A method of making a matte cellulose hairpiece fiber

CN118257008BActive Publication Date: 2026-09-18YIBIN HIEST FIBER +1
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Patent Information

Application Number
CN202211688782.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-28
Publication Date
2026-09-18
Estimated Expiration
2042-12-28

AI Technical Summary

Technical Problem

然而,消光剂的加入会对纺丝工艺造成一定的影响,不仅会增加工艺难度,还会导致纤维强度的下降

Benefits of technology

一、与现有纤维素假发纤维的制备方法相比,本发明具有显著的技术进步,首先,本发明采用低温碱/尿素的溶剂体系,通过绿色的再生方式制备出纤维素假发纤维,与传统粘胶纤维素假发纤维相比,本方法不会损害人体健康,制备过程环保无污染,且产品亲肤性更好;其次,本发明采用双纺丝浴的方式,一浴为柠檬酸/柠檬酸钠/PEG200混合水溶液,二浴为硫酸水溶液,通过一步法直接制备出哑光纤维素假发纤维,无需添加消光剂,解决了添加消光剂对纺丝工艺带来的不良影响,简化了传统需添加消光剂制备无光纤维的制备工艺,且获得的纤维性能优异,适合于工业化生产。

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Abstract

The application discloses a preparation method of a matte cellulose wig fiber, comprising a spinning solution preparation and a spinning process, the spinning solution preparation: adding cellulose with a copper viscosity of 5-6.5 Pa.s into an alkali / urea / ZnO aqueous solution, mixing thoroughly, freezing to-12-15 DEG C, and then grinding by stirring to prepare a cellulose solution; the spinning process: after the cellulose solution is extruded from a large-hole nozzle, the cellulose solution is reacted with a first coagulating bath and a second coagulating bath, primary fiber tows are obtained after forming, then the primary fiber tows are wound into fiber tows by a winding device, and then the fiber tows are washed and dried to obtain the matte cellulose wig fiber. The matte cellulose wig fiber is directly prepared by the one-step method without adding a matting agent, the adverse effects of adding the matting agent on the spinning process are solved, the preparation process of the conventional matte fiber prepared by adding the matting agent is simplified, and the obtained fiber has excellent performance and is suitable for industrialized production.
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Description

Technical Field

[0001] This invention belongs to the field of solvent-spun cellulose production technology, specifically relating to a matte cellulose wig fiber and its preparation method. Background Technology

[0002] With the improvement of people's living standards, wigs have become a part of our daily lives as a consumer product. Hair loss has become a global problem, and wigs are no longer just a fashion trend but also a necessity. As the wig industry expands, market demand for wigs is increasing. Wigs made from human hair are becoming increasingly scarce and expensive, unable to meet market demand. Therefore, the production and processing of artificial wigs is expanding. While artificial wigs made from chemical fibers are inexpensive, they lack realism and the smoothness of real hair is far inferior. Furthermore, they may cause scalp allergies and other skin problems when worn. Cellulose, as the most abundant renewable resource on Earth, has excellent renewability, environmental friendliness, biocompatibility, and biodegradability. Renewable fibers made from cellulose are a very promising wig material, not only inexpensive but also environmentally friendly. However, renewable cellulose fibers have a high gloss, and to achieve a more realistic effect, matte agents (such as titanium dioxide and protein solutions) are often added to prepare matte cellulose fibers. However, the addition of matting agents can have a certain impact on the spinning process, not only increasing the difficulty of the process but also leading to a decrease in fiber strength. Summary of the Invention

[0003] To address the aforementioned problems, this invention provides a method for preparing matte cellulose wig fibers. The objective of this invention is achieved through the following technical solution: A method for preparing matte cellulose wig fibers, comprising spinning solution preparation and spinning process, characterized in that: (1) Preparation of spinning solution: Add cellulose with a copper viscosity of 5~6.5 Pa·s to an alkali / urea / ZnO aqueous solution and mix thoroughly. Freeze to -12~15℃ and then prepare cellulose solution by stirring and grinding. (2) Spinning process: The cellulose solution is extruded from the large-hole nozzle and reacted with the first coagulation bath and the second coagulation bath. After molding, the nascent fiber bundle is obtained, which is then wound into a bundle by a winding device. After washing and drying, matte cellulose wig fiber is obtained.

[0004] Preferably, the degree of polymerization of the cellulose is 330-410.

[0005] Preferably, the alkali / urea / ZnO aqueous solution contains 7-8% sodium hydroxide, 11-15% urea, and 0.8-1.2 wt% zinc oxide.

[0006] Preferably, the cellulose solution has a falling ball viscosity of 45-60 seconds, a cellulose content of 5.5-6.5%, an alkali content of 7-8%, and a urea content of 11-15%.

[0007] Preferably, the orifice diameter of the large-hole nozzle is 0.1-0.2 mm, and the raw material of the large-hole nozzle is platinum:gold = 4:6.

[0008] Preferably, in the spinning process, the single filament fineness is 30D-100D, the spinning speed is 40-50 m / min, and the total draw is 5-10%.

[0009] Preferably, the coagulation solution in the first coagulation bath is a mixed aqueous solution of 15 wt% citric acid, 5 wt% sodium citrate, and 40 wt% PEG200.

[0010] Preferably, the coagulation solution in the second coagulation bath is an 8 wt% sulfuric acid aqueous solution.

[0011] Preferably, the temperatures of the first and second coagulation baths are 20-25°C.

[0012] A matte cellulose wig fiber with a single filament fineness of 30D-100D.

[0013] The beneficial effects of this technical solution are as follows: I. Compared with existing methods for preparing cellulose wig fibers, this invention represents a significant technological advancement. First, this invention employs a low-temperature alkali / urea solvent system to prepare cellulose wig fibers through a green regeneration process. Compared to traditional viscose cellulose wig fibers, this method does not harm human health, the preparation process is environmentally friendly and pollution-free, and the product has better skin-friendliness. Second, this invention uses a dual-spinning bath method: the first bath is a mixed aqueous solution of citric acid / sodium citrate / PEG200, and the second bath is an aqueous solution of sulfuric acid. This allows for the direct one-step preparation of matte cellulose wig fibers without the need for matting agents. This solves the problem of the adverse effects of adding matting agents on the spinning process, simplifies the traditional preparation process that requires the addition of matting agents to prepare matte fibers, and yields fibers with excellent properties suitable for industrial production.

[0014] II. This invention employs a dual-bath spinning process, where the first bath is a mixed aqueous solution of citric acid / sodium citrate / PEG200, and the second bath is an aqueous solution of sulfuric acid. Because the first coagulation bath uses a weak acid and contains PEG200 to delay the regeneration reaction, the fluid resistance of the coagulation bath increases. Therefore, the formation of the filaments in the first coagulation bath is primarily due to dual diffusion, which disrupts the original solvent components, causing cellulose to precipitate and solidify. This is not due to a neutralization reaction between the acid in the coagulation bath and the alkali in the solvent. During this process, since the alkali in the solvent is not neutralized by the acid in the coagulation bath, the ZnO in the solvent does not completely react with the acid and remains inside the fiber. In the first coagulation bath, the outer surface of the fiber solidifies first, encapsulating the ZnO in the solvent within the fiber. Therefore, in the second coagulation bath, after the filaments have fully reacted and solidified in the sulfuric acid aqueous solution, the ZnO remains unreacted, thus giving the filaments a natural matte finish, resulting in matte fibers. This invention directly prepares matte cellulose wig fibers in one step without the need for adding matting agents, thus solving the adverse effects of adding matting agents on the spinning process. It simplifies the traditional preparation process that requires the addition of matting agents to prepare matte fibers, and the resulting fibers have excellent properties and are suitable for industrial production. Detailed Implementation

[0015] Examples 1, 2, and 3, as well as Comparative Examples 1, 2, and 3, all employed the following testing methods: Dry breaking strength and dry breaking elongation were tested by taking a certain length of dry fiber sample and stretching it using a fiber strength testing machine at a constant rate of elongation until it broke. The strength and elongation at break were measured, and the dry breaking strength was calculated from the breaking strength and linear density. Whether the fiber exhibits a matting effect can be observed visually.

[0016] Example 1 A method for preparing matte cellulose wig fibers, comprising spinning solution preparation and spinning process, characterized in that: (1) Preparation of spinning solution: cellulose with a copper viscosity of 5 Pa·s (degree of polymerization of cellulose is 330) is added to an alkali / urea / ZnO aqueous solution and mixed thoroughly. The mixture is then frozen to -12°C and then stirred and ground to prepare a cellulose solution. The cellulose solution has a falling ball viscosity of 45 seconds, a cellulose content of 6.5%, a sodium hydroxide content of 7%, and a urea content of 11%. (2) Spinning process: The cellulose solution is extruded through a large-hole nozzle and reacted with the first coagulation bath and the second coagulation bath. The aperture of the large-hole nozzle is 0.1 mm. The raw material of the large-hole nozzle is platinum: gold = 4:6. The coagulation solution in the first coagulation bath is a mixed aqueous solution of 15 wt% citric acid, 5 wt% sodium citrate and 40 wt% PEG200. The coagulation solution in the second coagulation bath is an aqueous solution of 8 wt% sulfuric acid. The temperature of the first coagulation bath and the second coagulation bath is 20℃. The single filament fineness is 30D, the spinning speed is 40 m / min, the total draw is 5%, and the initial fiber bundle is obtained after forming. Then, it is wound into a bundle by a winding device, and after washing and drying, matte cellulose wig fiber is obtained. The fiber strength is 1.66 cN / dtex, the elongation is 13.2%, and it has a matting effect.

[0017] Example 2 A method for preparing matte cellulose wig fibers, comprising spinning solution preparation and spinning process, characterized in that: (1) Preparation of spinning solution: cellulose with a copper viscosity of 6.5 Pa·s (degree of polymerization of cellulose is 410) is added to an alkali / urea / ZnO aqueous solution and mixed thoroughly. The mixture is then frozen to 15°C and then stirred and ground to prepare a cellulose solution. The cellulose solution has a falling ball viscosity of 60 seconds, a cellulose content of 5.5%, a sodium hydroxide content of 8%, and a urea content of 15%. (2) Spinning process: The cellulose solution is extruded through a large-hole nozzle and reacted with the first coagulation bath and the second coagulation bath. The aperture of the large-hole nozzle is 0.2 mm. The raw material of the large-hole nozzle is platinum: gold = 4:6. The coagulation solution in the first coagulation bath is a mixed aqueous solution of 15 wt% citric acid, 5 wt% sodium citrate and 40 wt% PEG200. The coagulation solution in the second coagulation bath is an aqueous solution of 8 wt% sulfuric acid. The temperature of the first coagulation bath and the second coagulation bath is 25℃. The single filament fineness is 50D, the spinning speed is 50 m / min, the total draw is 10%, and the initial fiber bundle is obtained after forming. Then, it is wound into a bundle by a winding device, and after washing and drying, matte cellulose wig fiber is obtained. The fiber strength is 1.52 cN / dtex, the elongation is 14.1%, and it has a matting effect.

[0018] Example 3 A method for preparing matte cellulose wig fibers, comprising spinning solution preparation and spinning process, characterized in that: (1) Preparation of spinning solution: cellulose with a copper viscosity of 6 Pa·s (degree of polymerization of cellulose is 370) was added to an alkali / urea / ZnO aqueous solution and mixed thoroughly. The mixture was then frozen to 2°C and then stirred and ground to prepare a cellulose solution. The cellulose solution had a falling ball viscosity of 55 seconds, a cellulose content of 6.3%, a sodium hydroxide content of 8%, and a urea content of 11%. (2) Spinning process: The cellulose solution is extruded through a large-hole nozzle and reacted with the first coagulation bath and the second coagulation bath. The aperture of the large-hole nozzle is 0.15 mm. The raw material of the large-hole nozzle is platinum: gold = 4:6. The coagulation solution in the first coagulation bath is a mixed aqueous solution of 15 wt% citric acid, 5 wt% sodium citrate and 40 wt% PEG200. The coagulation solution in the second coagulation bath is an aqueous solution of 8 wt% sulfuric acid. The temperature of the first coagulation bath and the second coagulation bath is 23℃. The single filament fineness is 100D, the spinning speed is 45 m / min, the total draw is 7%, and the initial fiber bundle is obtained after forming. Then, it is wound into a bundle by a winding device, and after washing and drying, matte cellulose wig fiber is obtained. The fiber strength is 1.48 cN / dtex, the elongation is 12.3%, and it has a matting effect.

[0019] Comparative Example 1 The difference between this comparative example and the embodiment is that a coagulation bath is used to regenerate the fibers, specifically an 8 wt% sulfuric acid aqueous solution, to regenerate the cellulose fibers through an acid-base neutralization reaction. The cellulose wig fibers have a fiber strength of 1.51 cN / dtex, an elongation of 11.2%, and do not have a matting effect.

[0020] Comparative Example 2 The difference between this comparative example and Example 2 is that a coagulation bath is used to regenerate the fibers, specifically an 8 wt% sulfuric acid aqueous solution, to regenerate the cellulose fibers through an acid-base neutralization reaction. The cellulose wig fibers have a fiber strength of 1.44 cN / dtex, an elongation of 9.8%, and do not possess a matting effect.

[0021] Comparative Example 3 The difference between this comparative example and Example 3 is that a coagulation bath is used to regenerate the fibers, specifically an 8 wt% sulfuric acid aqueous solution, to regenerate the cellulose fibers through an acid-base neutralization reaction. The cellulose wig fibers have a strength of 1.35 cN / dtex, an elongation of 7.4%, and do not possess a matting effect.

[0022] As shown above, using only one coagulation bath—that is, sulfuric acid aqueous solution—to regenerate cellulose fibers through acid-base neutralization, cannot achieve a matting effect. The dual-bath method is crucial for achieving a matting effect during fiber preparation. Only by using a dual-bath approach—with a mixed aqueous solution of citric acid / sodium citrate / PEG200 in the first bath and a sulfuric acid aqueous solution in the second bath—can fibers with a matting effect be obtained, and the fiber's strength and other properties also improve.

[0023] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above descriptions are merely specific embodiments of the present invention and are not intended to limit the present invention. 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 method for preparing matte cellulose wig fibers, characterized in that, Includes the following steps: (1) Preparation of spinning solution: Add cellulose with a copper viscosity of 5~6.5 Pa·s to an alkali / urea / ZnO aqueous solution and mix thoroughly. Freeze to -12~15℃ and then prepare cellulose solution by stirring and grinding. The degree of polymerization of the cellulose is 330-410. (2) Spinning process: The cellulose solution is extruded through a large-hole nozzle and reacted with the first coagulation bath and the second coagulation bath. After molding, nascent fiber bundles are obtained, which are then wound into bundles by a winding device. After washing and drying, matte cellulose wig fibers are obtained. The coagulation solution in the first coagulation bath is a mixed aqueous solution of 15 wt% citric acid, 5 wt% sodium citrate and 40 wt% PEG200. The alkali / urea / ZnO aqueous solution contains 7-8 wt% sodium hydroxide, 11-15 wt% urea, and 0.8-1.2 wt% zinc oxide. The cellulose solution has a falling ball viscosity of 45-60 seconds, a cellulose content of 5.5-6.5 wt%, an alkali content of 7-8 wt%, and a urea content of 11-15 wt%. The orifice diameter of the large-aperture nozzle is 0.1-0.2 mm; in the spinning process, the single filament fineness is 30D-100D, the spinning speed is 40-50 m / min, and the total draw is 5-10%; The coagulation solution in the second coagulation bath is an 8 wt% sulfuric acid aqueous solution; The temperatures of the first and second coagulation baths are 20-25℃.

Citation Information

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