil and 8 parts jasmine ketone are mixed evenly to prepare a high-concentration aqueous solution, 36 parts nylon 6 powder impregnated in the high-concentration aqueous solution, 1 part dispersant, and 55 parts bright nylon 6 chips. (2) Mix the components weighed in step (1) and impregnate them at an ambient temperature of 30°C for 10 min. Then feed them into a twin-screw extruder to melt and form a melt strip. The temperatures of the twin-screw extruder in zones 1-9 are 230℃, 230℃, 230℃, 215℃, 205℃, 205℃, 195℃, 185℃, and 180℃, respectively, and the die head temperature is 230℃. (3) The extruded strip from step (2) is water-cooled and plasticized, and then granulated to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0028] Example 5 This embodiment provides a method for preparing nylon 6 masterbatch with a long-lasting jasmine fragrance, comprising the following steps: (1) Weigh the components of the jasmine masterbatch according to the following formula: 2 parts jasmine oil and 8 parts jasmine ketone are mixed evenly to prepare a high-concentration aqueous solution, 36 parts nylon 6 powder impregnated in the high-concentration aqueous solution, 1 part dispersant, and 55 parts bright nylon 6 chips. (2) Mix the components weighed in step (1) and soak them at an ambient temperature of 25°C for 5 min before feeding them into a twin-screw extruder to melt and form a melt strip; The temperatures of the twin-screw extruder in zones 1-9 are 230℃, 230℃, 230℃, 215℃, 205℃, 205℃, 195℃, 185℃, and 180℃, respectively, and the die head temperature is 230℃. (3) The extruded strip from step (2) is water-cooled and plasticized, and then granulated to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0029] Example 6 This embodiment provides a nylon 6 fiber with a long-lasting jasmine fragrance, the preparation method of which includes the following steps: (1) Weigh 5 parts of the nylon 6 masterbatch with long-lasting jasmine fragrance prepared in Example 1 and 95 parts of nylon 6 semi-dull chips, and dry them respectively. (2) The semi-bright nylon 6 chips are fed into the main feed port, the nylon 6 masterbatch is put into the buffer bin, and after being placed into the hopper, it is stirred evenly by a spiral and fed into the side feed port. After being mixed evenly, it is compounded and melted in a twin-screw extruder to obtain a composite melt. The extruder temperature zones are 243℃, 249℃, 253℃, 253℃, 253℃, and the die head temperature is 252℃. (3) The composite melt obtained in step (2) is metered by a metering pump and then enters the spinning box. The composite filament is obtained by spinning through the components. After slow cooling, monomer suction, side blowing cooling, bundling oiling, secondary cooling in the channel, stretching and shaping, and winding, the nylon 6 fiber with long-lasting jasmine fragrance is obtained with a specification of 85D / 24F.

[0030] Example 7 This embodiment provides a nylon 6 fiber with a long-lasting jasmine fragrance. Its preparation method is the same as that of Example 7, except that the nylon 6 masterbatch obtained in Example 2 is used. The extruder temperature zones are 250°C, 251°C, 245°C, 245°C, 245°C, and the die head temperature is 250°C.

[0031] Example 8 This embodiment provides a method for preparing nylon 6 fiber with a long-lasting jasmine fragrance. The only difference from Example 7 is that the nylon 6 masterbatch obtained in Example 3 is used.

[0032] The temperature zones of the twin-screw extruder are 244℃, 245℃, 245℃, 245℃, and the die head temperature is 249℃.

[0033] Example 9 This embodiment provides a method for preparing nylon 6 fiber with a long-lasting jasmine fragrance. The only difference from Example 7 is that the nylon 6 masterbatch obtained in Example 4 is used.

[0034] The temperature zones of the twin-screw extruder are 246℃, 251℃, 254℃, 254℃, and the die head temperature is 253℃.

[0035] Example 10 This embodiment provides a method for preparing nylon 6 fiber with a long-lasting jasmine fragrance. The only difference from Example 7 is that the nylon 6 masterbatch obtained in Example 5 is used.

[0036] The temperature zones of the twin-screw extruder are 240℃, 255℃, 255℃, 255℃, and the die head temperature is 255℃.

[0037] Example 11 This embodiment provides a method for preparing nylon 6 masterbatch with a long-lasting jasmine fragrance, comprising the following steps: (1) Weigh the components of the jasmine masterbatch according to the following formula: 3 parts jasmine oil and 8 parts jasmine ketone are mixed evenly to prepare a high-concentration aqueous solution, 18 parts nylon 6 powder impregnated in the high-concentration aqueous solution, 2 parts dispersant, and 77 parts bright nylon 6 chips; (2) Mix the components weighed in step (1) and soak them at an ambient temperature of 25°C for 5 min before feeding them into a twin-screw extruder to melt and form a melt strip; The temperatures of the twin-screw extruder in zones 1-9 are 230℃, 230℃, 230℃, 215℃, 205℃, 205℃, 195℃, 185℃, and 180℃, respectively, and the die head temperature is 230℃. (3) The extruded strip from step (2) is water-cooled and plasticized, and then granulated to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0038] Example 12 This embodiment provides a method for preparing nylon 6 masterbatch with a long-lasting jasmine fragrance, comprising the following steps: (1) Weigh the components of the jasmine masterbatch according to the following formula: 3 parts jasmine oil and 7 parts jasmine ketone are mixed evenly to prepare a high-concentration aqueous solution, 45 parts nylon 6 powder impregnated in the high-concentration aqueous solution, 1 part dispersant, and 44 parts bright nylon 6 chips. (2) Mix the weighed components in step (1) and impregnate them at an ambient temperature of 27°C for 7 min. Then feed them into a twin-screw extruder to melt and form a melt strip. The temperatures of the twin-screw extruder in zones 1-9 are 230℃, 230℃, 230℃, 215℃, 205℃, 205℃, 195℃, 185℃, and 180℃, respectively, and the die head temperature is 230℃. (3) The extruded strip from step (2) is water-cooled and plasticized, and then granulated to obtain the nylon 6 masterbatch with long-lasting jasmine fragrance.

[0039] Comparative Example 1 This comparative example provides a conventional method for preparing nylon 6 fibers. The only difference from Example 5 is that it does not use nylon 6 masterbatch with a long-lasting jasmine fragrance, but uses semi-dull nylon 6 chips instead.

[0040] Performance testing 1. Thermogravimetric analysis and infrared spectroscopy Thermogravimetric analysis and infrared spectroscopy analysis were performed on the nylon 6 masterbatch with long-lasting jasmine aroma and ordinary nylon 6 chips prepared in Example 1, respectively. The results are as follows: Figures 1-2 As shown.

[0041] like Figure 1 As shown, a comparison of the thermogravimetric curves of Example 1 and conventional nylon 6 chips reveals that, at a spinning temperature (approximately 250°C), the nylon 6 masterbatch prepared in Example 1 maintains good stability (only a weight loss of 3.08%). The thermogravimetric curves show continuous and slow weight loss between 250-370°C, demonstrating a relatively stable bond between the fragrance component and the nylon component. When the temperature reaches 370°C, the conventional nylon 6 component begins to decompose. At this point, Example 1 shows a weight loss of 8.93%, while conventional nylon 6 chips show a weight loss of 2.91%. This suggests that the fragrance component (jasmine oil / jasmone) has completely evaporated / decomposed, indirectly proving the presence of jasmine oil and jasmone components in Example 1.

[0042] like Figure 2 As shown, the nylon 6 masterbatch prepared in Example 1 simultaneously exhibited characteristic peaks of both fragrance and nylon 6 chips, proving that both are present in the nylon 6 masterbatch. In Example 1, the peak at 1542 cm⁻¹... -1 The amide II absorption peak (NH deformation vibration absorption peak) at 1500 cm⁻¹ shows a slight blue shift compared to nylon 6 chips, and at 1500 cm⁻¹... -1 The relatively broadened peak shape of the following wavenumbers proves the existence of hydrogen bonds between the fragrance and the nylon component.

[0043] 2. Standard performance tests of masterbatch The conventional properties of the nylon 6 masterbatch prepared in Examples 1-5 were tested, and the results are shown in Table 1: Table 1. Test results of masterbatch from Examples 1-5

[0044] As can be seen from the table above, the nylon 6 masterbatch prepared in Examples 1-5 of the present invention has a long-lasting jasmine fragrance and all indicators are still normal, making it suitable for various subsequent nylon 6 spinning processes.

[0045] 3. Standard fiber performance tests The conventional properties of the nylon 6 fibers obtained in Examples 6-10 and Comparative Example 1 were tested, and the results are shown in Table 2: Table 2 Fiber test results of Examples 6-10

[0046] As can be seen from the table above, the various indicators of the nylon 6 fibers obtained in Examples 6-10 of the present invention are not significantly different from those of conventional nylon 6 fibers, proving that the jasmine fragrance and preparation process used in the present invention will not have an adverse effect on the quality of its nylon 6 fiber products.

[0047] 4. Fragrance retention test The nylon 6 fiber products with long-lasting jasmine fragrance obtained in Examples 6-10 were woven into socks and washed every week to test their fragrance retention effect. The test results are shown in Table 3. Table 3. Results of fiber fragrance retention test in Examples 6-10

[0048] As can be seen from the table above, the products prepared using the nylon 6 fiber described in this invention exhibit good fragrance retention, with a fragrance retention time of more than four weeks and a long-lasting and stable fragrance release, which is significantly better than conventional technology. Among them, the products prepared in Examples 6-8 still have a noticeable fragrance after seven weeks of washing.

[0049] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent modifications made based on the content of the present invention specification and drawings, or direct or indirect applications in related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A process for the preparation of polyamide 6 masterbatch having long-lasting jasmine fragrance, characterized in that, It comprises the following steps: S11, according to the formula, the following components are weighed: 2-4 parts of jasmine oil and 2-8 parts of jasmine ketone mixed uniformly to form a high concentration aqueous solution, 18-45 parts of polyamide 6 powder immersed in the high concentration aqueous solution, 1-2 parts of dispersant, 44-77 parts of polyamide 6 bright chip; S12, the components weighed in S11 are mixed and fed into a double screw extruder to form a melt strip; S13, the melt strip extruded in step S12 is water cooled, plasticized and pelletized to obtain the polyamide 6 master batch with long-lasting jasmine fragrance.

2. A process for the preparation of a polyamide 6 masterbatch having long-lasting jasmine fragrance according to claim 1, characterized in that, The jasmine oil is 1 -[2-trans-2-buten-1 -yl]-2-methylcyclopentane, chemical formula C 10 H 16 , CAS No. 8022-96-6, structural formula as shown in I: （I）。 3. The process for the preparation of long-lasting jasmine-scented polyamide 6 masterbatch as claimed in claim 1, wherein, The jasmonate is 3-methyl-2-(2-pentenyl)-2-cyclopenten-1-one, having the chemical formula C 15 H 26 O3, CAS No. 158474-72-7, having the structural formula II: (I). (II).

4. The process for the preparation of long lasting jasmine fragranced polyamide 6 masterbatch as claimed in claim 1, wherein, The polyamide 6 powder is immersed in the high concentration aqueous solution at a temperature of 25-35℃ for 5-15 min; the dispersant is 330 dispersant.

5. The process for the preparation of long-lasting jasmine-scented polyamide 6 masterbatch as claimed in claim 1, wherein, The temperature of the double screw extruder in 1-9 temperature zones is 210-230℃, 210-230℃, 210-230℃, 205-215℃, 205-205℃, 195-205℃, 185-195℃, 175-185℃, 165-180℃, and the die temperature is 220-230℃.

6. A polyamide 6 master batch with long-lasting jasmine fragrance prepared by the preparation method of any one of claims 1 to 5.

7. A method for preparing long-lasting jasmine-scented nylon 6 fibers using the nylon 6 masterbatch of claim 6, characterized in that, It comprises the following steps: S21, 5 parts of polyamide 6 master batch with long-lasting jasmine fragrance and 95 parts of polyamide 6 semi-dull chip are weighed and dried respectively; S22, the polyamide 6 semi-dull chip is fed from the main feeding port, and the polyamide 6 master batch with long-lasting jasmine fragrance is put into the buffer bin and uniformly stirred by the screw after being lowered to the hopper, then it is fed from the side feeding port, and the mixture is uniformly mixed and then compounded and melted in the double screw extruder to obtain a composite melt; S23, the composite melt prepared in step S21 is metered by a metering pump and then enters the spinning box, and a composite yarn is obtained by spinning through the assembly, and then the composite yarn is slowly cooled, monomer suctioned, side blown and cooled, oil collected, cooled again in the duct, stretched and set, and wound to obtain the polyamide 6 fiber with long-lasting jasmine fragrance.

8. The process for preparing a nylon 6 fiber having a long-lasting jasmine fragrance according to claim 7, wherein the jasmine fragrance is added to the nylon 6 fiber in an amount of 0.0001 to 0.1% by weight. The temperature of the double screw extruder in 1-9 temperature zones is 240-250℃, 245-255℃, 245-255℃, 245-255℃, 245-255℃, and the die temperature is 245-255℃.

9. A polyamide 6 fiber with long-lasting jasmine fragrance prepared by the preparation method of any one of claims 7 to 9.

10. The nylon 6 fiber with long-lasting jasmine fragrance according to claim 9, characterized in that, The specification of the polyamide 6 fiber is 85D / 24F.

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