Durable hydrophobic cellulosic fiber sliver yarn and method of making same

Abstract

The application relates to the technical field of modified bobbin yarn preparation, and particularly discloses a durable hydrophobic cellulose fiber bobbin yarn and a preparation method thereof, specifically as follows: S1, completely immersing natural cotton fibers in a hydrophobic treatment solution, reacting for 23-24 hours, washing, drying to obtain rough treated cotton fibers; completely immersing the rough treated cotton fibers in a dehydrated ethanol solution of heptadecafluorodecyltriethoxysilane, then reacting at a temperature of 48-52 DEG C for 4.5-5 hours, washing, drying to obtain hydrophobic cotton fibers; S2, uniformly dispersing the hydrophobic cotton fibers and coated particles in dehydrated ethanol, the weight ratio of the hydrophobic cotton fibers and the coated particles being (50-55):(11.5-12.0), then reacting at a temperature of 60-65 DEG C for 5-6 hours, washing, drying to obtain durable hydrophobic cotton fibers; S3, weaving fibers. The product can be used as a raw material of protective clothing fabric, and has the advantages of durability and hydrophobicity.

Description

Technical Field

[0001] This application relates to the technical field of modified yarn package preparation, and in particular to a durable hydrophobic cellulose fiber yarn package and its preparation method. Background Technology

[0002] Yarn cones are a common type of textile. They are formed by winding yarn onto a bobbin for ease of use, transportation, and storage. Yarn cones are characterized by their tight weave and fine individual fibers, and are often used as raw materials for clothing and home furnishings. Yarn cones contribute excellent abrasion resistance and softness to the final fabric.

[0003] As the manufacturing process and procedures for yarn cones have matured, their abrasion resistance and softness have been further improved. Therefore, some technicians are considering using them as raw materials for protective clothing fabrics. However, protective clothing fabrics have high waterproofing requirements, necessitating waterproofing treatment of the yarn cones to obtain waterproof yarn cones. Current waterproofing treatments mainly involve adding the yarn cones to a mixed solution of organic alkali and organic solvent, and carrying out a grafting reaction under inert gas protection to ultimately obtain hydrophobic yarn cones. However, since the yarn cones themselves are already highly textile-compatible and structurally complex, the industrial application conditions for grafting reactions are quite demanding and unsuitable for mass production.

[0004] In response to the above problems, some technicians have pointed out that the raw materials for preparing yarn packages, namely cellulose fibers (usually cotton fibers), can be modified before they are set. This can improve the hydrophobic effect of the yarn packages by addressing the chemical properties of the fibers. However, a series of experiments have shown that modifying the fibers themselves to be hydrophobic can severely affect the tensile strength of the fibers, which greatly reduces the service life of the yarn packages, making it impossible for them to meet the requirements for durability. Summary of the Invention

[0005] To address the aforementioned technical problems, this application provides a durable hydrophobic cellulose fiber yarn and its preparation method.

[0006] In a first aspect, this application provides a method for preparing durable hydrophobic cellulose fiber packaged yarn, employing the following technical solution:

[0007] A method for preparing a durable hydrophobic cellulose fiber package yarn includes the following steps:

[0008] S1, hydrophobic treatment

[0009] S11. A hydrophobic treatment agent is obtained by mixing tromethamine and dopamine hydrochloride in a weight ratio of (14.2-15.6):(23.0-24.5). The hydrophobic treatment agent is then dispersed in water to obtain a hydrophobic treatment solution with a concentration of 36.2-37.0 wt%. Natural cotton fibers are completely immersed in the hydrophobic treatment solution and reacted for 23-24 hours. After rinsing and drying, coarsely treated cotton fibers are obtained.

[0010] S12. The coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 24-25 wt%, and then reacted at a temperature of 48-52℃ for 4.5-5 hours. After rinsing and drying, hydrophobic cotton fibers are obtained.

[0011] S2, Durability Treatment

[0012] S21. While stirring, disperse silica particles and polydopamine in anhydrous ethanol. The weight ratio of silica particles to polydopamine is (7.6-8.4):(16.0-16.2). Then, react under inert gas protection and at a reaction temperature of 48-50℃ for 25-26 hours. After centrifugation and drying, the coated particles are obtained.

[0013] S22. The hydrophobic cotton fiber obtained in step S12 and the coated particles obtained in step S21 are uniformly dispersed in anhydrous ethanol. The weight ratio of the hydrophobic cotton fiber to the coated particles is (50-55):(11.5-12.0). Then, the mixture is reacted at 60-65℃ for 5-6 hours. After rinsing and drying, durable hydrophobic cotton fiber is obtained.

[0014] S3, Fiber weaving

[0015] The durable hydrophobic cellulose fiber obtained in step S22 is processed by opening, carding, drawing, roving, spinning, and winding to obtain durable hydrophobic cellulose fiber package yarn.

[0016] By adopting the above technical solution, this application mixes polydopamine with high-strength adhesiveness and silica particles with large mesh size and high structural stability, and then reacts them to obtain coating particles with a large mesh size. The stirring treatment during the reaction can promote a more uniform and tighter bonding between the two, so that the coating particles have both the high structural stability of silica particles and the adhesiveness of polydopamine, resulting in a uniform internal structure. Then, this application blends the coating particles with natural cotton fibers. The coating particles adhere tightly to the surface of natural cotton fibers due to their high adhesiveness. At the same time, because the silica particles in the coating particles have a large mesh size (280-290 mesh) and extremely high structural stability, and natural cotton fibers have a rough surface structure, the coating particles can adhere to the surface of natural cotton fibers very uniformly and deeply. Through their own high structural stability, they bring high tensile strength to natural cotton fibers, effectively improving the service life of natural cotton fibers, thus obtaining durable natural cotton fibers.

[0017] Secondly, this application also uses a hydrophobic treatment agent obtained by uniformly mixing tromethamine and dopamine hydrochloride to perform hydrophobic modification treatment on natural cotton fibers. Tromethamine is used to enhance the chemical activity of dopamine hydrochloride. Then, highly active dopamine hydrochloride is used to react with natural cotton fibers, generating several active groups on the surface of natural cotton fibers, resulting in coarse-treated cotton fibers with a rough surface structure and a large number of surface active groups. Then, heptadecafluorodecyltriethoxysilane is used to react with the active groups on the surface of the coarse-treated cotton fibers, forming a uniform layer of hydrophobic groups on the surface of the coarse-treated cotton fibers, thereby giving the coarse-treated cotton fibers good hydrophobic properties, thus obtaining hydrophobic cotton fibers.

[0018] Ultimately, this application involves a series of treatments on durable hydrophobic cotton fibers to improve the hydrophobicity of the yarn package without affecting its durability, resulting in durable hydrophobic cellulose fiber yarn package.

[0019] Preferably, in step S11, the weight ratio of tromethamine to dopamine hydrochloride is 14.8:24.2.

[0020] By adopting the above technical solution, this application further optimizes the weight ratio of tromethamine and dopamine hydrochloride, thereby further increasing the number of active groups generated on the surface of natural cotton fibers. If the amount of tromethamine is too large, it will affect the contact degree between dopamine hydrochloride and natural cotton fibers, reducing the number of active groups. If the amount of dopamine hydrochloride is too large, the tromethamine cannot effectively make all dopamine hydrochloride have high chemical activity. At the same time, dopamine hydrochloride without high chemical activity will hinder the contact and reaction between highly active dopamine hydrochloride and natural cotton fibers, which will also reduce the number of active groups. Experimental data shows that when the weight ratio of tromethamine to dopamine hydrochloride is 14.8:24.2, the number of active groups generated on the surface of natural cotton fibers is the largest, thus maximizing the number of hydrophobic groups on the surface of natural cotton fibers, thereby giving the coarsely treated cotton fibers good hydrophobic properties.

[0021] Preferably, in step S21, the weight ratio of silica particles to polydopamine is 8:16.16.

[0022] By adopting the above technical solution, this application further optimizes the weight ratio of silica particles and polydopamine. Without affecting the structural stability of the coated particles, it fully utilizes polydopamine to enhance its adhesion, thereby improving the tensile strength and service life of durable hydrophobic cotton fibers. If the amount of polydopamine is too large, although the adhesion of the coated particles is improved to a certain extent, the soft texture of polydopamine will affect the effect of silica particles on improving the structural stability of the coated particles, and cannot effectively improve the tensile strength and service life of durable hydrophobic cotton fibers. If the amount of silica particles is too large, polydopamine cannot effectively make all silica particles tightly bonded, and the adhesion of the coated particles will inevitably decrease. When bonding with hydrophobic cotton fibers, it is impossible to ensure that all coated particles are firmly bonded to the surface of hydrophobic cotton fibers, which not only causes a certain cost waste, but also fails to effectively improve the tensile strength and service life of durable hydrophobic cotton fibers. Experimental data have shown that when the weight ratio of silica particles to polydopamine is 8:16.16, the adhesion and structural stability of the coated particles can reach the optimal balance, thereby maximizing the tensile strength of durable hydrophobic cotton fibers.

[0023] Preferably, in step S22, after the hydrophobic cotton fibers and coating particles are uniformly dispersed in anhydrous ethanol, heptadecafluorodecyltriethoxysilane is added to the system at an amount of 48-52 wt% of the amount of coating particles, and the mixture is mixed evenly before proceeding with the subsequent reaction.

[0024] Preferably, in step S22, the amount of heptadecafluorodecyltriethoxysilane used is 49.3 wt% of the amount of coating particles.

[0025] By adopting the above technical solution, this application adds heptadecafluorodecyltriethoxysilane after mixing the hydrophobic cotton fiber and the coating particles, thereby further improving the hydrophobicity of the durable hydrophobic cotton fiber. This is because during the co-heating reaction between the hydrophobic cotton fiber and the coating particles, a small portion of the hydrophobic groups formed by the heptadecafluorodecyltriethoxysilane on the surface of the coarsely treated cotton fiber in step S12 will be affected by heat and detach from the surface of the coarsely treated cotton fiber. The heptadecafluorodecyltriethoxysilane added again in step S22 can react with the hydrophobic cotton fiber again, thereby compensating for the loss of this portion of the hydrophobic groups, so that the hydrophobicity of the durable hydrophobic cotton fiber is not affected by the temperature of the durability treatment. Experimental data shows that when the amount of heptadecafluorodecyltriethoxysilane is 49.3 wt% of the amount of coating particles, this application can maximize the compensation for the loss of hydrophobic groups without incurring additional raw material costs.

[0026] Preferably, step S3 further includes a padding process, specifically:

[0027] S31. The durable hydrophobic cellulose fiber obtained in step S22 is opened, carded, drawn, roving, and spun to obtain the durable hydrophobic cellulose fiber yarn to be treated.

[0028] S32. The durable hydrophobic cellulose fiber yarn to be treated is completely immersed in the strengthening treatment solution, and then subjected to padding treatment at a temperature of 85-90℃ for 0.15-0.2h, dried, finished, and wound to obtain durable hydrophobic cellulose fiber package yarn.

[0029] The enhanced treatment solution comprises hexadecyltrimethoxysilane, sodium phosphite, and water in a weight ratio of (12-18):(7-9):(60-85).

[0030] Preferably, the weight ratio of hexadecyltrimethoxysilane, sodium phosphite, and water is 15:8.5:76.

[0031] By adopting the above technical solution, this application first performs a padding treatment on the yarn before winding. Hexadecyltrimethoxysilane undergoes a hydrolysis reaction on the surface of the durable hydrophobic cellulose fiber yarn to be treated, generating polyhexadecyltrimethylsiloxane with high hydrophobicity, thereby further improving the hydrophobicity of the yarn. Furthermore, sodium phosphite, with its antioxidant properties, optimizes the yarn's antioxidant capacity, extending its service life. Therefore, this application uses a reinforcing treatment solution to pad the durable hydrophobic cellulose fiber yarn, which can further improve its durability and hydrophobicity. Experimental data shows that when the weight ratio of hexadecyltrimethoxysilane, sodium phosphite, and water is 15:8.5:76, this application can maximize the durability and hydrophobicity of the durable hydrophobic cellulose fiber yarn without incurring additional raw material costs.

[0032] This application effectively optimizes the treatment effect of hexadecyltrimethoxysilane and sodium phosphite on durable hydrophobic cellulose fiber yarns by controlling the temperature and time of the padding process. When the padding temperature is too low or the padding time is too short, hexadecyltrimethoxysilane and sodium phosphite cannot exert their own properties due to insufficient temperature and time, and cannot significantly optimize the treatment effect on the durable hydrophobic cellulose fiber yarns. However, if the padding temperature is too high or the padding time is too long, the high temperature will affect the polydopamine in the coating particles adhering to the surface of the durable hydrophobic cellulose fiber yarns, and some coating ions will be detached from the surface of the durable hydrophobic cellulose fiber yarns, thus reducing the durability of the durable hydrophobic cellulose fiber yarns. Experimental data shows that when the padding temperature is 88℃ and the time is 0.19h, the durability and hydrophobicity of the durable hydrophobic cellulose fiber yarns are both optimal.

[0033] Preferably, the strengthening treatment solution further includes a crosslinking agent in an amount of 63.7-86.2 g / L.

[0034] Preferably, the crosslinking agent is butanetetraacetic acid.

[0035] By adopting the above technical solution, this application adds a crosslinking agent to the strengthening treatment solution, which forms a network structure on the surface of the durable hydrophobic cellulose fiber yarn to be treated, thereby improving the durability of the durable hydrophobic cellulose fiber yarn. This application also uses butanetetraacetic acid (TTAA) as the crosslinking agent, taking advantage of its more stable physical structure compared to other crosslinking agents. Even if the final durable hydrophobic cellulose fiber yarn is crumpled or squeezed during use, TTAA can still maintain good chemical properties, further improving the durability of the durable hydrophobic cellulose fiber yarn.

[0036] Secondly, this application provides a durable hydrophobic cellulose fiber package yarn with a contact angle of 146.3-146.4°, a tensile breaking strength of 351-353N, and an elongation at break of 27.98-28.56%, exhibiting good durability and hydrophobicity.

[0037] In summary, this application has the following beneficial technical effects:

[0038] 1. In this application, natural cotton fibers are treated with a hydrophobic agent and coating particles to achieve hydrophobicity and durability when they are not finished, resulting in a contact angle of 146.3-146.4°, a tensile breaking strength of 351-353N, and an elongation at break of 27.98-28.56% for cellulose fiber package yarns, effectively improving their durability and hydrophobicity;

[0039] 2. In this application, the cellulose fiber yarn is impregnated with a reinforcing treatment solution before winding, which further improves its durable hydrophobicity. Detailed Implementation

[0040] Material source

[0041] Unless otherwise specified, all raw materials used in this application are commercially available products, specifically:

[0042] Tromethamine was purchased from Xi'an Jinxiang Pharmaceutical Excipients Co., Ltd.

[0043] Dopamine hydrochloride was purchased from Sigma-Aldrich (Shanghai) Trading Co., Ltd.

[0044] Silica granules were purchased from Qinghe County Chaotai Metal Materials Co., Ltd., model JL-SiO2-W40, with a mesh size of 300-325; polydopamine was purchased from Sigma-Aldrich (Shanghai) Trading Co., Ltd.

[0045] Anhydrous ethanol was purchased from Sinopharm Holding Co., Ltd.

[0046] Nitrogen was purchased from Chengdu Hongjin Chemical Co., Ltd.

[0047] Hexadecyltrimethoxysilane was purchased from Sinopharm Holding Co., Ltd.

[0048] Sodium phosphite was purchased from Sinopharm Holding Co., Ltd.

[0049] 2-Octenylsuccinic anhydride was purchased from Guangdong Wengjiang Chemical Reagent Co., Ltd.

[0050] Butanetetraacetic acid was purchased from Sinopharm Holding Co., Ltd.

[0051] The heptadecafluorodecyltriethoxysilane was purchased from Nanjing Quanxi Chemical Co., Ltd., with a purity of 97 wt%.

[0052] The silicone zirconium stearic acid waterproofing agent was purchased from Greenlink (Jining) Chemical Technology Co., Ltd., model YF-556.

[0053] The natural cotton fibers were purchased from Yancheng Yankang Medical Equipment Co., Ltd.

[0054] Preparation Example 1

[0055] The preparation method of the hydrophobic treatment solution includes the following steps:

[0056] 14.2 kg of tromethorphanol, 24.5 kg of dopamine hydrochloride and 65.9 kg of water were mixed evenly and stirred for 10 min to obtain a hydrophobic treatment solution with a concentration of 37.0 wt%.

[0057] Preparation Example 2

[0058] The preparation method of the hydrophobic treatment solution includes the following steps:

[0059] 15.6 kg of tromethorphan, 23.0 kg of dopamine hydrochloride and 68.0 kg of water were mixed evenly and stirred for 10 min to obtain a hydrophobic treatment solution with a concentration of 36.2 wt%.

[0060] Preparation Example 3

[0061] The preparation method of the hydrophobic treatment solution includes the following steps:

[0062] 14.8 kg of tromethorphan, 24.2 kg of dopamine hydrochloride and 66.4 kg of water were mixed evenly and stirred for 10 min to obtain a hydrophobic treatment solution with a concentration of 37.0 wt%.

[0063] Preparation Example 4

[0064] The preparation method of the hydrophobic treatment solution differs from that of Preparation Example 1 in that: 18 kg of tromethamine and 20.7 kg of dopamine hydrochloride are used, while the rest are the same as in Preparation Example 1.

[0065] Preparation Example 5

[0066] The preparation method of the hydrophobic treatment solution differs from that of Preparation Example 1 in that: 28 kg of tromethamine and 10.7 kg of dopamine hydrochloride are used, while the rest are the same as in Preparation Example 1.

[0067] Preparation Example 6

[0068] The method for preparing coated particles includes the following steps:

[0069] 7.6 kg of silica particles with a mesh size of 300 and 16.2 kg of polydopamine were uniformly dispersed in 30 kg of anhydrous ethanol. Nitrogen gas was introduced into the system, and the reaction was carried out at 48°C for 26 h. After centrifugation and drying, coated particles with a mesh size of 280 were obtained.

[0070] Preparation Example 7

[0071] The method for preparing coated particles includes the following steps:

[0072] 8.4 kg of silica particles with a mesh size of 325 and 16.0 kg of polydopamine were uniformly dispersed in 30 kg of anhydrous ethanol. Nitrogen gas was introduced into the system, and the reaction was carried out at 50 °C for 25 h. After centrifugation and drying, coated particles with a mesh size of 290 were obtained.

[0073] Preparation Example 8

[0074] The method for preparing coated particles includes the following steps:

[0075] 8.0 kg of silica particles with a mesh size of 300 and 16.16 kg of polydopamine were uniformly dispersed in 30 kg of anhydrous ethanol. Nitrogen gas was introduced into the system and the reaction was carried out at 48°C for 26 h. After centrifugation and drying, coated particles with a mesh size of 280 were obtained.

[0076] Preparation Example 9

[0077] The preparation method of the coated particles differs from that of Preparation Example 6 in that the amount of silica particles is 5.0 kg and the amount of polydopamine is 18.8 kg, while the rest are the same as those in Preparation Example 6.

[0078] Preparation Example 10

[0079] The preparation method of the coated particles differs from that of Preparation Example 6 in that: the amount of silica particles is 15 kg and the amount of polydopamine is 8.8 kg, while the rest are the same as in Preparation Example 6.

[0080] Preparation Example 11

[0081] The preparation method of the enhanced treatment solution includes the following steps:

[0082] The enhanced treatment solution was obtained by mixing 12 kg of hexadecyltrimethoxysilane, 9.0 kg of sodium phosphite and 60 kg of water evenly.

[0083] Preparation Example 12

[0084] The preparation method of the enhanced treatment solution includes the following steps:

[0085] The enhanced treatment solution was obtained by mixing 18 kg of hexadecyltrimethoxysilane, 7.0 kg of sodium phosphite and 85 kg of water evenly.

[0086] Preparation Example 13

[0087] The preparation method of the enhanced treatment solution includes the following steps:

[0088] The enhanced treatment solution was obtained by mixing 15 kg of hexadecyltrimethoxysilane, 8.5 kg of sodium phosphite and 76 kg of water evenly.

[0089] Preparation Example 14

[0090] The preparation method of the enhanced treatment solution includes the following steps:

[0091] The enhanced treatment solution was obtained by mixing 12 kg of hexadecyltrimethoxysilane, 9.0 kg of sodium phosphite, 3.82 kg of triethanolamine and 60 kg of water evenly.

[0092] Preparation Example 15

[0093] The preparation method of the enhanced treatment solution includes the following steps:

[0094] The enhanced treatment solution was obtained by mixing 12 kg of hexadecyltrimethoxysilane, 9.0 kg of sodium phosphite, 5.17 kg of triethanolamine and 60 kg of water evenly.

[0095] Preparation Example 16

[0096] The preparation method of the enhanced treatment solution differs from that of Example 14 in that triethanolamine is replaced with 2-octenylsuccinic anhydride, while the rest is the same as in Example 14.

[0097] Preparation Example 17

[0098] The preparation method of the enhanced treatment solution differs from that of Example 14 in that triethanolamine is replaced with butanetetraacetic acid, while the rest is the same as in Example 14.

[0099] Example 1.1

[0100] A method for preparing a durable hydrophobic cellulose fiber package yarn includes the following steps:

[0101] S1, hydrophobic treatment

[0102] S11. The natural cotton fiber was completely immersed in the hydrophobic treatment solution prepared in Preparation Example 1, reacted for 24 hours, rinsed repeatedly with deionized water, and dried in a dryer to obtain coarsely treated cotton fiber.

[0103] S12. All the coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 24wt%, and then reacted at 52℃ for 4.5h. After rinsing with deionized water multiple times and drying in a dryer, hydrophobic cotton fibers are obtained.

[0104] S2, Durability Treatment

[0105] 5.0 kg of hydrophobic cotton fiber obtained in step S12 and 1.2 kg of coating particles prepared in Preparation Example 6 were uniformly dispersed in anhydrous ethanol, and then reacted at 65°C for 5 h. After rinsing and drying, durable hydrophobic cotton fiber was obtained.

[0106] S3, Fiber weaving

[0107] The durable hydrophobic cellulose fiber obtained in step S22 is opened in a cotton opener, carded in a carding machine, and then drawn in a drawing frame to obtain a sliver. The sliver is then wound through roving and spinning to obtain a durable hydrophobic cellulose fiber package yarn with a fineness of 1.53D.

[0108] Example 1.2

[0109] A method for preparing a durable hydrophobic cellulose fiber package yarn includes the following steps:

[0110] S1, hydrophobic treatment

[0111] S11. The natural cotton fiber was completely immersed in the hydrophobic treatment solution prepared in Preparation Example 2, reacted for 23 hours, rinsed repeatedly with deionized water, and dried in a dryer to obtain coarsely treated cotton fiber.

[0112] S12. All the coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 25wt%, and then reacted at 48°C for 5 hours. After rinsing with deionized water multiple times and drying in a dryer, hydrophobic cotton fibers are obtained.

[0113] S2, Durability Treatment

[0114] 5.5 kg of hydrophobic cotton fiber obtained in step S12 and 1.15 kg of coating particles prepared in Preparation Example 7 were uniformly dispersed in anhydrous ethanol, and then reacted at 60°C for 6 h. After rinsing and drying, durable hydrophobic cotton fiber was obtained.

[0115] S3, Fiber weaving

[0116] The durable hydrophobic cellulose fiber obtained in step S22 is opened in a cotton opener, carded in a carding machine, and then drawn in a drawing frame to obtain a sliver. The sliver is then wound through roving and spinning to obtain a durable hydrophobic cellulose fiber package yarn with a fineness of 1.51D.

[0117] Example 2

[0118] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 1.1 in that: in step S11, the hydrophobic treatment solution obtained in Preparation Example 1 is replaced with the hydrophobic treatment solution obtained in Preparation Example 3, while the rest is the same as in Example 1.1.

[0119] Example 3

[0120] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 1.1 in that: in step S2, the coating particles obtained in Preparation Example 6 are replaced with the coating particles obtained in Preparation Example 8, and the rest are the same as in Example 1.1.

[0121] Example 4.1

[0122] A method for preparing a durable hydrophobic cellulose fiber package yarn includes the following steps:

[0123] S1, hydrophobic treatment

[0124] S11. The natural cotton fiber was completely immersed in the hydrophobic treatment solution prepared in Preparation Example 1, reacted for 24 hours, rinsed repeatedly with deionized water, and dried in a dryer to obtain coarsely treated cotton fiber.

[0125] S12. All the coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 24wt%, and then reacted at 52℃ for 4.5h. After rinsing with deionized water multiple times and drying in a dryer, hydrophobic cotton fibers are obtained.

[0126] S2, Durability Treatment

[0127] 5.0 kg of hydrophobic cotton fiber obtained in step S12, 1.2 kg of coating particles prepared in Preparation Example 5, and 0.576 kg of heptadecafluorodecyltriethoxysilane were uniformly dispersed in anhydrous ethanol, and then reacted at 65°C for 5 h. After rinsing and drying, durable hydrophobic cotton fiber was obtained.

[0128] S3, Fiber weaving

[0129] The durable hydrophobic cellulose fiber obtained in step S22 is opened in a cotton opener, carded in a carding machine, and then drawn in a drawing frame to obtain a sliver. The sliver is then wound through roving and spinning to obtain a durable hydrophobic cellulose fiber package yarn with a fineness of 1.53D.

[0130] Example 4.2

[0131] A method for preparing a durable hydrophobic cellulose fiber package yarn includes the following steps:

[0132] S1, hydrophobic treatment

[0133] S11. The natural cotton fiber was completely immersed in the hydrophobic treatment solution prepared in Preparation Example 1, reacted for 24 hours, rinsed repeatedly with deionized water, and dried in a dryer to obtain coarsely treated cotton fiber.

[0134] S12. All the coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 24wt%, and then reacted at 52℃ for 4.5h. After rinsing with deionized water multiple times and drying in a dryer, hydrophobic cotton fibers are obtained.

[0135] S2, Durability Treatment

[0136] 5.0 kg of hydrophobic cotton fiber obtained in step S12, 1.2 kg of coating particles prepared in Preparation Example 5, and 0.624 kg of heptadecafluorodecyltriethoxysilane were uniformly dispersed in anhydrous ethanol, and then reacted at 65°C for 5 h. After rinsing and drying, durable hydrophobic cotton fiber was obtained.

[0137] S3, Fiber weaving

[0138] The durable hydrophobic cellulose fiber obtained in step S22 is opened in a cotton opener, carded in a carding machine, and then drawn in a drawing frame to obtain a sliver. The sliver is then wound through roving and spinning to obtain a durable hydrophobic cellulose fiber package yarn with a fineness of 1.53D.

[0139] Example 4.3

[0140] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 4.1 in that: the amount of heptadecafluorodecyltriethoxysilane in step S2 is 0.5916 kg, while the rest is the same as in Example 4.1.

[0141] Example 5.1

[0142] A method for preparing a durable hydrophobic cellulose fiber package yarn includes the following steps:

[0143] S1, hydrophobic treatment

[0144] S11. The natural cotton fiber was completely immersed in the hydrophobic treatment solution prepared in Preparation Example 1, reacted for 24 hours, rinsed repeatedly with deionized water, and dried in a dryer to obtain coarsely treated cotton fiber.

[0145] S12. All the coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 24wt%, and then reacted at 52℃ for 4.5h. After rinsing with deionized water multiple times and drying in a dryer, hydrophobic cotton fibers are obtained.

[0146] S2, Durability Treatment

[0147] 5.0 kg of hydrophobic cotton fiber obtained in step S12 and 1.2 kg of coating particles prepared in Preparation Example 5 were uniformly dispersed in anhydrous ethanol, and then reacted at 65°C for 5 h. After rinsing and drying, durable hydrophobic cotton fiber was obtained.

[0148] S3, Fiber weaving

[0149] S31. The durable hydrophobic cellulose fiber obtained in step S22 is opened in a cotton opener, carded in a cotton carding machine, and then drawn in a drawing frame to obtain a sliver. The sliver is then passed through roving and spinning to obtain the durable hydrophobic cellulose fiber yarn to be treated.

[0150] S32. The durable hydrophobic cellulose fiber yarn to be treated is completely immersed in the strengthening treatment solution prepared in Preparation Example 11, and then padded at 90°C for 0.15 h, dried in a dryer, finished, and wound to obtain a durable hydrophobic cellulose fiber package yarn with a fineness of 1.53D.

[0151] Example 5.2

[0152] A method for preparing a durable hydrophobic cellulose fiber package yarn includes the following steps:

[0153] S1, hydrophobic treatment

[0154] S11. The natural cotton fiber was completely immersed in the hydrophobic treatment solution prepared in Preparation Example 1, reacted for 24 hours, rinsed repeatedly with deionized water, and dried in a dryer to obtain coarsely treated cotton fiber.

[0155] S12. All the coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 24wt%, and then reacted at 52℃ for 4.5h. After rinsing with deionized water multiple times and drying in a dryer, hydrophobic cotton fibers are obtained.

[0156] S2, Durability Treatment

[0157] 5.0 kg of hydrophobic cotton fiber obtained in step S12 and 1.2 kg of coating particles prepared in Preparation Example 5 were uniformly dispersed in anhydrous ethanol, and then reacted at 65°C for 5 h. After rinsing and drying, durable hydrophobic cotton fiber was obtained.

[0158] S3, Fiber weaving

[0159] S31. The durable hydrophobic cellulose fiber obtained in step S22 is opened in a cotton opener, carded in a cotton carding machine, and then drawn in a drawing frame to obtain a sliver. The sliver is then passed through roving and spinning to obtain the durable hydrophobic cellulose fiber yarn to be treated.

[0160] S32. The durable hydrophobic cellulose fiber yarn to be treated is completely immersed in the strengthening treatment solution prepared in Preparation Example 12, and then padded at 85°C for 0.2 h, dried in a dryer, finished, and wound to obtain a durable hydrophobic cellulose fiber package yarn with a fineness of 1.53D.

[0161] Example 5.3

[0162] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 5.1 in that: in step S32, the reinforcing treatment liquid obtained in Preparation Example 11 is replaced with the reinforcing treatment liquid obtained in Preparation Example 13, and the rest is the same as in Example 5.1.

[0163] Examples 5.4-5.5

[0164] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 5.1 in that: in step S32, the reinforcing solution obtained in Preparation Example 11 is replaced with the reinforcing solution obtained in Preparation Examples 14-15, and the rest is the same as in Example 5.1.

[0165] Examples 5.6-5.7

[0166] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 5.1 in that: in step S32, the reinforcing solution obtained in Preparation Example 14 is replaced with the reinforcing solution obtained in Preparation Examples 16-17, and the rest is the same as in Example 5.1.

[0167] Example 6.1

[0168] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 5.1 in that: in step S32, the padding temperature is 88°C and the time is 0.19h, while the rest are the same as in Example 5.1.

[0169] Example 6.2

[0170] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 5.1 in that: in step S32, the impregnation temperature is 100°C and the time is 0.25h, while the rest are the same as in Example 5.1.

[0171] Example 6.3

[0172] A method for preparing a durable hydrophobic cellulose fiber package yarn differs from Example 5.1 in that: in step S32, the padding temperature is 60°C and the time is 0.10h, while the rest are the same as in Example 5.1.

[0173] Comparative Example 1.1

[0174] The difference from Example 1.1 is that in step S1, all the coarsely treated cotton fibers are completely immersed in a 3.5 wt% silicone zirconium stearic acid waterproofing agent, and then stirred continuously at room temperature for 3.5 h, followed by rinsing and drying. The rest is the same as in Example 1.1.

[0175] Comparative Example 1.2

[0176] The difference from Example 1.1 is that step S2 is removed, while the rest is the same as in Example 1.1.

[0177] Comparative Examples 2.1-2.2

[0178] The difference from Example 1.1 is that in step S11, the hydrophobic treatment solution obtained in Preparation Example 1 is replaced with the hydrophobic treatment solution obtained in Preparation Examples 4-5, and the rest is the same as in Example 1.1.

[0179] Comparative Examples 3.1-3.2

[0180] The difference from Example 1.1 is that in step S2, the coated particles obtained in Preparation Example 6 are replaced with the coated particles obtained in Preparation Examples 9-10, and the rest are the same as in Example 1.1.

[0181] Performance testing

[0182] 1. Hydrophobicity test: The contact angles of the durable hydrophobic cellulose fiber package yarns obtained in Examples 1.1-6.3 and Comparative Examples 1-3.2 were determined according to DB44 / T1872-2016 "Determination of surface wettability of textiles - Contact angle method", and the results are recorded in Table 1;

[0183] 2. Durability test: In accordance with GB / T3923.1-2013 "Textiles - Tensile Properties of Fabrics", the tensile breaking strength and elongation at break of the durable hydrophobic cellulose fiber package yarns obtained in Examples 1.1-6.3 and Comparative Examples 1-3.2 were tested, and the results are recorded in Table 1.

[0184] Table 1

[0185]

[0186]

[0187] Analyze the data in Table 1:

[0188] Examples 1.1-1.2 show a contact angle of 146.3-146.4°, a tensile breaking strength of 351-353N, and an elongation at break of 27.98-28.56%, demonstrating that this application effectively improves the durability and hydrophobicity of cellulose fiber package yarn by using hydrophobic treatment agents and coating particles to perform hydrophobic and durable treatment on natural cotton fibers.

[0189] The contact angle of Example 2 is higher than that of Example 1.1, which proves that this application effectively improves the hydrophobicity of cellulose fiber package yarn by further controlling the weight ratio of tromethamine and dopamine hydrochloride.

[0190] The tensile breaking strength and elongation at break of Example 3 are higher than those of Example 1.1, proving that this application effectively improves the durability of cellulose fiber package yarn by controlling the weight ratio of silica particles and polydopamine.

[0191] The contact angles of Examples 4.1-4.3 are all higher than those of Example 1.1, and the tensile strength and elongation at break are not significantly different from those of Example 1.1. This proves that by adding a certain amount of heptadecafluorodecyltriethoxysilane, this application can compensate for the decrease in hydrophobicity caused by the loss of hydrophobic groups due to heat. Among them, the contact angle of Example 4.3 is higher than that of Examples 4.1-4.2, which proves that by further controlling the amount of heptadecafluorodecyltriethoxysilane added, this application can maximize the compensation for the loss of hydrophobic groups without incurring additional raw material costs.

[0192] The contact angle, tensile breaking strength, and elongation at break of Examples 5.1-5.7 are all higher than those of Example 1.1, proving that the present application can further improve the durability and hydrophobicity of durable hydrophobic cellulose fiber yarns by using a reinforcing treatment solution for padding treatment.

[0193] The tensile breaking strength and elongation at break of Example 5.3 were not significantly different from those of Example 5.1, while the contact angle was higher than that of Example 5.1. The contact angle of Example 5.3 was not significantly different from that of Example 5.2, while the tensile breaking strength and elongation at break were higher than those of Example 5.2. This demonstrates that by further controlling the weight ratio of hexadecyltrimethoxysilane, sodium phosphite, and water, this application can maximize the durability and hydrophobicity of cellulose fiber package yarns without incurring additional raw material costs. The tensile breaking strength and elongation at break of Examples 5.4-5.7 were all higher than those of Example 5.1, and the contact angle was not significantly different from that of Example 5.1. This demonstrates that by adding a crosslinking agent to the strengthening treatment solution, this application effectively improved the durability of cellulose fiber package yarns. The tensile breaking strength and elongation at break of Example 5.7 were higher than those of Examples 5.4 and 5.6, demonstrating that the use of butanetetraacetic acid as the crosslinking agent in this application further improved the durability of cellulose fiber package yarns.

[0194] The contact angle, tensile breaking strength, and elongation at break of Example 6.1 are all higher than those of Example 5.1, while the contact angle, tensile breaking strength, and elongation at break of Examples 6.2-6.3 are all lower than those of Example 5.1. This proves that by controlling the temperature and time of the padding process, this application achieves optimal durability and hydrophobicity of the cellulose fiber package yarn.

[0195] The hydrophobic angles of Comparative Examples 1.1-1.2 were not significantly different from those of Example 1.1, while their tensile breaking strength and elongation at break were lower than those of Example 1.1. The difference in tensile breaking strength between Comparative Example 1.1 and Example 1.1 was 45 N, while the difference in tensile breaking strength between Comparative Example 1.2 and Example 1.1 was 79 N. This proves that the durability of cellulose fiber yarn can be effectively improved by performing the durability treatment in step S2. At the same time, the hydrophobic treatment used in this application can achieve better optimization results in subsequent durability treatment.

[0196] The contact angles of Comparative Examples 2.1-2.2 were lower than those of Example 1.1, demonstrating that this application effectively improved the hydrophobicity of cellulose fiber package yarns by further controlling the weight ratio of tromethamine and dopamine hydrochloride.

[0197] The tensile breaking strength and elongation at break of Comparative Examples 3.1-3.2 were both lower than those of Example 1.1, demonstrating that this application effectively improves the durability of cellulose fiber package yarn by controlling the weight ratio of silica particles and polydopamine.

[0198] The embodiments described in this specific implementation are preferred embodiments of this application and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A method for preparing a durable hydrophobic cellulose fiber packaged yarn, characterized in that: Includes the following steps: S1, hydrophobic treatment S11. A treatment agent is obtained by mixing tromethamine and dopamine hydrochloride in a weight ratio of (14.2-15.6):(23.0-24.5) and dispersing the treatment agent in water to obtain a treatment solution with a concentration of 36.2-37.0 wt%. Natural cotton fibers are completely immersed in the treatment solution and reacted for 23-24 hours. After rinsing and drying, coarsely treated cotton fibers are obtained. S12. The coarsely treated cotton fibers are completely immersed in an anhydrous ethanol solution of heptadecafluorodecyltriethoxysilane with a concentration of 24-25wt%, and then reacted at a temperature of 48-52℃ for 4.5-5h. After rinsing and drying, hydrophobic cotton fibers are obtained. S2, Durability Treatment S21. While stirring, disperse silica particles and polydopamine in anhydrous ethanol. The weight ratio of silica particles to polydopamine is (7.6-8.4):(16.0-16.2). Then, react under inert gas protection and at a reaction temperature of 48-50℃ for 25-26 hours. After centrifugation and drying, the coated particles are obtained. S22. The hydrophobic cotton fiber obtained in step S12 and the coated particles obtained in step S21 are uniformly dispersed in anhydrous ethanol. The weight ratio of the hydrophobic cotton fiber to the coated particles is (50-55):(11.5-12.0). Then, the mixture is reacted at 60-65℃ for 5-6 hours. After rinsing and drying, durable hydrophobic cotton fiber is obtained. S3, Fiber weaving The durable hydrophobic cellulose fiber obtained in step S22 is processed through opening, carding, drawing, roving, spinning, and winding to obtain durable hydrophobic cellulose fiber package yarn.

2. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 1, characterized in that: In step S11, the weight ratio of tromethamine to dopamine hydrochloride is 14.8:24.

2.

3. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 1, characterized in that: In step S21, the weight ratio of silica particles to polydopamine is 8:16.

16.

4. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 1, characterized in that: In step S22, after the hydrophobic cotton fibers and coating particles are uniformly dispersed in anhydrous ethanol, heptadecafluorodecyltriethoxysilane is added to the system at an amount of 48-52 wt% of the amount of coating particles. After mixing evenly, the subsequent reaction is carried out.

5. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 4, characterized in that: In step S22, the amount of heptadecafluorodecyltriethoxysilane used is 49.3 wt% of the amount of coating particles.

6. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 1, characterized in that: Step S3 further includes a padding process, specifically: The yarn to be treated, obtained after fine spinning, is completely immersed in the strengthening treatment solution, and then subjected to padding treatment at a temperature of 85-90℃ for 0.15-0.2h. After drying and finishing, it is then wound. The strengthening treatment solution includes hexadecyltrimethoxysilane, sodium phosphite and water in a weight ratio of (12-18):(7-9):(60-85).

7. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 6, characterized in that: The weight ratio of hexadecyltrimethoxysilane, sodium phosphite, and water is 15:8.5:

76.

8. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 6, characterized in that: The enhanced treatment solution also includes a crosslinking agent added at a concentration of 63.7-86.2 g / L.

9. The method for preparing a durable hydrophobic cellulose fiber package yarn according to claim 8, characterized in that: The crosslinking agent is butanetetraacetic acid.

10. A durable hydrophobic cellulose fiber packaged yarn prepared by the method of any one of claims 1-9, characterized in that: The contact angle reaches 146.3-146.4°, the tensile breaking strength reaches 351-353N, and the elongation at break reaches 27.98-28.56%.

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