A preparation method of high-shrinkage polyethylene furandicarboxylate fiber

Abstract

The present invention belongs to the technical field of the preparation of bio-based functional fibers, and relates to a preparation method of highly shrinkable polyethylene furandicarboxylate fibers. Preparation method: The polyethylene furandicarboxylate chips are dried and then melt-blended and spun to obtain highly shrinkable polyethylene furandicarboxylate fibers. The linear density of the fibers is 2.22 - 4.44 dtex, and the linear density deviation rate is -5% - 5%. The breaking strength of the fibers is 3.5 - 4.5 cN / dtex, the breaking elongation rate is 53.5 - 68.5%, the content of ultra-long fibers is 0 - 3 mg / 100 g, the content of defects is 3 - 20 mg / 100 g, the number of crimps is 12 - 15 per 25 mm, the crimp rate is 14% - 18%, and the boiling water shrinkage rate is 60 - 80%. The highly shrinkable polyethylene furandicarboxylate fibers prepared by the present invention are 100% highly shrinkable polyester fibers, and the fiber properties far exceed those of conventional highly shrinkable fibers, and can become an alternative product to PET.

Description

Technical Field

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

[0002] Governments and international organizations around the world have introduced relevant policies to promote green and low-carbon development in response to the challenges of global environmental problems. The "Implementation Plan for the Innovation and Development of the Fine Chemical Industry (2024-2027)" issued by nine departments including the Ministry of Industry and Information Technology requires focusing on building a bio-based material system based on the utilization of non-grain biomass resources such as large-scale crop straws and residues, developing bio-based chemicals such as furan, bio-based polymers such as polyethylene furandicarboxylate (PEF), etc., to form an effective supplement to existing fossil-based materials. PEF is a 100% bio-based material synthesized by adding FDCA as a monomer to a diol through a direct esterification method or a transesterification method. It has a very high similarity in structure to PET and similar properties. It is the material most likely to achieve similar or better performance than PET polyester. In the industry, PEF is also known as the next-generation polyester, with huge potential.

[0003] However, during the PEF spinning process, due to the replacement of the benzene ring structure in PET by FDCA, the asymmetry and permanent dipole moment of the furan ring result in restricted molecular chain movement and increased steric hindrance between molecules, making the orientation and crystallization properties of the molecular chain in the PEF spinning process poor, and further causing a decrease in the fiber breaking strength and elongation at break. CN117209735 discloses a method for preparing a cation-dyeable high-shrinkage furandicarboxylic acid polyester and fibers. The cation-dyeable high-shrinkage furandicarboxylic acid polyester chips are dried, then metered, cooled, bundled, heat-drawn, and wound through a screw extruder. The highest fiber breaking strength reaches 3.4 cN / dtex, but its elongation at break is only 17%. CN 117286598 discloses a low-heat-shrinkage bio-based furan copolyester fiber and its preparation method. This invention involves the formulation design of FDCA and mixed diols. Through a polymerization process combined with a heat setting and stretching process, a low-shrinkage bio-based furan copolyester fiber is prepared. The highest breaking strength of the PEF fiber reaches 3.8 cN / dtex, and the elongation at break is 33.2%. Based on the environmental protection and good mechanical properties of PEF fibers, they can be blended with wool, rabbit hair, etc. to make products such as cashmere-like and wool-like fabrics. However, animal hairs usually have the characteristic of high shrinkage. Therefore, by designing and preparing high-shrinkage PEF products, they can easily curl into loops, be fluffy and round like yarns, and the blended yarns with wool, rabbit hair, etc. are light, fluffy, have a soft wool-like feel, and good warmth retention. In addition, due to the increase in oxygen-containing functional groups in the PEF molecular chain, its hydrophilicity is enhanced, and the blended yarns also have the property of moisture absorption and sweat discharge.

[0004] Commercially available high-shrinkage polyester products are mainly produced by chemical-physical methods, that is, raw filaments are obtained by drying, melt spinning, winding, and barrel forming of high-shrinkage polyester chips; a certain number of raw filaments are obtained through post-spinning first-stage oil bath drawing, second-stage cold drawing, filament stacking, curling, oiling, low-temperature drying in an oven, cutting, and packing. However, high-shrinkage bio-based products have not yet appeared. Therefore, blending bio-based high-shrinkage fibers with natural animal hairs (such as wool, rabbit hair, etc.) to prepare yarns not only conforms to the environmental protection concept of green development but also has very important significance for the high-value application of bio-based fibers. Summary of the Invention

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

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

[0007] A preparation method for high-shrinkage polyethylene furandicarboxylate fibers, wherein polyethylene furandicarboxylate chips are dried and then melt-blended and spun to obtain high-shrinkage polyethylene furandicarboxylate fibers.

[0008] As a preferred technical solution:

[0009] In the preparation method for high-shrinkage polyethylene furandicarboxylate fibers as described above, the intrinsic viscosity of PEF is 0.60 - 0.80 dL / g, and the melting point is 210 - 230 °C.

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

[0011] In the preparation method for high-shrinkage polyethylene furandicarboxylate fibers as described above, the drying process is as follows: first dry at 80 - 100 °C for 2 - 3 h, and then vacuum dry at 90 - 110 °C for 6 - 10 h.

[0012] In the preparation method for high-shrinkage polyethylene furandicarboxylate fibers as described above, the process of melt-blending and spinning high-shrinkage polyethylene furandicarboxylate to obtain high-shrinkage polyethylene furandicarboxylate fibers is as follows: melt-extrude high-shrinkage polyethylene furandicarboxylate through a screw extruder, spin, cool, wind, and form to obtain a nascent filament,

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

[0014] The preparation method of the high-shrinkage polyethylene furandicarboxylate fiber as described above, the nascent filament is successively subjected to bunching, drawing, tension heat setting, crimping, oiling, and relaxation heat setting to obtain the high-shrinkage polyethylene furandicarboxylate fiber.

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

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

[0017] As a preferred technical solution:

[0018] For the high-shrinkage polyethylene furandicarboxylate fiber as described above, the fiber breaking strength is 3.5 - 4.5 cN / dtex, the breaking elongation rate is 53.5 - 68.5%. The boiling water shrinkage rate is 60% - 80%, the content of ultra-long fibers is 0 - 3 mg / 100 g, the content of defects is 3 - 20 mg / 100 g, the number of crimps is 12 - 15 per 25 mm, and the crimp ratio is 14% - 18%.

[0019] As a preferred technical solution:

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

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

[0022] The stabilization agent treatment step for the dried polyethylene furandicarboxylate chips is to mix the dried polyethylene furandicarboxylate chips with the stabilization agent, stir at 80°C for 10 minutes, and then vacuum dry at 100°C for 10 hours before use.

[0023] Based on the above technical solution, lubrication and plasticization are carried out by poly(borodiphenylsiloxane) and dipentaerythritol hexaacrylate, so that the binding strength between nano-silica modified silk fibroin and polyethylene furandicarboxylate is increased, thereby enhancing the fiber strength. At the same time, the excellent reactivity of dipentaerythritol hexaacrylate makes poly(borodiphenylsiloxane) 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 by melt polycondensation. FDCA and diol are directly reacted to form an esterified product, and then PEF is synthesized by polycondensation. This method has the advantages of low raw material consumption, short reaction time, gentle reaction rate, high relative molecular mass of the product, and no harmful by-products, so 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 transesterification stage, the esterification temperature is 190 - 210°C, which is 30°C lower than that of PET; in the polycondensation stage, the temperature is 240 - 245°C, which is 40°C lower than that of PET. This not only increases the safety and controllability of the reaction, reduces the probability of safety accidents such as fires and explosions, but also reduces energy consumption, and indirectly reduces greenhouse gas emissions. The spinning of PEF is similar to the melt spinning process of PET, but the PEF obtained under these conditions has the characteristics of high viscosity and low melting point, so it will have varying degrees of influence on the screw speed, screw temperature, barrel temperature, ring blowing pressure, post-spinning drawing temperature, and drawing rate during the spinning process. It is not difficult to obtain PEF fibers by melt spinning, but it is not easy to prepare high-shrinkage PEF fibers 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 rate.

[0026] The present invention starts from the drying process of high-shrinkage polyethylene furandicarboxylate (PEF) chips, and adopts a combination of programmed temperature rise and programmed vacuum pumping 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 too high melt viscosity. At the same time, the set screw temperature is ensured to maintain its fluidity and extrusion volume. In the fiber spinning and forming stage, the ring blowing pressure is increased to promote rapid crystallization and solidification to obtain the nascent fiber. In the post-spinning stage, the draw temperature is increased to ensure the uniformity of drawing, and at the same time, the setting temperature is reduced to ensure the stability of fiber forming.

[0027] Beneficial effects:

[0028] (1) The preparation method used in the present invention has low requirements for 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 properties far exceed those of PET high-shrinkage fibers and can be comparable to them, and can become an alternative product to PET. Specific embodiments

[0030] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these examples are only used to illustrate the present invention and not 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 also fall within the scope defined by the appended claims of this application.

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

[0032] Crystallinity: Tested according to the standard of GB / T 19466.3-2004.

[0033] Softening temperature: Tested according to the standard of GB / T 1633-2000.

[0034] Intrinsic viscosity: Tested according to the standard of GB / T 14190-2017.

[0035] Melting point: Tested according to the standard of GB / T 14190-2017.

[0036] Linear density, super-long fiber content: Determined according to the standard of GB / T 14335-2008.

[0037] Tensile strength, elongation at break: Determined according to the standard of GB / T 14337-2022, where the tensile speed is 30 mm / min.

[0038] Defect content: It is measured with reference to the standard of GB / T 14339-2008.

[0039] Number of crimps, crimp ratio: It is measured with reference to the standard of GB / T 14338-2022.

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

[0041] Example 1

[0042] A preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0043] (1) Preparation of raw materials;

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

[0045] (2) Dry the polyethylene furandicarboxylate (first dry it at 80 °C for 2 h, and then vacuum dry it at 116 °C for 9 h), and then melt-extrude, spin, cool, wind, and form the polyethylene furandicarboxylate through a screw extruder to obtain polyethylene furandicarboxylate nascent filaments;

[0046] Among them, the process parameters of melt-blending spinning are: screw speed 31 r / min, temperature of the first zone of the screw 250 °C, temperature of the second zone 255 °C, temperature of the third zone 260 °C, temperature of the fourth zone 265 °C, temperature of the fifth zone 260 °C, temperature of the sixth zone 255 °C, temperature of the spinning box 265 °C, pump supply 890 g / min, pressure difference between the inlet and outlet of the ring blowing 720 Pa, winding speed 1050 m / min;

[0047] (3) Bundle, draw, tension heat-set, crimp, oil, and relaxation heat-set the polyethylene furandicarboxylate nascent filaments to obtain polyethylene furandicarboxylate fibers;

[0048] Among them, the process parameters of post-spinning drawing are: temperature of the first oil bath drawing oil bath 72 °C, temperature of the second drawing 110 °C, drawing ratio 3.25 times, temperature of tension heat-setting 80 °C;

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

[0050] Comparative Example 1

[0051] Patent Application CN117286598, a preparation method of a high-shrinkage furan copolyester fiber with low heat shrinkage, which is different only in that: 2,5-furandicarboxylic acid and a mixed diol are subjected to copolymerization reaction to obtain a high-shrinkage furan copolyester chip; the high-shrinkage furan copolyester chip is spun to obtain a high-shrinkage furan copolyester fiber with low heat shrinkage; the resulting high-shrinkage furan copolyester fiber has an intrinsic viscosity of 0.75 dL / g, a melting point of 242 °C, a breaking strength of 3.8 cN / dtex, and a breaking elongation of 33.2%.

[0052] Compared with the examples, the intrinsic viscosity and melting point of the high-shrinkage furan copolyester chip in the comparative example are significantly higher. Especially the melting point is relatively close to that of PET. Therefore, this breaking strength can be achieved under conventional processing techniques. By purchasing a high-viscosity (0.752 dL / g) chip and spinning it under the process conditions of Example 1, it is found that the breaking strength can reach 4.8 cN / dtex and the breaking elongation is 46.5%, which are significantly higher than the data in the comparative example.

[0053] Comparative Example 2

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

[0055] In this comparative example, terephthalic acid and furandicarboxylic acid are simultaneously introduced into the molecular chain for copolymerization. Compared with PEF, the molecular chain regularity of the high-shrinkage 2,5-furandicarboxylic acid-based copolyester fiber is better. Therefore, the obtained breaking strength and breaking elongation are similar to those of PET. Terephthalic acid belongs to the product of petroleum cracking and is a non-renewable resource. The fibers in this comparative example are not 100% high-shrinkage materials, and there are still potential safety hazards of microplastics in subsequent degradation.

[0056] Example 2

[0057] Preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0058] (1) Preparation of raw materials;

[0059] Polyethylene furandicarboxylate: The manufacturer is Hefei Lifu Biotechnology Co., Ltd., and the grade is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217 °C.

[0060] (2) Dry the polyethylene furandicarboxylate (first dry at 80 °C for 2 h, then vacuum dry at 116 °C for 9 h), and then melt-extrude, spin, cool, wind up, and form the polyethylene furandicarboxylate through a screw extruder to obtain the as-spun polyethylene furandicarboxylate filament;

[0061] Among them, the process parameters of melt blending and spinning are: screw speed 31 r / min, temperature of the first zone of the screw 250 °C, temperature of the second zone 255 °C, temperature of the third zone 260 °C, temperature of the fourth zone 265 °C, temperature of the fifth zone 260 °C, temperature of the sixth zone 255 °C, temperature of the spinning box 265 °C, pump supply 890 g / min, pressure difference between the inlet and outlet air of the ring blower 720 Pa, winding speed 1050 m / min;

[0062] (3) Bundle, draw, tension heat set, crimp, oil, and relaxation heat set the as-spun polyethylene furandicarboxylate filament to obtain the polyethylene furandicarboxylate fiber;

[0063] Among them, the process parameters of post-spinning drawing are: oil bath temperature of the first-stage oil bath drawing 72 °C, temperature of the second-stage drawing 110 °C, draw ratio 3.35 times, temperature of the tension heat setting 90 °C;

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

[0065] Example 3

[0066] Preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0067] (1) Preparation of raw materials;

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

[0069] (2) The polyethylene furandicarboxylate is dried (first dried at 80 °C for 2 h, and then vacuum dried at 116 °C for 9 h), and then the polyethylene furandicarboxylate is melt extruded, spun, cooled, wound, and formed through a screw extruder to obtain the as-spun polyethylene furandicarboxylate filament;

[0070] Among them, the process parameters of the melt blending and spinning are as follows: the screw speed is 31 r / min, the temperature of the first zone of the screw is 250 °C, the temperature of the second zone is 255 °C, the temperature of the third zone is 260 °C, the temperature of the fourth zone is 265 °C, the temperature of the fifth zone is 260 °C, the temperature of the sixth zone is 255 °C, the temperature of the spinning box is 265 °C, the pump supply rate is 890 g / min, the pressure difference between the inlet and outlet air of the ring blower is 720 Pa, and the winding speed is 1100 m / min;

[0071] (3) The as-spun polyethylene furandicarboxylate filament is bundled, drawn, tension heat set, crimped, oiled, and relaxed heat set to obtain the polyethylene furandicarboxylate fiber;

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

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

[0074] Example 4

[0075] A method for preparing high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0076] (1) Preparation of raw materials;

[0077] Polyethylene furandicarboxylate: The manufacturer is Hefei Leaf Biotechnology Co., Ltd., and the grade is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217 °C.

[0078] (2) The polyethylene furandicarboxylate is dried (first dried at 80 °C for 2 h, and then vacuum dried at 116 °C for 9 h), and then the polyethylene furandicarboxylate is melt extruded, spun, cooled, wound, and formed through a screw extruder to obtain the as-spun polyethylene furandicarboxylate filament;

[0079] Among them, the process parameters of melt blending and spinning are as follows: screw rotation speed 31 r / min, temperature of the first zone of the screw 250 °C, temperature of the second zone 255 °C, temperature of the third zone 260 °C, temperature of the fourth zone 265 °C, temperature of the fifth zone 260 °C, temperature of the sixth zone 255 °C, temperature of the spinning box 265 °C, pump supply rate 890 g / min, pressure difference between the inlet and return air of the ring blower 740 Pa, winding speed 1050 m / min;

[0080] (3) Subject the as-spun polyethylene furandicarboxylate filaments to bundling, drawing, stress heat setting, crimping, oiling, and relaxation heat setting to obtain polyethylene furandicarboxylate fibers;

[0081] Among them, the process parameters of post-spinning drawing are as follows: oil bath temperature of the first-stage oil bath drawing 72 °C, temperature of the second-stage drawing 110 °C, draw ratio 3.35 times, temperature of the stress heat setting 100 °C;

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

[0083] Example 5

[0084] A method for preparing high-shrinkage polyethylene furandicarboxylate fibers, the specific steps are as follows:

[0085] (1) Preparation of raw materials;

[0086] Polyethylene furandicarboxylate: The manufacturer is Hefei Leaf Biotechnology Co., Ltd., and the grade is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217 °C.

[0087] (2) Dry the polyethylene furandicarboxylate (first dry at 80 °C for 2 h, then vacuum dry at 116 °C for 9 h), and then melt-extrude, spin, cool, wind, and form the polyethylene furandicarboxylate through a screw extruder to obtain as-spun polyethylene furandicarboxylate filaments;

[0088] Among them, the process parameters of melt blending and spinning are as follows: screw rotation speed 31 r / min, temperature of the first zone of the screw 250 °C, temperature of the second zone 255 °C, temperature of the third zone 260 °C, temperature of the fourth zone 265 °C, temperature of the fifth zone 260 °C, temperature of the sixth zone 255 °C, temperature of the spinning box 265 °C, pump supply rate 890 g / min, pressure difference between the inlet and return air of the ring blower 740 Pa, winding speed 1050 m / min;

[0089] (3) The virgin polyethylene furandicarboxylate filaments are bundled, drawn, heat-set under tension, crimped, oiled, and heat-set under relaxation to obtain polyethylene furandicarboxylate fibers;

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

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

[0092] Example 6

[0093] A method for preparing high-shrinkage polyethylene furandicarboxylate fibers, the specific steps are as follows:

[0094] (1) Preparation of raw materials;

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

[0096] (2) The polyethylene furandicarboxylate is dried (first dried at 80 °C for 2 h, and then vacuum dried at 116 °C for 9 h), and then the polyethylene furandicarboxylate is melt-extruded, spun, cooled, wound, and formed by a screw extruder to obtain virgin polyethylene furandicarboxylate filaments;

[0097] Among them, the process parameters of melt-blending spinning are: the screw speed is 33 r / min, the temperature of the first zone of the screw is 250 °C, the temperature of the second zone is 255 °C, the temperature of the third zone is 260 °C, the temperature of the fourth zone is 265 °C, the temperature of the fifth zone is 260 °C, the temperature of the sixth zone is 255 °C, the temperature of the spinning box is 265 °C, the pump supply rate is 940 g / min, the pressure difference between the inlet and outlet air of the ring blowing is 720 Pa, and the winding speed is 1050 m / min;

[0098] (3) The virgin polyethylene furandicarboxylate filaments are bundled, drawn, heat-set under tension, crimped, oiled, and heat-set under relaxation to obtain polyethylene furandicarboxylate fibers;

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

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

[0101] Example 7

[0102] A preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0103] (1) Preparation of raw materials;

[0104] Polyethylene furandicarboxylate: The manufacturer is Hefei Leaf Biotechnology Co., Ltd., and the grade is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217 °C.

[0105] (2) Dry the polyethylene furandicarboxylate (first dry at 80 °C for 2 h, then vacuum dry at 116 °C for 9 h), and then melt-extrude, spin, cool, wind up, and form the polyethylene furandicarboxylate through a screw extruder to obtain the polyethylene furandicarboxylate nascent fiber;

[0106] Among them, the process parameters of the melt blending and spinning are: screw speed 35 r / min, temperature of the first zone of the screw 250 °C, temperature of the second zone 255 °C, temperature of the third zone 260 °C, temperature of the fourth zone 265 °C, temperature of the fifth zone 260 °C, temperature of the sixth zone 255 °C, temperature of the spinning box 265 °C, pump supply 980 g / min, pressure difference between the inlet and outlet of the ring blowing 720 Pa, winding speed 1050 m / min;

[0107] (3) Bundle, draw, tension heat set, crimp, oil, and relaxation heat set the polyethylene furandicarboxylate nascent fiber to obtain the polyethylene furandicarboxylate fiber;

[0108] Among them, the process parameters of the post-spinning drawing are: oil bath temperature of the first-stage oil bath drawing 72 °C, temperature of the second-stage drawing 110 °C, drawing ratio 3.25 times, temperature of the tension heat setting 95 °C;

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

[0110] Example 8

[0111] Preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0112] (1) Preparation of raw materials;

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

[0114] (2) Dry the polyethylene furandicarboxylate (first dry at 80 °C for 2 h, then vacuum dry at 116 °C for 9 h), and then melt-extrude, spin, cool, wind up and form the polyethylene furandicarboxylate through a screw extruder to obtain the as-spun polyethylene furandicarboxylate filament;

[0115] Among them, the process parameters of melt blending and spinning are: screw speed 30 r / min, temperature of the first zone of the screw 255 °C, temperature of the second zone 260 °C, temperature of the third zone 265 °C, temperature of the fourth zone 270 °C, temperature of the fifth zone 265 °C, temperature of the sixth zone 260 °C, temperature of the spinning box 270 °C, pump supply 890 g / min, pressure difference between the inlet and outlet air of the ring blower 720 Pa, winding speed 1100 m / min;

[0116] (3) Bundle, draw, tension heat set, crimp, oil, and relaxation heat set the as-spun polyethylene furandicarboxylate filament to obtain polyethylene furandicarboxylate fiber;

[0117] Among them, the process parameters of post-spinning drawing are: oil bath temperature of the first-stage oil bath drawing 72 °C, temperature of the second-stage drawing 110 °C, drawing ratio 3.35 times, temperature of tension heat setting 100 °C;

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

[0119] Example 9

[0120] Preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0121] (1) Preparation of raw materials;

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

[0123] (2) The polyethylene furandicarboxylate is dried (first dried at 80 °C for 2 h, then vacuum dried at 116 °C for 9 h), and then the polyethylene furandicarboxylate is melt extruded, spun, cooled, wound, and formed through a screw extruder to obtain the as-spun polyethylene furandicarboxylate filament;

[0124] Among them, the process parameters of the melt blending and spinning are as follows: screw speed 29 r / min, temperature of the first zone of the screw 260 °C, temperature of the second zone 265 °C, temperature of the third zone 270 °C, temperature of the fourth zone 275 °C, temperature of the fifth zone 270 °C, temperature of the sixth zone 265 °C, temperature of the spinning box 275 °C, pump supply 890 g / min, pressure difference between the inlet and outlet air of the ring blower 720 Pa, winding speed 1100 m / min;

[0125] (3) The as-spun polyethylene furandicarboxylate filament is bundled, drawn, tension heat set, crimped, oiled, and relaxed heat set to obtain the polyethylene furandicarboxylate fiber;

[0126] Among them, the process parameters of the post-spinning drawing are as follows: oil bath temperature of the first-stage oil bath drawing 72 °C, temperature of the second-stage drawing 110 °C, drawing ratio 3.25 times, temperature of the tension heat setting 90 °C;

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

[0128] Example 10

[0129] A method for preparing high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0130] (1) Preparation of raw materials;

[0131] Polyethylene furandicarboxylate: The manufacturer is Hefei Leaf Biotechnology Co., Ltd., and the grade is PEF; the intrinsic viscosity of PEF is 0.66 dL / g, and the melting point is 217 °C.

[0132] (2) The polyethylene furandicarboxylate is dried (first dried at 80 °C for 2 h, then vacuum dried at 116 °C for 9 h), and then the polyethylene furandicarboxylate is melt extruded, spun, cooled, wound, and formed through a screw extruder to obtain the as-spun polyethylene furandicarboxylate filament;

[0133] Among them, the process parameters of melt blending and spinning are as follows: screw rotation speed 28 r / min, temperature of the first zone of the screw 265 °C, temperature of the second zone 270 °C, temperature of the third zone 275 °C, temperature of the fourth zone 280 °C, temperature of the fifth zone 275 °C, temperature of the sixth zone 270 °C, temperature of the spinning box 280 °C, pump supply 890 g / min, pressure difference between the inlet and outlet air of the ring blower 720 Pa, winding speed 1100 m / min;

[0134] (3) The poly(ethylene furandicarboxylate) nascent filaments are bundled, drawn, heat-set under tension, crimped, oiled, and heat-set under relaxation to obtain poly(ethylene furandicarboxylate) fibers;

[0135] Among them, the process parameters of post-spinning drawing are as follows: oil bath temperature of the first-stage oil bath drawing 72 °C, drawing temperature of the second stage 110 °C, drawing ratio 4.00 times, temperature of heat-setting under tension 80 °C;

[0136] The linear density of the poly(ethylene furandicarboxylate) fiber is 2.22 dtex, and the deviation rate of linear density is 0.7%. The fiber breaking strength is 3.5 cN / dtex, the breaking elongation is 65.5%, the content of over-length fibers is 0.4 mg / 100 g, the content of defects is 3.3 mg / 100 g, the number of crimps is 15 per 25 mm, the crimp ratio is 18%, and the boiling water shrinkage rate is 60%.

[0137] Example 11

[0138] A method for preparing high-shrinkage poly(ethylene furandicarboxylate) fibers, the specific steps are as follows:

[0139] (1) Preparation of raw materials;

[0140] Poly(ethylene furandicarboxylate): The manufacturer is Hefei Lifu Biotechnology Co., Ltd., and the grade is PEF; the intrinsic viscosity of PEF is 0.65 dL / g, and the melting point is 215 °C.

[0141] (2) The poly(ethylene furandicarboxylate) is dried (first dried at 80 °C for 2 h, and then vacuum dried at 116 °C for 9 h), and then the poly(ethylene furandicarboxylate) is mixed with poly(borodiphenylsiloxane) in a ratio of 40:1, stirred at 80 °C for 10 min, and then vacuum dried at 100 °C for 10 h before use.

[0142] The poly(ethylene furandicarboxylate) nascent filaments are 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) The as-spun polyethylene furandicarboxylate filaments are bundled, drawn, heat-set under tension, crimped, oiled, and heat-set under relaxation to obtain polyethylene furandicarboxylate fibers;

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

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

[0157] Example 13

[0158] A method for preparing high-shrinkage polyethylene furandicarboxylate fibers, the specific steps are as follows:

[0159] (1) Preparation of raw materials;

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

[0161] (2) The polyethylene furandicarboxylate is dried (first dried at 80 °C for 2 h, and then vacuum dried at 116 °C for 9 h), and then the polyethylene furandicarboxylate is 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 as-spun polyethylene furandicarboxylate filaments are obtained by melt extrusion, spinning, cooling, winding, and forming through a screw extruder;

[0163] The preparation method of nano-silica modified silk fibroin is to dissolve silk fibroin in a 0.1 mol / L formic acid solution, then add tetraethyl orthosilicate, stir at 600 r / min at room temperature for 2 h, and then vacuum dry at 40 °C for 7 d, where tetraethyl orthosilicate is added according to the weight ratio of silk fibroin to silica of 10:1.

[0164] Among them, the process parameters of melt blending and spinning are: screw speed 29 r / min, temperature of the first zone of the screw 260 °C, temperature of the second zone 265 °C, temperature of the third zone 270 °C, temperature of the fourth zone 275 °C, temperature of the fifth zone 270 °C, temperature of the sixth zone 265 °C, temperature of the spinning box 275 °C, pump supply 890 g / min, pressure difference between the inlet and outlet of the ring blower 720 Pa, winding speed 1100 m / min;

[0165] (3) The virgin polyethylene furandicarboxylate filaments are bundled, drawn, tension heat-set, crimped, oiled, and relaxation heat-set to obtain polyethylene furandicarboxylate fibers;

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

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

[0168] Example 14

[0169] A method for preparing high-shrinkage polyethylene furandicarboxylate fibers, the specific steps are as follows:

[0170] (1) Preparation of raw materials;

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

[0172] (2) The polyethylene furandicarboxylate is dried (first dried at 80 °C for 2 h, and then vacuum dried at 116 °C for 9 h), and then the polyethylene furandicarboxylate, poly(borodiphenylsiloxane), and dipentaerythritol hexaacrylate are mixed 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.

[0173] The virgin polyethylene furandicarboxylate filaments are obtained by melt extrusion, spinning, cooling, winding, and forming through a screw extruder;

[0174] Among them, the process parameters of melt blending and spinning are: the screw speed is 29 r / min, the temperature of the first zone of the screw is 260 °C, the temperature of the second zone is 265 °C, the temperature of the third zone is 270 °C, the temperature of the fourth zone is 275 °C, the temperature of the fifth zone is 270 °C, the temperature of the sixth zone is 265 °C, the temperature of the spinning box is 275 °C, the pump supply rate is 890 g / min, the pressure difference between the inlet and outlet of the ring blowing air is 720 Pa, and the winding speed is 1100 m / min;

[0175] (3) The virgin polyethylene furandicarboxylate filaments are bundled, drawn, tension heat-set, crimped, oiled, and relaxation heat-set to obtain polyethylene furandicarboxylate fibers;

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

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

[0178] Example 15

[0179] A preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0180] (1) Preparation of raw materials;

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

[0182] (2) Dry the polyethylene furandicarboxylate (first dry at 80 °C for 2 h, then vacuum dry at 116 °C for 9 h), and then mix the polyethylene furandicarboxylate with poly(borodiphenylsiloxane) and nano-silica modified silk fibroin in a ratio of 40:1:2, stir at 80 °C for 10 min, and then vacuum dry at 100 °C for 10 h before use.

[0183] Melt extrude, spin, cool, wind up and form the polyethylene furandicarboxylate nascent fiber through a screw extruder;

[0184] Among them, the process parameters of melt blending and spinning are: screw speed 29 r / min, temperature of the first zone of the screw 260 °C, temperature of the second zone 265 °C, temperature of the third zone 270 °C, temperature of the fourth zone 275 °C, temperature of the fifth zone 270 °C, temperature of the sixth zone 265 °C, temperature of the spinning box 275 °C, pump supply 890 g / min, pressure difference between the inlet and outlet of the ring blowing 720 Pa, winding speed 1100 m / min;

[0185] (3) Bundle, draw, tension heat set, crimp, oil, and relaxation heat set the polyethylene furandicarboxylate nascent fiber to obtain polyethylene furandicarboxylate fiber;

[0186] Among them, the process parameters of post-spinning drawing are: oil bath temperature of the first-stage oil bath drawing 72 °C, temperature of the second-stage drawing 110 °C, drawing ratio 3.25 times, temperature of tension heat setting 90 °C;

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

[0188] Example 16

[0189] A preparation method of high-shrinkage polyethylene furandicarboxylate fiber, the specific steps are as follows:

[0190] (1) Preparation of raw materials;

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

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

[0193] The as-spun polyethylene furandicarboxylate filaments are obtained by melt extrusion, spinning, cooling, winding and forming through a screw extruder;

[0194] Among them, the process parameters of melt blending and spinning are: screw speed 29 r / min, temperature of the first zone of the screw 260 °C, temperature of the second zone 265 °C, temperature of the third zone 270 °C, temperature of the fourth zone 275 °C, temperature of the fifth zone 270 °C, temperature of the sixth zone 265 °C, temperature of the spinning box 275 °C, pump supply 890 g / min, pressure difference between the inlet and outlet air of the ring blower 720 Pa, winding speed 1100 m / min;

[0195] (3) Bundle, draw, tension heat set, crimp, oiling and relaxation heat set the as-spun polyethylene furandicarboxylate filaments to obtain polyethylene furandicarboxylate fibers;

[0196] Among them, the process parameters of post-spinning drawing are: oil bath temperature of the first-stage oil bath drawing 72 °C, temperature of the second-stage drawing 110 °C, draw ratio 3.25 times, temperature of the tension heat setting 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 rate is 70%.

[0198] Example 17

[0199] A method for preparing high-shrinkage polyethylene furandicarboxylate fibers, the specific steps are as follows:

[0200] (1) Preparation of raw materials;

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

[0202] (2) The polyethylene furandicarboxylate was dried (first dried at 80 °C for 2 h, and then vacuum dried at 116 °C for 9 h). Then, the polyethylene furandicarboxylate, poly(borodiphenylsiloxane), 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 as-spun polyethylene furandicarboxylate filaments were obtained by melt extrusion, spinning, cooling, winding, and shaping through a screw extruder.

[0204] Among them, the process parameters for melt blending and spinning were as follows: screw speed 29 r / min, temperature of the first zone of the screw 260 °C, temperature of the second zone 265 °C, temperature of the third zone 270 °C, temperature of the fourth zone 275 °C, temperature of the fifth zone 270 °C, temperature of the sixth zone 265 °C, temperature of the spinning box 275 °C, pump supply 890 g / min, pressure difference between the inlet and outlet of the ring blower 720 Pa, winding speed 1100 m / min.

[0205] (3) The as-spun polyethylene furandicarboxylate filaments were bundled, drawn, tension heat-set, crimped, oiled, and relaxed heat-set to obtain polyethylene furandicarboxylate fibers.

[0206] Among them, the process parameters for post-spinning drawing were as follows: oil bath temperature for the first-stage oil bath drawing 72 °C, drawing temperature for the second stage 110 °C, drawing ratio 3.25 times, temperature for tension heat-setting 90 °C.

[0207] The fiber breaking strength of the polyethylene furandicarboxylate fiber was 4.4 cN / dtex, the breaking elongation was 61.2%, and the boiling water shrinkage rate was 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, wherein the slices are polyethylene furandicarboxylate; The polyethylene furandicarboxylate slices are dried, treated with a stabilizer, and then melt-blended and spun to obtain high-shrinkage polyethylene furandicarboxylate fibers, wherein the weight ratio of the polyethylene furandicarboxylate slices to the stabilizer is 10:1; The stabilizer comprises poly(boron diphenylsiloxane), dipentaerythritol hexaacrylate and nano-silica modified silk fibroin, wherein the weight ratio of the poly(boron diphenylsiloxane), dipentaerythritol hexaacrylate and nano-silica modified silk fibroin is 1:2:2; The step of treating the polyethylene furandicarboxylate slices with a stabilizer after drying is as follows: mixing the dried polyethylene furandicarboxylate slices with a stabilizer, stirring at 80° C. for 10 minutes, and then vacuum drying at 100° C. for 10 hours before use; wherein, before melt blending and spinning, the high shrinkage polyethylene furandicarboxylate is dried to a water content of less than 200 ppm.

2. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 1, characterized in that: The intrinsic viscosity of polyethylene furandicarboxylate 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: The drying process is: first drying at 80-100°C for 2-3h, and then vacuum drying at 90-110°C for 6-10h.

4. 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 28-35 r / 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.

5. The method for preparing high shrinkage polyethylene furandicarboxylate fiber according to claim 4, 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℃.

6. A high shrinkage polyethylene furandicarboxylate fiber prepared by the preparation method according to any one of claims 1 to 5, 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 crimps is 12-15 / 25mm, the crimp rate is 14%-18%, and the boiling water shrinkage is 60-80%.