Preparation method of high-shrinkage polyethylene furandicarboxylate fiber

Through the drying treatment and melt spinning process optimization of polyethylene furandiformate slices, the problem of insufficient performance of high shrinkage fibers in PEF spinning is solved, and high shrinkage polyfurandiformic acid with high break strength and elongation of break is achieved The preparation of ethylene glycol ester fiber is suitable for the replacement of PET.

CN119162684AActive Publication Date: 2024-12-20SHANGHAI DEFULUN CHEM FIBER

Patent Information

Application Number
CN202411414849.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-10
Publication Date
2024-12-20
Estimated Expiration
2044-10-10

AI Technical Summary

Technical Problem

It is difficult for the prior art to achieve high-condensation polyethylene furandiformate fibers with high break strength, elongation of break and boiling water shrinkage at the same time during the PEF spinning process, and bio-based high-condensation fiber products have not yet appeared.

Method used

By drying the polyethylene furandiformate slices, the moisture content is reduced, and the screw speed and ring blowing pressure are increased during the melt spinning process, combined with the program heating and vacuuming, the problem of excessive melt viscosity is overcome. Prepare highly condensation polyethylene furandicarboxylate fibers.

Benefits of technology

It achieves high break strength and elongation of break of fibers, and has low production equipment requirements and high efficiency, which is convenient for large-scale production. The fiber performance exceeds PET high shrinkage fibers and is suitable as a replacement product for PET.

✦ Generated by Eureka AI based on patent content.
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Abstract

The invention belongs to the technical field of preparation of bio-based functional fibers, and relates to a preparation method of high-shrinkage polyethylene furandicarboxylate fibers. The preparation method comprises the following steps: drying the polyethylene furandicarboxylate slices, and carrying out melt blending spinning to obtain the high-shrinkage polyethylene furandicarboxylate fiber. The linear density of the fiber is 2.22-4.44 dtex, and the linear density deviation ratio is-5%-5%. The breaking strength of the fiber is 3.5-4.5 cN / dtex, the elongation at break is 53.5-68.5%, the content of super-long fibers is 0-3 mg / 100 g, the defect content is 3-20 mg / 100 g, the crimp number is 12-15 / 25 mm, the crimp rate is 14-18%, and the boiling water shrinkage rate is 60-80%. The prepared high-shrinkage polyethylene furandicarboxylate fiber is a 100% high-shrinkage polyester fiber, the performance of the fiber is far superior to that of a conventional high-shrinkage fiber, and the high-shrinkage polyethylene furandicarboxylate fiber can become a substitute product of PET.
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Description

Technical Field

[0001] The invention belongs to the technical field of bio-based functional fiber preparation, and relates to a method for preparing high-shrinkage polyethylene furandicarboxylate fiber. Background Art

[0002] Governments and international organizations have introduced relevant policies to promote green and low-carbon development to meet the challenges of global environmental issues. The "Implementation Plan for the Innovation and Development of the Fine Chemical Industry (2024-2027)" issued by the Ministry of Industry and Information Technology and other nine departments requires that a bio-based material system based on the utilization of non-food biomass resources such as bulk crop straw and residues will be focused on, and bio-based chemicals such as furan and bio-based polymers such as polyethylene furandicarboxylate (PEF) will be developed to effectively supplement existing fossil-based materials. PEF is a 100% bio-based material synthesized by direct esterification or transesterification by adding FDCA as a monomer to diols. It has a very high similarity to PET structure and similar properties. It is the material most likely to achieve similar or better performance than PET polyester. In the industry, PEF is also called the next generation of polyester, and has huge potential.

[0003] However, in the spinning process of PEF, since FDCA replaces the benzene ring structure in PET, the asymmetry and permanent dipole moment of the furan ring lead to limited molecular chain movement and increased intermolecular steric hindrance, which makes the orientation and crystallization performance of the molecular chain of PEF deteriorate during the spinning process, thereby causing the reduction of fiber breaking strength and breaking elongation. CN117209735 discloses a method for preparing a cationic dyeable high shrinkage furan dicarboxylic acid polyester and a fiber. The patent prepares the cationic dyeable high shrinkage furan dicarboxylic acid polyester slice by drying, screw extrusion, metering, cooling, bundling, hot drawing and winding. The fiber breaking strength reaches up to 3.4 cN / dtex, but its breaking elongation is only 17%. CN 117286598 discloses a low heat shrinkage bio-based furan copolyester fiber and a preparation method thereof. The invention is designed by formulating FDCA and mixed diols. A low shrinkage bio-based furan copolyester fiber is prepared by a polymerization process in combination with a heat setting and stretching process. The breaking strength of PEF fiber is up to 3.8cN / dtex, and the breaking elongation is 33.2%. Based on the environmental protection and good mechanical properties of PEF fiber, it can be blended with wool, rabbit hair, etc. to make cashmere, imitation wool and other products. However, animal hair usually has the characteristics of high shrinkage, so high-shrinkage PEF products can be designed to make them easy to curl into loops, fluffy and round like wool yarn. The yarn blended with wool, rabbit hair, etc. is light and fluffy, soft and warm. In addition, due to the increase of oxygen-containing functional groups in the PEF molecular chain, its hydrophilicity is enhanced, and the blended yarn also has moisture absorption and perspiration properties.

[0004] Commercially available high-shrinkage polyester products are mainly produced through chemical-physical methods, that is, high-shrinkage polyester chips are dried, melt-spun, wound, and barreled to produce raw yarn; a certain amount of raw yarn is then spun through primary oil bath drawing, secondary cold drawing, folding, curling, oiling, oven low-temperature drying, cutting, and packaging. However, high-shrinkage bio-based products have not yet appeared, so blending bio-based high-shrinkage fibers with natural animal hair (wool, rabbit hair, etc.) to prepare yarns not only conforms to the concept of green development and environmental protection, but is also of great significance to the high-value application of bio-based fibers. Summary of the invention

[0005] The purpose of the present invention is to solve the problems existing in the prior art and provide a method for preparing high-shrinkage polyethylene furandicarboxylate fiber.

[0006] To achieve the above object, the technical solution adopted by the present invention is as follows:

[0007] The invention discloses a method for preparing high-shrinkage polyethylene furandicarboxylate fiber. Polyethylene furandicarboxylate slices are dried and melt-blended and spun to prepare the high-shrinkage polyethylene furandicarboxylate fiber.

[0008] As the preferred technical solution:

[0009] According to the method for preparing high shrinkage polyethylene furandicarboxylate fiber, the intrinsic viscosity of PEF is 0.60-0.80 dL / g and the melting point is 210-230°C.

[0010] In the method for preparing the high shrinkage polyethylene furandicarboxylate fiber as described above, the high shrinkage polyethylene furandicarboxylate is first dried to a water content of less than 200 ppm before melt blending and spinning.

[0011] The preparation method of the high shrinkage polyethylene furandicarboxylate fiber as described above comprises the following steps of drying: first drying at 80-100° C. for 2-3 hours, and then vacuum drying at 90-110° C. for 6-10 hours.

[0012] The method for preparing the high shrinkage polyethylene furandicarboxylate fiber as described above comprises the following steps: melt-blending and spinning the high shrinkage polyethylene furandicarboxylate to obtain the high shrinkage polyethylene furandicarboxylate fiber: melt-extruding the high shrinkage polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the high shrinkage polyethylene furandicarboxylate to obtain the primary yarn;

[0013] The preparation method of high shrinkage polyethylene furandicarboxylate fiber as described above, the process parameters of melt blending spinning include: screw speed 28-35r / min; screw temperature 250-280°C, spinning box temperature 265-280°C, pump supply 500-900g / min, pressure difference between annular air inlet and return air 600-800Pa, winding speed 1000-1150m / min.

[0014] According to the method for preparing high shrinkage polyethylene furandicarboxylate fiber, the raw silk is subjected to sequential bundling, drawing, tension heat setting, curling, oiling and relaxation heat setting to obtain high shrinkage polyethylene furandicarboxylate fiber.

[0015] In the preparation method of the high shrinkage polyethylene furandicarboxylate fiber as described above, the oil bath temperature in the first oil bath drawing is 70-80°C, the second oil bath drawing temperature is 80-100°C, the drawing multiple is 3.1-4.1 times, and the temperature of the tense heat setting is 80-100°C.

[0016] The present invention also provides high shrinkage polyethylene furandicarboxylate fiber prepared by the preparation method of high shrinkage polyethylene furandicarboxylate fiber as described in any one of the above items, wherein the linear density of the fiber is 2.22-4.44 dtex and the linear density deviation rate is -5%-5%.

[0017] As the preferred technical solution:

[0018] The high shrinkage polyethylene furandicarboxylate fiber has a fiber breaking strength of 3.5-4.5 cN / dtex, a breaking elongation of 53.5-68.5%, a boiling water shrinkage of 60%-80%, an ultra-long fiber content of 0-3 mg / 100g, a defect content of 3-20 mg / 100g, a crimp number of 12-15 / 25mm, and a crimp rate of 14%-18%.

[0019] As the preferred technical solution:

[0020] The polyethylene furandicarboxylate slices are dried, treated with a stabilizer, and then melt-blended and spun to obtain high-shrinkage polyethylene furandicarboxylate fibers. The weight ratio of the polyethylene furandicarboxylate slices to the stabilizer is 10:1.

[0021] The stabilizer comprises poly(boron diphenylsiloxane), dipentaerythritol hexaacrylate and nano-silica modified silk fibroin, and the weight ratio of the poly(boron diphenylsiloxane), dipentaerythritol hexaacrylate and nano-silica modified silk fibroin is 1:2:2.

[0022] The step of treating the polyethylene furandicarboxylate slices with a stabilizer after drying is as follows: mixing the dried polyethylene furandicarboxylate slices with the stabilizer, stirring at 80° C. for 10 minutes, and then vacuum drying at 100° C. for 10 hours before use.

[0023] Based on the above technical solution, poly(boron diphenylsiloxane) and dipentaerythritol hexaacrylate are used for lubrication and plasticization, so that the bonding strength between nano-silica modified silk protein and polyethylene furandicarboxylate is increased, thereby enhancing the fiber strength. At the same time, the excellent reactivity of dipentaerythritol hexaacrylate makes poly(boron diphenylsiloxane) bind more tightly to polyethylene furandicarboxylate, thereby further improving its plasticity.

[0024] Principle of the invention:

[0025] The synthesis of PEF is similar to that of PET, and is mainly achieved through the melt polycondensation method, where FDCA and diols are directly reacted to form an ester, and then PEF is synthesized through polycondensation. This method has the advantages of low raw material consumption, short reaction time, slow reaction rate, high relative molecular mass of the product, and no harmful side reaction products. Therefore, it has become the most effective method for the industrial production of PEF. In addition, compared with the synthesis reaction of PET, the reaction conditions of PEF are milder. In the ester exchange stage, the esterification temperature is 190-210℃, which is 30℃ lower than the esterification temperature of PET; and in the polycondensation stage, the temperature is 240-245℃, which is 40℃ lower than the esterification temperature of PET; it not only increases the safety and controllability of the reaction, reduces the probability of safety accidents such as fire and explosion, but also reduces energy consumption, thereby indirectly reducing greenhouse gas emissions. The spinning process of PEF is similar to the melt spinning process of PET, but the PEF obtained under this condition has the characteristics of high viscosity and low melting point. Therefore, during the spinning process, the screw speed, screw temperature, box temperature, ring blowing air pressure, post-spinning drafting temperature, and drafting rate will be affected to varying degrees. It is not difficult to obtain PEF fiber by melt spinning, but it is not easy to prepare high shrinkage PEF fiber while controlling the fiber linear density, linear density deviation rate, and defect content within a certain range; in addition, according to literature and patent research, there is currently no high shrinkage PEF fiber on the market that can simultaneously have high breaking strength, breaking elongation, and boiling water shrinkage.

[0026] The present invention starts with the drying process of high-shrinkage polyethylene furandicarboxylate chips, and adopts a combination of programmed temperature increase and programmed vacuuming to reduce the moisture content of the chips to below 200 ppm, while achieving the purpose of increasing the crystallinity and softening temperature of the chips. In the melt-spinning stage, the shear thinning effect of the PEF melt is enhanced by increasing the screw speed to overcome the problem of poor fluidity caused by excessive melt viscosity, while the screw temperature is set to not guarantee its fluidity and extrusion volume; in the fiber spinning stage, the annular blowing pressure is increased to promote rapid crystallization, and solidification molding is performed to obtain primary silk. In the post-spinning stage, the uniformity of the drawing is ensured by increasing the drawing temperature, while the shaping temperature is reduced to ensure the stability of the fiber molding.

[0027] Beneficial effects:

[0028] (1) The preparation method used in the present invention has low requirements on production equipment, high efficiency, and is convenient for large-scale production.

[0029] (2) The high shrinkage polyethylene furandicarboxylate fiber prepared by the present invention is a bio-based high shrinkage fiber, and its fiber performance far exceeds that of PET high shrinkage fiber and can become a substitute product for PET. DETAILED DESCRIPTION

[0030] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0031] The following are the test methods for the relevant performance indicators in each embodiment and comparative example:

[0032] Crystallinity: Tested in accordance with GB / T 19466.3-2004 standard.

[0033] Softening temperature: Tested in accordance with GB / T 1633-2000 standard.

[0034] Intrinsic viscosity: Tested in accordance with GB / T 14190-2017 standard.

[0035] Melting point: Tested in accordance with GB / T 14190-2017 standard.

[0036] Linear density and extra-long fiber content: measured in accordance with GB / T 14335-2008.

[0037] Breaking strength and breaking elongation: measured in accordance with GB / T 14337-2022, where the tensile speed is 30 mm / min.

[0038] Defect content: Determined in accordance with GB / T 14339-2008 standard.

[0039] Curl number and curl rate: measured in accordance with GB / T 14338-2022 standard.

[0040] Boiling water shrinkage: Prepare the fiber sample in the manner specified by the standard, usually by fixing both ends of the fiber to keep it in a straight line. Use precise measuring tools (such as vernier calipers, electronic rulers, etc.) to measure and record the initial length of the fiber sample; immerse the fiber sample completely in boiling water for 30 minutes; take out the immersed fiber sample, quickly cool it to room temperature, and then measure its length again; calculate the boiling water shrinkage of the fiber according to the shrinkage calculation formula (length before shrinkage - length after shrinkage) / length before shrinkage × 100%.

[0041] Example 1

[0042] A method for preparing high shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0043] (1) Preparation of raw materials;

[0044] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0045] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0046] Among them, the process parameters of melt blending spinning are: screw speed 31r / min, screw zone 1 temperature 250℃, zone 2 temperature 255℃, zone 3 temperature 260℃, zone 4 temperature 265℃, zone 5 temperature 260℃, zone 6 temperature 255℃, spinning box temperature 265℃, pump supply 890g / min, pressure difference between inlet and return air of annular blowing 720Pa, winding speed 1050m / min;

[0047] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0048] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 80°C;

[0049] The linear density of polyethylene furandicarboxylate fiber is 3.33dtex, the linear density deviation rate is 0.1%, the fiber breaking strength is 4.5cN / dtex, the breaking elongation is 58.9%, the ultra-long fiber content is 0.5mg / 100g, the defect content is 3mg / 100g, the number of crimps is 14.5 / 25mm, the crimp rate is 16.4%, and the boiling water shrinkage is 80%.

[0050] Comparative Example 1

[0051] Patent application CN117286598, a method for preparing a high shrinkage furan copolyester fiber with low thermal shrinkage, the only difference is: 2,5-furandicarboxylic acid and mixed diols are copolymerized to obtain high shrinkage furan copolyester chips; the high shrinkage furan copolyester chips are spun to obtain low thermal shrinkage high shrinkage furan copolyester fibers; the high shrinkage furan copolyester fibers finally obtained have an intrinsic viscosity of 0.75 dL / g, a melting point of 242°C, a breaking strength of 3.8 cN / dtex, and an elongation at break of 33.2%.

[0052] Compared with the embodiment, the characteristic viscosity and melting point of the high shrinkage furan copolyester chips in the comparative example are significantly higher, especially the melting point, which is closer to the melting point of PET. Therefore, the breaking strength can be achieved under conventional processing technology. By purchasing high viscosity (0.752dL / g) chips and spinning them under the process conditions of Example 1, it is found that the breaking strength can reach 4.8cN / dtex and the elongation at break is 46.5%, which is significantly higher than the data in the comparative example.

[0053] Comparative Example 2

[0054] Patent application CN112760740, the preparation method and application of high shrinkage 2,5-furandicarboxylic acid copolyester fiber, the only difference is: the 2,5-furandicarboxylic acid copolyester fiber is mainly prepared by polymerizing 2,5-furandicarboxylic acid, terephthalic acid, ethylene glycol and C12-C20 diol ether composition to form 2,5-furandicarboxylic acid copolyester, and then melt spinning and heat drawing treatment. The high shrinkage 2,5-furandicarboxylic acid copolyester fiber finally prepared has a breaking strength of 4.1 cN / dtex and a breaking elongation of 45%.

[0055] This comparative example introduces terephthalic acid and furandicarboxylic acid into the molecular chain for copolymerization. Compared with PEF, the molecular chain of high-shrinkage 2,5-furandicarboxylic acid-based copolyester fiber is more regular, so the obtained breaking strength and elongation are similar to those of PET. Terephthalic acid is a petroleum cracking product and a non-renewable resource. The comparative fiber is not 100% high-shrinkage material, and there is still a safety hazard of microplastics in subsequent degradation.

[0056] Example 2

[0057] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0058] (1) Preparation of raw materials;

[0059] Poly(ethylene furandicarboxylate): The manufacturer is Hefei Lifu Biotechnology Co., Ltd., and the brand name is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217°C.

[0060] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0061] Among them, the process parameters of melt blending spinning are: screw speed 31r / min, screw zone 1 temperature 250℃, zone 2 temperature 255℃, zone 3 temperature 260℃, zone 4 temperature 265℃, zone 5 temperature 260℃, zone 6 temperature 255℃, spinning box temperature 265℃, pump supply 890g / min, pressure difference between inlet and return air of annular blowing 720Pa, winding speed 1050m / min;

[0062] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0063] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.35 times, and the temperature of tense heat setting is 90°C;

[0064] The linear density of polyethylene furandicarboxylate fiber is 3.21dtex, the linear density deviation rate is -0.5%, the fiber breaking strength is 4.3cN / dtex, the breaking elongation is 58.2%, the ultra-long fiber content is 0.7mg / 100g, the defect content is 3.2mg / 100g, the number of crimps is 14.3 / 25mm, the crimp rate is 15.7%, and the boiling water shrinkage is 75%.

[0065] Example 3

[0066] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0067] (1) Preparation of raw materials;

[0068] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0069] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0070] Among them, the process parameters of melt blending spinning are: screw speed 31r / min, screw zone 1 temperature 250℃, zone 2 temperature 255℃, zone 3 temperature 260℃, zone 4 temperature 265℃, zone 5 temperature 260℃, zone 6 temperature 255℃, spinning box temperature 265℃, pump supply 890g / min, pressure difference between annular blowing inlet and return air 720Pa, winding speed 1100m / min;

[0071] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0072] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 95°C;

[0073] The linear density of polyethylene furandicarboxylate fiber is 3.26 dtex, the linear density deviation rate is 0.3%, the fiber breaking strength is 4.3 cN / dtex, the breaking elongation is 58.3%, the ultra-long fiber content is 1.0 mg / 100 g, the defect content is 3.0 mg / 100 g, the number of crimps is 13.9 / 25 mm, the crimp rate is 14.5%, and the boiling water shrinkage is 70%.

[0074] Example 4

[0075] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0076] (1) Preparation of raw materials;

[0077] Poly(ethylene furandicarboxylate): The manufacturer is Hefei Lifu Biotechnology Co., Ltd., and the brand name is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217°C.

[0078] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0079] Among them, the process parameters of melt blending spinning are: screw speed 31r / min, screw zone 1 temperature 250℃, zone 2 temperature 255℃, zone 3 temperature 260℃, zone 4 temperature 265℃, zone 5 temperature 260℃, zone 6 temperature 255℃, spinning box temperature 265℃, pump supply 890g / min, pressure difference between inlet and return air of annular blowing 740Pa, winding speed 1050m / min;

[0080] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0081] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.35 times, and the temperature of tense heat setting is 100°C;

[0082] The linear density of polyethylene furandicarboxylate fiber is 3.41 dtex, the linear density deviation rate is 1%, the fiber breaking strength is 4.1 cN / dtex, the breaking elongation is 52.4%, the ultra-long fiber content is 0 mg / 100g, the defect content is 3.5 mg / 100g, the number of crimps is 12.7 / 25mm, the crimp rate is 14.3%, and the boiling water shrinkage is 60%.

[0083] Example 5

[0084] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0085] (1) Preparation of raw materials;

[0086] Poly(ethylene furandicarboxylate): The manufacturer is Hefei Lifu Biotechnology Co., Ltd., and the brand name is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217°C.

[0087] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0088] Among them, the process parameters of melt blending spinning are: screw speed 31r / min, screw zone 1 temperature 250℃, zone 2 temperature 255℃, zone 3 temperature 260℃, zone 4 temperature 265℃, zone 5 temperature 260℃, zone 6 temperature 255℃, spinning box temperature 265℃, pump supply 890g / min, pressure difference between inlet and return air of annular blowing 740Pa, winding speed 1050m / min;

[0089] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0090] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 95°C;

[0091] The linear density of polyethylene furandicarboxylate fiber is 3.40 dtex, the linear density deviation rate is 0.7%, the fiber breaking strength is 4.1 cN / dtex, the breaking elongation is 61.5%, the ultra-long fiber content is 1.2 mg / 100 g, the defect content is 3.5 mg / 100 g, the number of crimps is 12 / 25 mm, the crimp rate is 14%, and the boiling water shrinkage is 70%.

[0092] Example 6

[0093] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0094] (1) Preparation of raw materials;

[0095] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0096] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0097] Among them, the process parameters of melt blending spinning are: screw speed 33r / min, screw zone 1 temperature 250℃, zone 2 temperature 255℃, zone 3 temperature 260℃, zone 4 temperature 265℃, zone 5 temperature 260℃, zone 6 temperature 255℃, spinning box temperature 265℃, pump supply 940g / min, pressure difference between inlet and return air of annular blowing 720Pa, winding speed 1050m / min;

[0098] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0099] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.35 times, and the temperature of tense heat setting is 90°C;

[0100] The linear density of polyethylene furandicarboxylate fiber is 3.84 dtex, the linear density deviation rate is -0.3%, the fiber breaking strength is 4.0 cN / dtex, the breaking elongation is 60.2%, the ultra-long fiber content is 1.4 mg / 100 g, the defect content is 4.0 mg / 100 g, the number of crimps is 12.5 / 25 mm, the crimp rate is 17.1%, and the boiling water shrinkage is 75%.

[0101] Example 7

[0102] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0103] (1) Preparation of raw materials;

[0104] Poly(ethylene furandicarboxylate): The manufacturer is Hefei Lifu Biotechnology Co., Ltd., and the brand name is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217°C.

[0105] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0106] Among them, the process parameters of melt blending spinning are: screw speed 35r / min, screw zone 1 temperature 250℃, zone 2 temperature 255℃, zone 3 temperature 260℃, zone 4 temperature 265℃, zone 5 temperature 260℃, zone 6 temperature 255℃, spinning box temperature 265℃, pump supply 980g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1050m / min;

[0107] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0108] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 95°C;

[0109] The linear density of polyethylene furandicarboxylate fiber is 4.44dtex, the linear density deviation rate is 0.5%, the fiber breaking strength is 4.0cN / dtex, the breaking elongation is 55.2%, the ultra-long fiber content is 2mg / 100g, the defect content is 4.3mg / 100g, the number of crimps is 13.4 / 25mm, the crimp rate is 16.8%, and the boiling water shrinkage is 80%.

[0110] Example 8

[0111] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0112] (1) Preparation of raw materials;

[0113] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0114] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0115] Among them, the process parameters of melt blending spinning are: screw speed 30r / min, screw zone 1 temperature 255℃, zone 2 temperature 260℃, zone 3 temperature 265℃, zone 4 temperature 270℃, zone 5 temperature 265℃, zone 6 temperature 260℃, spinning box temperature 270℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0116] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0117] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.35 times, and the temperature of tense heat setting is 100°C;

[0118] The linear density of polyethylene furandicarboxylate fiber is 3.17 dtex, the linear density deviation rate is -1%, the fiber breaking strength is 3.9 cN / dtex, the breaking elongation is 59.4%, the ultra-long fiber content is 0.6 mg / 100 g, the defect content is 3.2 mg / 100 g, the number of crimps is 13.9 / 25 mm, the crimp rate is 17.3%, and the boiling water shrinkage is 80%.

[0119] Example 9

[0120] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0121] (1) Preparation of raw materials;

[0122] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0123] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0124] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0125] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0126] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0127] The linear density of polyethylene furandicarboxylate fiber is 3.10 dtex, the linear density deviation rate is 0.8%, the fiber breaking strength is 3.7 cN / dtex, the breaking elongation is 60.1%, the ultra-long fiber content is 0.6 mg / 100 g, the defect content is 3.2 mg / 100 g, the number of crimps is 14.6 / 25 mm, the crimp rate is 17.6%, and the boiling water shrinkage is 70%.

[0128] Example 10

[0129] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0130] (1) Preparation of raw materials;

[0131] Poly(ethylene furandicarboxylate): The manufacturer is Hefei Lifu Biotechnology Co., Ltd., and the brand name is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217°C.

[0132] (2) drying the polyethylene furandicarboxylate (first drying at 80° C. for 2 h, then vacuum drying at 116° C. for 9 h), and then melt-extruding the polyethylene furandicarboxylate through a screw extruder, spinning, cooling, winding, and forming the polyethylene furandicarboxylate primary yarn;

[0133] Among them, the process parameters of melt blending spinning are: screw speed 28r / min, screw zone 1 temperature 265℃, zone 2 temperature 270℃, zone 3 temperature 275℃, zone 4 temperature 280℃, zone 5 temperature 275℃, zone 6 temperature 270℃, spinning box temperature 280℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0134] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0135] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 4.00 times, and the temperature of tense heat setting is 80°C;

[0136] The linear density of polyethylene furandicarboxylate fiber is 2.22dtex, the linear density deviation rate is 0.7%, the fiber breaking strength is 3.5cN / dtex, the breaking elongation is 65.5%, the ultra-long fiber content is 0.4mg / 100g, the defect content is 3.3mg / 100g, the number of crimps is 15 / 25mm, the crimp rate is 18%, and the boiling water shrinkage is 60%.

[0137] Embodiment 11

[0138] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0139] (1) Preparation of raw materials;

[0140] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0141] (2) The polyethylene furandicarboxylate was dried (first dried at 80°C for 2 hours and then vacuum dried at 116°C for 9 hours), and then the polyethylene furandicarboxylate was mixed with poly(boranediphenylsiloxane) in a ratio of 40:1, stirred at 80°C for 10 minutes, and then vacuum dried at 100°C for 10 hours before use.

[0142] The polyethylene furandicarboxylate primary yarn is obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0143] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0144] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0145] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0146] The fiber breaking strength of the polyethylene furandicarboxylate fiber is 3.8 cN / dtex, the breaking elongation is 60.4%, and the boiling water shrinkage is 71%.

[0147] Example 12

[0148] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0149] (1) Preparation of raw materials;

[0150] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0151] (2) The polyethylene furandicarboxylate was dried (first dried at 80°C for 2 hours, then vacuum dried at 116°C for 9 hours), and then the polyethylene furandicarboxylate was mixed with dipentaerythritol hexaacrylate in a ratio of 20:1, stirred at 80°C for 10 minutes, and then vacuum dried at 100°C for 10 hours before use.

[0152] The polyethylene furandicarboxylate primary yarn is obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0153] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0154] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0155] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0156] The fiber breaking strength of the polyethylene furandicarboxylate fiber is 3.8 cN / dtex, the breaking elongation is 60.5%, and the boiling water shrinkage is 71%.

[0157] Example 13

[0158] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0159] (1) Preparation of raw materials;

[0160] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0161] (2) The polyethylene furandicarboxylate was dried (first dried at 80°C for 2 h, then vacuum dried at 116°C for 9 h), then the polyethylene furandicarboxylate was mixed with nano-silica modified silk fibroin in a ratio of 20:1, stirred at 80°C for 10 min, and then vacuum dried at 100°C for 10 h before use.

[0162] The polyethylene furandicarboxylate primary yarn is obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0163] The preparation method of nano-silica modified silk fibroin is as follows: dissolving the silk fibroin in a 0.1 mol / L formic acid solution, then adding tetraethyl orthosilicate, stirring at 600 r / min at room temperature for 2 hours, and then vacuum drying at 40°C for 7 days, wherein the tetraethyl orthosilicate is added in a ratio of 10:1 by weight of silk fibroin to silica.

[0164] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0165] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0166] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0167] The fiber breaking strength of the polyethylene furandicarboxylate fiber is 3.9 cN / dtex, the breaking elongation is 60.3%, and the boiling water shrinkage is 68%.

[0168] Embodiment 14

[0169] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0170] (1) Preparation of raw materials;

[0171] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0172] (2) The polyethylene furandicarboxylate was dried (first dried at 80°C for 2 hours and then vacuum dried at 116°C for 9 hours), and then the polyethylene furandicarboxylate was mixed with poly(boron diphenylsiloxane) and dipentaerythritol hexaacrylate in a ratio of 40:1:2, stirred at 80°C for 10 minutes, and then vacuum dried at 100°C for 10 hours before use.

[0173] The polyethylene furandicarboxylate primary yarn is obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0174] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0175] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0176] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0177] The fiber breaking strength of the polyethylene furandicarboxylate fiber is 4.0 cN / dtex, the breaking elongation is 60.9%, and the boiling water shrinkage is 72%.

[0178] Embodiment 15

[0179] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0180] (1) Preparation of raw materials;

[0181] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0182] (2) The polyethylene furandicarboxylate was dried (first dried at 80°C for 2 h, then vacuum dried at 116°C for 9 h), and then the polyethylene furandicarboxylate was mixed with poly(boron diphenylsiloxane) and nano-silica modified silk fibroin in a ratio of 40:1:2, stirred at 80°C for 10 min, and then vacuum dried at 100°C for 10 h before use.

[0183] The polyethylene furandicarboxylate primary yarn is obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0184] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0185] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0186] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0187] The fiber breaking strength of the polyethylene furandicarboxylate fiber is 4.2 cN / dtex, the breaking elongation is 60.6%, and the boiling water shrinkage is 71%.

[0188] Example 16

[0189] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0190] (1) Preparation of raw materials;

[0191] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0192] (2) The polyethylene furandicarboxylate was dried (first dried at 80°C for 2 h, then vacuum dried at 116°C for 9 h), and then the polyethylene furandicarboxylate was mixed with dipentaerythritol hexaacrylate and nano-silica modified silk fibroin in a ratio of 20:1:1, stirred at 80°C for 10 min, and then vacuum dried at 100°C for 10 h before use.

[0193] The polyethylene furandicarboxylate primary yarn is obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0194] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0195] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0196] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0197] The fiber breaking strength of the polyethylene furandicarboxylate fiber is 4.1 cN / dtex, the breaking elongation is 60.8%, and the boiling water shrinkage is 70%.

[0198] Embodiment 17

[0199] The preparation method of high shrinkage polyethylene furandicarboxylate fiber comprises the following specific steps:

[0200] (1) Preparation of raw materials;

[0201] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., the brand name is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215°C.

[0202] (2) Poly(ethylene furandicarboxylate) was dried (first dried at 80°C for 2 h, then vacuum dried at 116°C for 9 h), then poly(ethylene furandicarboxylate), poly(boranediphenylsiloxane), dipentaerythritol hexaacrylate and nano-silica modified silk fibroin were mixed in a ratio of 40:1:2:2, stirred at 80°C for 10 min, and then vacuum dried at 100°C for 10 h before use.

[0203] The polyethylene furandicarboxylate primary yarn is obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0204] Among them, the process parameters of melt blending spinning are: screw speed 29r / min, screw zone 1 temperature 260℃, zone 2 temperature 265℃, zone 3 temperature 270℃, zone 4 temperature 275℃, zone 5 temperature 270℃, zone 6 temperature 265℃, spinning box temperature 275℃, pump supply 890g / min, annular air inlet and return air pressure difference 720Pa, winding speed 1100m / min;

[0205] (3) bundling, drawing, tensile heat setting, curling, oiling, and relaxing heat setting the polyethylene furandicarboxylate spun yarn to obtain polyethylene furandicarboxylate fibers;

[0206] Among them, the process parameters of post-spinning drafting are: the oil bath temperature of the first-stage oil bath drafting is 72°C, the temperature of the second-stage drafting is 110°C, the drafting multiple is 3.25 times, and the temperature of tense heat setting is 90°C;

[0207] The fiber breaking strength of the polyethylene furandicarboxylate fiber is 4.4 cN / dtex, the breaking elongation is 61.2%, and the boiling water shrinkage is 73%.

Claims

1. A method for preparing high shrinkage polyethylene furandicarboxylate fiber, characterized in that: The high shrinkage polyethylene furandicarboxylate fiber is prepared by drying polyethylene furandicarboxylate slices and then melt-blending and spinning. The slices are polyethylene furandicarboxylate.

2. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 1, characterized in that: The intrinsic viscosity of PEF is 0.60-0.80 dL / g and the melting point is 210-230°C.

3. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 1, characterized in that: Before melt blending and spinning, the high shrinkage polyethylene furandicarboxylate is dried to a water content of less than 200 ppm.

4. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 3, characterized in that: The drying process is: first drying at 80-100°C for 2-3h, and then vacuum drying at 90-110°C for 6-10h.

5. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 1, characterized in that: The process of melt-blending and spinning high-shrinkage polyethylene furandicarboxylate to obtain high-shrinkage polyethylene furandicarboxylate fiber is as follows: melt-extrude the high-shrinkage polyethylene furandicarboxylate through a screw extruder, spin, cool, wind, and shape to obtain primary yarn. The process parameters of melt blending spinning include: screw speed 28-35r / min; screw temperature 250-280℃, spinning box temperature 265-280℃, pump supply 500-900g / min, pressure difference between inlet and return air of ring blowing 600-800Pa, winding speed 1000-1150m / min.

6. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 5, characterized in that: The raw silk is sequentially subjected to bundling, drawing, tension heat setting, crimping, oiling, and relaxation heat setting to obtain high shrinkage polyethylene furandicarboxylate fiber. The oil bath temperature in the first-stage oil bath drawing is 70-80℃, the second-stage drawing temperature is 100-120℃, the drawing multiple is 3.1-4.1 times, and the temperature of tense heat setting is 80-100℃.

7. A high shrinkage polyethylene furandicarboxylate fiber prepared by the preparation method according to any one of claims 1 to 8, characterized in that: The fiber linear density is 2.22-4.44dtex, the linear density deviation rate is -5%-5%, the fiber breaking strength is 3.5-4.5cN / dtex, the breaking elongation is 53.5-68.5%, the extra-long fiber content is 0-3mg / 100g, the defect content is 3-20mg / 100g, the number of curls is 12-15 / 25mm, the curl rate is 14%-18%, and the boiling water shrinkage is 60-80%.

8. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 1, characterized in that: The polyethylene furandicarboxylate slices are dried, treated with a stabilizer, and then melt-blended and spun to obtain high-shrinkage polyethylene furandicarboxylate fibers. The weight ratio of the polyethylene furandicarboxylate slices to the stabilizer is 10:

1.

9. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 8, characterized in that: The stabilizer comprises poly(boron diphenylsiloxane), dipentaerythritol hexaacrylate and nano-silica modified silk fibroin, and the weight ratio of the poly(boron diphenylsiloxane), dipentaerythritol hexaacrylate and nano-silica modified silk fibroin is 1:2:

2.

10. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 9, characterized in that: The step of treating the polyethylene furandicarboxylate slices with a stabilizer after drying is as follows: mixing the dried polyethylene furandicarboxylate slices with the stabilizer, stirring at 80° C. for 10 minutes, and then vacuum drying at 100° C. for 10 hours before use.

Citation Information

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