Hyaluronic acid microcapsules, hyaluronic acid - nylon 6 masterbatch, hyaluronic acid - nylon 6 filament and preparation method

By preparing hyaluronic acid microcapsules coated with gelatin and gum arabic and combining them with nylon 6 masterbatch, the problem of poor fusion of hyaluronic acid in textile materials was solved, achieving stable dispersion and excellent filament mechanical properties.

CN117051490BActive Publication Date: 2026-03-27TAI CHI STONE (SHANGHAI) TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-18
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

In existing technologies, hyaluronic acid is difficult to effectively integrate with textile materials, is easily lost, and its addition to textile raw materials results in poor spinnability and poor mechanical properties of filaments.

Method used

Hyaluronic acid was prepared into microcapsules, and hyaluronic acid-nylon 6 masterbatch was prepared using gelatin and gum arabic as wall materials. Hyaluronic acid-nylon 6 filaments were prepared by screw extrusion granulation and spinning process. Ethylene-vinyl acetate copolymer was used as a dispersant to ensure that the hyaluronic acid microcapsules were uniformly dispersed in the nylon 6 fibers.

Benefits of technology

The stability and uniform dispersion of hyaluronic acid in textile materials were achieved, maintaining the spinnability and excellent mechanical properties of the fibers. The breaking strength and elongation at break of the prepared filaments reached 3.89–4.02 cN/dtex and 26.31–28.02%, respectively.

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Abstract

The application relates to the technical field of textile materials, and provides hyaluronic acid microcapsules, hyaluronic acid-polyamide 6 master batches, hyaluronic acid-polyamide 6 filaments and preparation methods. The hyaluronic acid microcapsules are prepared by taking gum arabic and gelatin as wall materials, the hyaluronic acid-polyamide 6 master batches are prepared by using the hyaluronic acid microcapsules, and then the hyaluronic acid-polyamide 6 filaments are prepared by using the hyaluronic acid-polyamide 6 master batches. The hyaluronic acid microcapsules provided by the application can be uniformly dispersed in polyamide 6 fibers, and the spinnability and mechanical properties of the fibers are not affected, and the mechanical properties of the obtained filaments are excellent. The results of examples show that the breaking strength of the hyaluronic acid-polyamide 6 DTY filaments prepared by the application is 3.89-4.02 cN / dtex, and the breaking elongation is 26.31-28.02%.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of textile materials, and particularly relates to a hyaluronic acid microcapsule, a hyaluronic acid-polyamide 6 master batch, a hyaluronic acid-polyamide 6 fiber and a preparation method. BACKGROUND

[0002] Polyamide refers to a kind of polymer containing amide bond in the molecular main chain. Schlack of German Farben Corporation discovered in 1938 that caprolactam can be ring-opening polymerized to form high molecular weight polyamide 6 (also known as PA6 or polyamide 6) in the presence of water. In 1939, polyamide 6 fiber was developed, and industrialization was realized in 1941. Polyamide 6 has excellent strength, wear resistance, elastic recovery rate and moisture absorption, and plays an important role in the fields of clothing, home textiles and industrial textiles. With the development and modification of new fibers and new varieties, the absolute output of polyamide fibers will still continue to increase in the future.

[0003] Hyaluronic acid, whose scientific name is hyaluronic acid, is a polysaccharide substance extracted from the vitreous body of the eye of a cow by Karl Meyer and John Palmer, scientists of Columbia University in the United States in 1934. It is viscous and transparent, like glass, so it is named "Hyaluronic Acid", abbreviated as "HA". HA is a white solid in normal state, and contains a large number of hydroxyl groups and other polar groups in the molecule, which can adsorb about 1000 times the weight of water, and is praised as an ideal natural moisturizing factor, and has excellent skin care and moisturizing effect. HA has obvious repair effect on cell damage caused by factors such as ultraviolet light, high temperature and scratching, can reduce the release of inflammatory cytokines, clear free radicals, promote cell migration and proliferation, and is beneficial to the recovery of normal tissue morphology. Compared with cosmetics, textiles have longer contact time and larger contact area with the human body, and the addition of cosmetic and skin care ingredients in fabrics can achieve the effect of skin care to a greater extent.

[0004] At present, the functional textile fabric containing hyaluronic acid is usually realized by the way of post-finishing auxiliary agent, but such a way cannot make the hyaluronic acid effectively fuse with the textile material, and the hyaluronic acid is easy to be lost in the process of wearing and washing. Adding hyaluronic acid to the textile raw material will cause poor spinnability and poor mechanical properties of the obtained filament. SUMMARY

[0005] Therefore, the present application provides a hyaluronic acid microcapsule, a hyaluronic acid-polyamide 6 master batch, a hyaluronic acid-polyamide 6 filament and a preparation method. In the present application, hyaluronic acid is prepared into a microcapsule, the microcapsule is prepared into a hyaluronic acid-polyamide 6 master batch, and then the hyaluronic acid-polyamide 6 master batch is used to prepare a hyaluronic acid-polyamide 6 filament, and the obtained filament has excellent mechanical properties.

[0006] In order to achieve the above-mentioned application purposes, the present application provides the following technical solutions:

[0007] A hyaluronic acid microcapsule, comprising a core material and a wall material coated on the surface of the core material; the core material is hyaluronic acid, and the wall material is gelatin and gum arabic; the mass ratio of the gelatin, gum arabic and hyaluronic acid is (0.1-0.4):(0.1-0.4):1.

[0008] The application further provides a preparation method of the hyaluronic acid microcapsule in the above-mentioned scheme, comprising the following steps:

[0009] The hyaluronic acid and an emulsifier aqueous solution are mixed to perform first emulsification, so as to obtain a first emulsified solution;

[0010] The first emulsified solution, a gelatin aqueous solution and a gum arabic aqueous solution are mixed to perform second emulsification, and the obtained second emulsified solution is subjected to spray drying, so as to obtain the hyaluronic acid microcapsule.

[0011] Preferably, the emulsifier in the emulsifier aqueous solution is Tween-80, and the mass ratio of the hyaluronic acid and the emulsifier in the emulsifier aqueous solution is (2-20):1;

[0012] The mass fraction of the emulsifier in the emulsifier aqueous solution is 20-25%, the mass fraction of the gelatin in the gelatin aqueous solution is 15-25%, and the mass fraction of the gum arabic in the gum arabic aqueous solution is 20-25%;

[0013] The temperature of the first emulsification and the second emulsification is independently 50-70 DEG C; the time of the first emulsification is 3-10 min; and the time of the second emulsification is 10-60 min.

[0014] The application further provides a hyaluronic acid-polyamide 6 master batch, which comprises hyaluronic acid microcapsules, polyamide 6 and ethylene-vinyl acetate copolymer; the mass ratio of the hyaluronic acid microcapsules, the polyamide 6 and the ethylene-vinyl acetate copolymer is (5-10):(90-95):(1-2); and the hyaluronic acid microcapsules are the hyaluronic acid microcapsules in the above-mentioned scheme or the hyaluronic acid microcapsules prepared by the preparation method in the above-mentioned scheme.

[0015] The application further provides a preparation method of the hyaluronic acid-polyamide 6 master batch in the above-mentioned scheme, comprising the following steps:

[0016] The hyaluronic acid microcapsules, polyamide 6 chips and ethylene-vinyl acetate copolymer are mixed to perform screw extrusion granulation, so as to obtain the hyaluronic acid-polyamide 6 master batch.

[0017] Preferably, the screw extrusion granulation comprises a melt plasticizing process, a screw shearing process, a water cooling and granulating process and a vacuum plasticizing process which are sequentially performed;

[0018] The melting plasticizing process includes nine heating zones, which are sequentially recorded as first section temperature zone to ninth section temperature zone according to the passing order of raw materials, the temperature of the first section temperature zone is 205-210 DEG C, the temperature of the second section temperature zone is 215-225 DEG C, the temperature of the third section temperature zone is 220-230 DEG C, the temperature of the fourth section temperature zone is 240-250 DEG C, the temperature of the fifth section temperature zone is 220-230 DEG C, the temperature of the sixth section temperature zone is 200-210 DEG C, the temperature of the seventh section temperature zone, the eighth section temperature zone and the ninth section temperature zone is independently 180-200 DEG C;

[0019] The main machine rotating speed of the screw shearing process is 500-600 r / min.

[0020] The main machine rotating speed of the water cooling and pelletizing process is 900-1000 r / min.

[0021] The application further provides a hyaluronic acid-polyamide 6 filament prepared from hyaluronic acid-polyamide 6 master batch and polyamide 6 chip; the hyaluronic acid-polyamide 6 master batch is the hyaluronic acid-polyamide 6 master batch prepared by the preparation method in the above scheme; and the hyaluronic acid-polyamide 6 filament is false twist yarn.

[0022] Preferably, the mass ratio of the hyaluronic acid-polyamide 6 master batch and the polyamide 6 chip is 1:(15-25).

[0023] The application further provides a preparation method of the hyaluronic acid-polyamide 6 filament in the above scheme, which comprises the following steps:

[0024] The hyaluronic acid-polyamide 6 master batch and the polyamide chip are mixed and melt-extruded, the obtained melt is spun, and the obtained yarn is sequentially oiled and crimped to obtain hyaluronic acid-polyamide 6 pre-oriented yarn.

[0025] The hyaluronic acid-polyamide 6 pre-oriented yarn is sequentially processed through a first roller, a twist stopper, a hot box, a cooling plate, a false twister, a second roller, a third roller, an oiling device and a winding device to obtain the hyaluronic acid-polyamide 6 filament.

[0026] Preferably, the speed of the first roller, the second roller and the third roller is independently 600-700 m / min, the temperature of the hot box is 170-180 DEG C, and the D / Y ratio of the false twister is 1.6-1.8.

[0027] The hyaluronic acid microcapsule provided by the application comprises a core material and a wall material coated on the surface of the core material; the core material is hyaluronic acid, and the wall material is gelatin and gum arabic; the mass ratio of the gelatin, gum arabic and hyaluronic acid is (0.1-0.4):(0.1-0.4). The hyaluronic acid microcapsule is prepared by taking gum arabic and gelatin as the wall material, and the hyaluronic acid can be wrapped up, which is beneficial to keeping the hyaluronic acid stable and not being degraded by high temperature in the spinning process. The finally obtained hyaluronic acid microcapsule can be uniformly dispersed in the polyamide 6 fiber, and does not substantially affect the spinnability and mechanical properties of the fiber.

[0028] The application further provides a hyaluronic acid-polyamide 6 master batch, and the composition comprises hyaluronic acid microcapsules, polyamide 6 and ethylene-vinyl acetate copolymer; the mass ratio of the hyaluronic acid microcapsules, polyamide 6 and ethylene-vinyl acetate copolymer is (5-10):(90-95):(1-2). The ethylene-vinyl acetate copolymer is used as a dispersant, and the hyaluronic acid microcapsules can be uniformly dispersed in the polyamide 6 master batch.

[0029] The application further provides a hyaluronic acid-polyamide 6 filament prepared from the hyaluronic acid-polyamide 6 master batch and polyamide 6 chips. The hyaluronic acid-polyamide 6 filament is prepared by using the hyaluronic acid-polyamide 6 master batch, the hyaluronic acid microcapsules can be uniformly dispersed in the polyamide 6, and the spinnability and mechanical properties of the polyamide 6 are not affected, and the mechanical properties of the obtained filament are excellent. The results of the examples show that the breaking strength of the hyaluronic acid-polyamide 6 DTY filament prepared by the application is 3.89-4.02 cN / dtex, and the breaking elongation is 26.31-28.02%. BRIEF DESCRIPTION OF DRAWINGS

[0030] Figure 1 It is a physical map of the hyaluronic acid-polyamide 6 master batch prepared in Example 1.

[0031] Figure 2 It is a physical map of the hyaluronic acid-polyamide 6 DTY filament prepared in Example 1. DETAILED DESCRIPTION

[0032] The application provides a hyaluronic acid microcapsule, which comprises a core material and a wall material coated on the surface of the core material; the core material is hyaluronic acid, and the wall material is gelatin and gum arabic; the mass ratio of the gelatin, gum arabic and hyaluronic acid is (0.1-0.4):(0.1-0.4):1.

[0033] In the application, the mass ratio of the gelatin, gum arabic and hyaluronic acid is preferably (0.2-0.3):(0.2-0.3):1, and more preferably 0.2:0.2:1.

[0034] In the application, the particle size of the hyaluronic acid microcapsule is preferably 400-600 nm.

[0035] The present application also provides a preparation method of the hyaluronic acid microcapsule.

[0036] The hyaluronic acid and the emulsifier aqueous solution are mixed to perform first emulsification, to obtain a first emulsified solution.

[0037] The first emulsified solution, the gelatin aqueous solution and the gum arabic aqueous solution are mixed to perform second emulsification, and the obtained second emulsified solution is dried to obtain the hyaluronic acid microcapsule.

[0038] In the present application, the emulsifier in the emulsifier aqueous solution is preferably Tween-80, the mass ratio of the hyaluronic acid to the emulsifier in the emulsifier aqueous solution is preferably (2-20):1, more preferably (3-15):1, and further preferably (5-10):1, and the mass fraction of the emulsifier in the emulsifier aqueous solution is preferably 20-25%, and more preferably 20-22%.

[0039] In the present application, the temperature of the first emulsification is preferably 50-70°C, and more preferably 55-65°C, and the time of the first emulsification is preferably 3-10 min, and more preferably 5-8 min.

[0040] In the present application, the mass fraction of the gelatin in the gelatin aqueous solution is preferably 15-25%, and more preferably 20%, the mass fraction of the gum arabic in the gum arabic aqueous solution is preferably 20-25%, and more preferably 20-22%, and the mass ratio of the hyaluronic acid, the gelatin in the gelatin aqueous solution and the gum arabic in the gum arabic aqueous solution is (0.1-0.4):(0.1-0.4):1, preferably (0.2-0.3):(0.2-0.3):1, and further preferably 0.2:0.2:1.

[0041] In the present application, the temperature of the second emulsification is preferably 50-70°C, and more preferably 55-65°C, the time of the second emulsification is preferably 10-60 min, and more preferably 20-40 min, and in a specific embodiment of the present application, the temperature of the obtained first emulsified solution is maintained at 50-70°C after the first emulsification, and then the gelatin aqueous solution and the gum arabic aqueous solution are added to perform the second emulsification.

[0042] In the present application, the drying method is preferably spray drying, and the conditions of the spray drying are not particularly required, and the conditions well known to those skilled in the art can be used.

[0043] The application further provides a hyaluronic acid-polyamide 6 master batch, which comprises hyaluronic acid microcapsules, polyamide 6 and ethylene-vinyl acetate copolymer; the mass ratio of the hyaluronic acid microcapsules, the polyamide 6 and the ethylene-vinyl acetate copolymer is (5-10):(90-95):(1-2), preferably (6-8):(92-94):(1.3-1.5); the mass fraction of vinyl acetate in the ethylene-vinyl acetate copolymer is preferably 55-65%, preferably 60%.

[0044] The application further provides a preparation method of the hyaluronic acid-polyamide 6 master batch described in the above scheme, which comprises the following steps:

[0045] The hyaluronic acid microcapsules, the polyamide 6 chips and the ethylene-vinyl acetate copolymer are mixed and then subjected to screw extrusion granulation to obtain the hyaluronic acid-polyamide 6 master batch.

[0046] In the application, the polyamide 6 chips are preferably polyamide 6 semi-light chips, and the mass fraction of titanium dioxide matting agent in the polyamide 6 semi-light chips is preferably 0.1%-0.2%; before use, the polyamide 6 chips are preferably subjected to powder grinding and drying in sequence, the particle size of the powder obtained by the powder grinding is preferably less than 20 μm; the drying preferably comprises a first stage and a second stage in sequence, the temperature of the first stage is preferably 50-70 ℃, and the time is preferably 5-6 h; the temperature of the second stage is preferably 100-110 ℃, and the time is preferably 2 h; the water content of the polyamide 6 powder obtained after the drying is preferably less than 0.06%.

[0047] In the application, the hyaluronic acid microcapsules are preferably dried before use, and the drying preferably comprises a first stage and a second stage in sequence, the temperature of the first stage is preferably 50-70 ℃, and the time is preferably 3-4 h; the temperature of the second stage is preferably 90-100 ℃, and the time is preferably 2 h; the water content of the hyaluronic acid microcapsules obtained after the drying is preferably less than 0.08%.

[0048] In the application, the mixing of the hyaluronic acid microcapsules, the polyamide 6 chips and the ethylene-vinyl acetate copolymer is preferably performed in a blender, the rotating speed of the mixing is preferably 100-400 r / min, and the time of the mixing is preferably 1-2 h. After the mixing, the obtained mixture is added into a twin-screw extruder for extrusion granulation.

[0049] In the present application, the screw extrusion granulation preferably comprises sequentially a melt plasticizing process, a screw shearing process, a water cooling and pelletizing process and a vacuum plasticizing process; the melt plasticizing process comprises nine heating zones, which are sequentially recorded as first section temperature zone to ninth section temperature zone according to the passing order of raw materials, the temperature of the first section temperature zone is preferably 205-210℃, more preferably 210℃, the temperature of the second section temperature zone is preferably 215-225℃, more preferably 220℃, the temperature of the third section temperature zone is preferably 220-230℃, more preferably 225℃, the temperature of the fourth section temperature zone is preferably 240-250℃, more preferably 242℃, the temperature of the fifth section temperature zone is preferably 220-230℃, more preferably 225℃, the temperature of the sixth section temperature zone is preferably 200-210℃, more preferably 205℃, the temperature of the seventh section temperature zone, the eighth section temperature zone and the ninth section temperature zone is independently preferably 180-200℃, more preferably 190℃; the temperature of the head of the melt plasticizing process is preferably 200-220℃, more preferably 210℃.

[0050] In the present application, the main machine rotating speed of the screw shearing process is preferably 500-600r / min; the main machine rotating speed of the pelletizer used in the water cooling and pelletizing process is preferably 900-1000r / min.

[0051] The present application also provides a hyaluronic acid-polyamide 6 filament prepared from hyaluronic acid-polyamide 6 masterbatch and polyamide 6 chip; the hyaluronic acid-polyamide 6 masterbatch is the hyaluronic acid-polyamide 6 masterbatch described in the above scheme or prepared by the preparation method described in the above scheme; the mass ratio of the hyaluronic acid-polyamide 6 masterbatch and the polyamide 6 chip is preferably 1:(15-25), more preferably 1:(16-20), further preferably 1:16, 1:18 or 1:19; the polyamide 6 chip is preferably polyamide 6 semi-dull chip, and the mass fraction of titanium dioxide matting agent in the polyamide 6 semi-dull chip is preferably 0.1%-0.2%.

[0052] In the present application, the hyaluronic acid-polyamide 6 filament is specifically draw textured yarn (DTY).

[0053] In the present application, the content of hyaluronic acid in the hyaluronic acid-polyamide 6 filament is preferably 100-700mg / kg.

[0054] The present application also provides a preparation method of the hyaluronic acid-polyamide 6 filament described in the above scheme, which comprises the following steps:

[0055] The hyaluronic acid-polyamide 6 masterbatch and the polyamide 6 chip are mixed and melt extruded, the obtained melt is spun, and the obtained yarn is sequentially oiled and crimped to form a hyaluronic acid-polyamide 6 pre-oriented yarn (i.e. hyaluronic acid-polyamide 6 POY filament);

[0056] The hyaluronic acid-polyamide 6 pre-oriented yarn is sequentially processed through a first roller, a twist stopper, a hot box, a cooling plate, a false twister, a second roller, a third roller, oiling and a winding device to obtain hyaluronic acid-polyamide 6 filament (i.e. hyaluronic acid-polyamide 6 false twist elastic yarn, also known as hyaluronic acid-polyamide 6 DTY filament).

[0057] In the present application, the melt extrusion is preferably performed in a screw extruder, and the temperature of the melt extrusion is preferably 253-263°C; the present application preferably feeds the hyaluronic acid-polyamide 6 master batch and polyamide 6 chips into the screw extruder after metering by a metering feeder.

[0058] In the present application, the spinning is preferably performed in a spinning assembly, the melt is metered by a metering pump and then enters the spinning assembly, is sprayed out through a spinneret to form a filament bundle, and the filament bundle is cooled by side blowing to obtain filament (as-spun yarn); in the present application, the number of holes on the spinneret is preferably 72F, the temperature of the side blowing cooling is preferably 15-25°C, the humidity is preferably 80-95%, and the wind speed is preferably 0.4-0.7 m / s.

[0059] In the present application, the oiling agent for the oiling of the filament bundle obtained by melt spinning is preferably bamboo 5178 with a mass fraction of 5%; the obtained filament bundle after oiling is crimped and formed by a pre-networker and a godet; the production speed of the crimping is preferably 4000-4500 m / min.

[0060] After obtaining the hyaluronic acid-polyamide 6 pre-oriented yarn, the present application sequentially processes the hyaluronic acid-polyamide 6 pre-oriented yarn through a first roller, a twist stopper, a hot box, a cooling plate, a false twister, a second roller, a third roller, oiling and a winding device to obtain hyaluronic acid-polyamide 6 false twist elastic yarn (hyaluronic acid-polyamide 6 DTY filament); the speed of the first roller, the second roller and the third roller is preferably 600-700 m / min, the temperature of the hot box is preferably 170-180°C, the D / Y ratio of the false twister is preferably 1.6-1.8, and the oiling agent for the oiling is preferably bamboo 5178 with a mass fraction of 5%.

[0061] The technical solutions in the present application will be clearly and completely described below in combination with the embodiments in the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the protection scope of the present application.

[0062] Example 1

[0063] Preparation of hyaluronic acid microcapsules: A 20 wt% gelatin aqueous solution, a 20 wt% gum arabic aqueous solution, and a 3.2 wt% Tween-80 aqueous solution were prepared. Hyaluronic acid and the Tween-80 aqueous solution were emulsified in an emulsification tank with stirring for 5 minutes at 50°C. The mass ratio of hyaluronic acid to Tween-80 was 5:1. Then, the gelatin and gum arabic aqueous solutions were slowly added and emulsified together for 30 minutes. The mass ratio of gelatin, gum arabic, and hyaluronic acid was 0.2:0.2:1. Finally, the hyaluronic acid microcapsule suspension was dried using a spray dryer to obtain hyaluronic acid microcapsule powder with gelatin and gum arabic as the wall material and hyaluronic acid as the core material.

[0064] Preparation of hyaluronic acid-nylon 6 masterbatch: Semi-dull nylon 6 chips were ground into powder with a particle size of less than 20 μm. The resulting powder was dried at 55℃ for 6 h, then heated to 105℃ and held for 2 h to ensure thorough drying, resulting in a nylon 6 powder moisture content of less than 0.06%. Hyaluronic acid microcapsule powder was dried at 50℃ for 3.5 h, then heated to 90℃ and held for 2 h to ensure thorough drying, resulting in a hyaluronic acid microcapsule powder moisture content of less than 0.08%. Ethylene-vinyl acetate copolymer (EVA, in which the mass fraction of vinyl acetate is 60%) was selected as the dispersant. The dried hyaluronic acid microcapsule powder, dried nylon 6 powder, and EVA were mixed in a mass ratio of 6:93:1 and stirred in a mixer for 1.5 h at a speed of 320 r / min. After thorough mixing, the mixture was fed into a twin-screw extruder and subjected to melt plasticizing, screw shearing, water-cooled pelletizing, and vacuum drying processes to finally obtain the hyaluronic acid-nylon 6 masterbatch. The temperature control for each melting and plasticizing zone is as follows: Zone 1: 210℃; Zone 2: 220℃; Zone 3: 225℃; Zone 4: 242℃; Zone 5: 225℃; Zone 6: 205℃; Zones 7, 8, and 9: 190℃; Die head zone: 210℃. The screw shearing unit rotates at 550 r / min; the water-cooled pelletizer rotates at 900 r / min. Figure 1 This is a photograph of the hyaluronic acid-nylon 6 masterbatch prepared in this embodiment.

[0065] Preparation of hyaluronic acid-polyamide 6 filament: 1 part of hyaluronic acid-polyamide 6 master batch and 19 parts of polyamide 6 semi-dull chip are metered by a metering feeder and then sent into a screw extruder, mixed and extruded after being fully melted, and the temperature of the screw extruder is 256°C; the melt is metered by a metering pump, enters a spinning assembly, and is sprayed through a spinneret to form a filament bundle, the number of holes on the spinneret is 72F; the filament bundle is cooled by side blowing, the side blowing cooling temperature is 18°C, the humidity is 85%, and the wind speed is 0.42 m / s; the post-filament is oiled by an oil nozzle to form a bundle after being metered by an oil agent, and the oil agent used is 5% Zhumen 5178; the oiled filament bundle is crimped into shape through a pre-networker, a godet, and a production speed is 4200 m / min, and hyaluronic acid-polyamide 6 POY filament is obtained. The hyaluronic acid-polyamide 6 POY filament is subjected to a first roller, a twist stopper, a hot box, a cooling plate, a false twister, a second roller, a third roller, oiling, and a winding device, and hyaluronic acid-polyamide 6 DTY filament is prepared, the speed of the first roller, the second roller, and the third roller is all 620 m / min, the temperature of the hot box is 172°C, and the D / Y ratio of the false twister is 1.62. Figure 2 A physical map of the hyaluronic acid-polyamide 6 DTY filament prepared in this example.

[0066] Example 2

[0067] The preparation method of the hyaluronic acid-polyamide 6 master batch is the same as in Example 1.

[0068] The preparation method of the hyaluronic acid-polyamide 6 filament is as follows: 1 part of hyaluronic acid-polyamide 6 master batch and 18 parts of polyamide 6 semi-dull chip are metered by a metering feeder and then sent into a screw extruder, mixed and extruded after being fully melted, and the temperature of the screw extruder is 255°C; the melt is metered by a metering pump, enters a spinning assembly, and is sprayed through a spinneret to form a filament bundle, the number of holes on the spinneret is 72F; the filament bundle is cooled by side blowing, the side blowing cooling temperature is 16°C, the humidity is 85%, and the wind speed is 0.41 m / s; the post-filament is oiled by an oil nozzle to form a bundle after being metered by an oil agent, and the oil agent used is 5% Zhumen 5178; the oiled filament bundle is crimped into shape through a pre-networker, a godet, and a production speed is 4100 m / min, and hyaluronic acid-polyamide 6 POY filament is obtained. The hyaluronic acid-polyamide 6 POY filament is subjected to a first roller, a twist stopper, a hot box, a cooling plate, a false twister, a second roller, a third roller, oiling, and a winding device, and hyaluronic acid-polyamide 6 DTY filament is prepared, the speed of the first roller, the second roller, and the third roller is all 610 m / min, the temperature of the hot box is 170°C, and the D / Y ratio of the false twister is 1.68.

[0069] Example 3

[0070] The preparation method of the hyaluronic acid-polyamide 6 master batch is the same as in Example 1.

[0071] The preparation method of hyaluronic acid-polyamide 6 filament: 1 part of hyaluronic acid-polyamide 6 master batch and 16 parts of polyamide 6 semi-light slice are metered by a metering feeder and then sent into a screw extruder. Other spinning processes are the same as those in Example 2.

[0072] Performance test:

[0073] The fineness, breaking strength, elongation at break, crimp shrinkage, network degree and hyaluronic acid content of the hyaluronic acid-polyamide 6 DTY filaments obtained in Examples 1-3 are tested, and the results are shown in Table 1.

[0074] Table 1: Performance test results of hyaluronic acid-polyamide 6 DTY filaments

[0075]

[0076]

[0077] According to the data in Table 1, it can be seen that the hyaluronic acid-polyamide 6 DTY filaments prepared by the present application have excellent mechanical properties, which indicates that the hyaluronic acid microcapsules prepared by using gelatin and gum arabic as wall materials can be uniformly dispersed in the polyamide 6 fibers and do not affect the spinnability and mechanical properties of the fibers.

[0078] The above only describes the preferred embodiments of the present application, and it should be noted that those skilled in the art can make several improvements and refinements without departing from the principles of the present application, and these improvements and refinements should also be considered within the protection scope of the present application.

Claims

1. A hyaluronic acid-nylon 6 filament, characterized in that, It is prepared from hyaluronic acid-nylon 6 masterbatch and nylon 6 chips; the hyaluronic acid-nylon 6 masterbatch is composed of hyaluronic acid microcapsules, nylon 6 and ethylene-vinyl acetate copolymer; the mass ratio of hyaluronic acid microcapsules, nylon 6 and ethylene-vinyl acetate copolymer is (5-10):(90-95):(1-2); the hyaluronic acid microcapsules include a core material and a wall material covering the surface of the core material; the core material is hyaluronic acid, and the wall material is gelatin and gum arabic; the mass ratio of gelatin, gum arabic and hyaluronic acid is (0.1-0.4):(0.1-0.4):1; the hyaluronic acid-nylon 6 filament is false-twisted elastic yarn; The preparation method of the hyaluronic acid-nylon 6 masterbatch includes the following steps: Hyaluronic acid microcapsules, nylon 6 chips and ethylene-vinyl acetate copolymer were mixed and then granulated by screw extrusion to obtain the hyaluronic acid-nylon 6 masterbatch. The screw extrusion granulation process includes sequentially performed melt plasticizing, screw shearing, water-cooled pelletizing, and vacuum plasticizing processes. The melting and plasticizing process includes nine heating zones, which are sequentially labeled as the first to the ninth temperature zone according to the order in which the raw materials pass through. The temperature of the first temperature zone is 205–210°C, the temperature of the second temperature zone is 215–225°C, the temperature of the third temperature zone is 220–230°C, the temperature of the fourth temperature zone is 240–250°C, the temperature of the fifth temperature zone is 220–230°C, the temperature of the sixth temperature zone is 200–210°C, and the temperatures of the seventh, eighth, and ninth temperature zones are independently 180–200°C. The preparation method of the hyaluronic acid-nylon 6 filament includes the following steps: Hyaluronic acid-nylon 6 masterbatch and nylon 6 chips are mixed and melt-extruded. The resulting melt is spun into fibers. The resulting fiber bundles are then oiled and crimped to obtain hyaluronic acid-nylon 6 pre-oriented yarn. The hyaluronic acid-nylon 6 pre-oriented yarn is processed sequentially through a first roller, an anti-twist device, a hot box, a cooling plate, a false twister, a second roller, a third roller, an oiling device, and a winding device to obtain hyaluronic acid-nylon 6 filament. The melt extrusion temperature is 253-263℃; the crimping production speed is 4000-4500 m / min; the speeds of the first, second, and third rollers are independently 600-700 m / min; the temperature of the hot box is 170-180℃; and the D / Y ratio of the false twister is 1.6-1.

8.

2. The hyaluronic acid-nylon 6 filament according to claim 1, characterized in that, The preparation method of the hyaluronic acid microcapsules includes the following steps: Hyaluronic acid and an emulsifier aqueous solution are mixed and emulsified to obtain a first emulsion. The first emulsion, gelatin aqueous solution, and gum arabic aqueous solution are mixed for a second emulsification, and the resulting second emulsion is spray-dried to obtain the hyaluronic acid microcapsules.

3. The hyaluronic acid-nylon 6 filament according to claim 2, characterized in that, The emulsifier in the emulsifier aqueous solution is Tween-80, and the mass ratio of hyaluronic acid to the emulsifier in the emulsifier aqueous solution is (2-20):1; The emulsifier aqueous solution contains 20-25% emulsifier by mass; the gelatin aqueous solution contains 15-25% gelatin by mass; and the gum arabic aqueous solution contains 20-25% gum arabic by mass. The temperatures for the first and second emulsifications are independently 50–70°C; the time for the first emulsification is 3–10 min; and the time for the second emulsification is 10–60 min.

4. The hyaluronic acid-nylon 6 filament according to claim 1, characterized in that, The main machine speed in the screw shearing process is 500-600 r / min; The main rotation speed of the pelletizer used in the water-cooled pelletizing process is 900-1000 r / min.

5. The hyaluronic acid-nylon 6 filament according to claim 1, characterized in that, The mass ratio of the hyaluronic acid-nylon 6 masterbatch to the nylon 6 chips is 1:(15-25).

6. The method for preparing hyaluronic acid-nylon 6 filament according to any one of claims 1 to 5, characterized in that, Includes the following steps: Hyaluronic acid-nylon 6 masterbatch and nylon 6 chips are mixed and melt-extruded. The resulting melt is spun into fibers. The resulting fiber bundles are then oiled and crimped to obtain hyaluronic acid-nylon 6 pre-oriented yarn. The hyaluronic acid-nylon 6 pre-oriented yarn is processed sequentially through a first roller, an anti-twist device, a hot box, a cooling plate, a false twister, a second roller, a third roller, an oiling device, and a winding device to obtain hyaluronic acid-nylon 6 filament. The melt extrusion temperature is 253-263℃; the crimping production speed is 4000-4500 m / min; the speeds of the first, second, and third rollers are independently 600-700 m / min; the temperature of the hot box is 170-180℃; and the D / Y ratio of the false twister is 1.6-1.8.

Citation Information

Patent Citations

  • Hyaluronic acid microcapsule, fiber containing hyaluronic acid microcapsule, preparation method and application

    CN112094419A

  • Preparation method of composite fibers capable of being gelatinized

    CN113699619A

  • Anti-wrinkle shrink-proof wool knitted fabric

    CN216032901U