WO2018112734A1 - 一种高抗紫外功能纤维的制备方法及功能纤维与应用 - Google Patents

一种高抗紫外功能纤维的制备方法及功能纤维与应用 Download PDF

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WO2018112734A1
WO2018112734A1 PCT/CN2016/111002 CN2016111002W WO2018112734A1 WO 2018112734 A1 WO2018112734 A1 WO 2018112734A1 CN 2016111002 W CN2016111002 W CN 2016111002W WO 2018112734 A1 WO2018112734 A1 WO 2018112734A1
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Prior art keywords
fiber
fabric
preparing
spinning
functional
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PCT/CN2016/111002
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English (en)
French (fr)
Inventor
刘水平
夏清明
李伯璇
刘伟峰
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江苏启弘新材料科技有限公司
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Priority to PCT/CN2016/111002 priority Critical patent/WO2018112734A1/zh
Publication of WO2018112734A1 publication Critical patent/WO2018112734A1/zh

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent

Definitions

  • the invention belongs to the technical field of functional textile materials, and particularly relates to a preparation method and functional fiber and application of a high anti-UV functional fiber.
  • UVA having a wavelength of 320 to 400 nm
  • UVB having a wavelength of 290 to 320 nm.
  • the harm of ultraviolet rays to humans is generally caused by the combined action of UVA and UVB.
  • the existing anti-UV functional fabrics on the market are mostly processed in the future, and the additives with ultraviolet absorption function are added to the surface of the fabric, such as umbrellas, by means of coating or compounding, but this method is not resistant to washing and rubbing.
  • the effect is not lasting, and can not meet the needs of sports brands, especially outdoor sportswear; there are also fibers with anti-UV function obtained by adding ultraviolet absorber, but its UV absorption function is limited, and it can not reach the cotton to prevent ultraviolet transmission, especially It is the transmission of ultraviolet light, so it has limited protection for the human body.
  • the modified absorbent is added in an amount of not more than 2.5% because the amount of addition is too large to solve the problem of dispersibility and cannot be spun.
  • one of the objects of the present invention is to solve the deficiencies in the prior art and to provide a method for preparing a high-quality, high-anti-UV functional fiber.
  • a high anti-UV functional fiber The preparation method comprises the steps of: mixing titanium dioxide with resin powder, blending and granulating to obtain ultraviolet absorption masterbatch, drying and mixing the same with the resin slice, and melt-spinning the mixture to obtain high anti-UV fiber;
  • the blending granulation has an extrusion temperature of 160 to 350 ° C and a screw rotation speed of 150 to 2500 rpm.
  • the mass ratio of the modified ultraviolet absorber to the resin powder is 1:9 to 4:6.
  • the mixture wherein the ultraviolet absorption masterbatch has a mass percentage of 3% to 20%.
  • the modified ultraviolet absorber has a particle diameter of 30 to 100 nm.
  • the melt spinning has a spinning temperature of 270 to 290 ° C and a spinning speed of 600 to 3200 m/min.
  • the initial pressure of the module is 8-16 MPa.
  • the drying is carried out at a temperature of 125 to 135 ° C for a period of 4 to 6 hours.
  • the mixture is mixed with a resin slice, which is mixed at a rotation speed of 70 to 100 rpm for 20 to 40 minutes.
  • Another object of the present invention is to provide a highly resistant UV fiber which is excellent in mechanical properties.
  • the present invention provides the following technical solution: a high anti-UV fiber having a single filament fineness of 0.5 to 10D, a tow fineness of 10 to 150D, and a length of 30 to 150 mm.
  • Still another object of the present invention is to provide a high-anti-UV fiber for use in the preparation of fabrics.
  • the present invention provides the following technical solution: the high-anti-UV fiber is used on one side of the top wire or the bottom wire, and the fabric is obtained by weaving.
  • the high-anti-UV fiber of the present invention is added in an amount of 15% to 100% of the total mass of the fabric.
  • the mechanical properties of the fibers and fabrics produced by the present invention are extremely excellent and can reach the standard of ordinary fibers.
  • the DTY fiber has a strength of 4 cN/dtex and an elongation at break of 21%, which fully satisfies the requirements of various weaving.
  • the present invention produces fibers and fabrics in which the dispersibility of the modified absorbent enables spinning and fabric formation.
  • the functional fiber obtained by the invention has a single fiber fineness of 0.5 to 10D and a tow fineness of 10 to 150D, and can be used for developing a light and thin fabric.
  • the invention adopts a new anti-ultraviolet mechanism to prepare a new high anti-UV fiber, the fiber diameter can be made into ultra-fine fiber, the fiber can be made white, and has permanent anti-UV function.
  • Figure 1 is an SEM image of the anti-UV fiber obtained in the present invention. It can be seen from the figure that the anti-ultraviolet particles are evenly distributed in the fiber and can effectively absorb ultraviolet rays;
  • FIG. 2 is a diagram showing the mechanism of action of anti-ultraviolet fibers obtained in the present invention.
  • an embodiment or “an embodiment” as used herein refers to a particular feature, structure, or characteristic that can be included in at least one implementation of the invention.
  • the modified titanium dioxide ultraviolet absorber having a particle diameter of 100 nm is uniformly mixed with the resin powder PBT, wherein the mass ratio of the ultraviolet absorber to the resin powder is 3:7; after mixing, the mixture is extruded by twin-screw extrusion, and extruded.
  • the temperature is 275 ° C, the rotation speed is 300 rpm, the ultraviolet absorption masterbatch is obtained; the master batch is dried, the drying temperature is 130 degrees Celsius, the time is 5 hours; then the resin PET slice is evenly mixed for 30 minutes, the rotation speed is 80 rpm, in which the mass of the masterbatch is 8%, fed into a spinning machine for melt spinning, spinning temperature is 285 ° C, speed is 2900 m / min, initial pressure of spinning assembly is 12 MPa, and high anti-UV fiber is obtained.
  • the anti-UV fiber is used in the weft direction, and the mass ratio is 25%, and the target fabric 1 is obtained.
  • the modified titanium dioxide ultraviolet absorber having a particle diameter of 80 nm is uniformly mixed with the resin powder PBT, wherein the mass ratio of the ultraviolet absorber to the PBT powder is 4:6; after mixing, the mixture is granulated by twin-screw extrusion and the extrusion temperature is 275 ° C, the rotation speed is 2500 rpm, the UV absorption masterbatch is obtained; the masterbatch is dried, the drying temperature is 130 ° C, the time is 5 h; then uniformly mixed with the PET slice for 25 min, the rotation speed is 100 rpm, wherein the mass percentage of the masterbatch is 6%. Feeding into a spinning machine for melt spinning, the spinning temperature is 290 ° C, the speed is 2900 m / min, the initial pressure of the spinning assembly is 12 MPa, and the high anti-UV fiber (sample fiber 2) is obtained;
  • the woven fabric is used in the radial direction, and the mass ratio is 33%, and the target fabric 2 is obtained.
  • the modified titanium dioxide ultraviolet absorber having a particle diameter of 100 nm is uniformly mixed with the resin powder PBT, wherein the mass ratio of the ultraviolet absorber to the resin powder is 4:6; after mixing, the mixture is extruded by twin-screw extrusion, and extruded.
  • the temperature was 350 ° C, the rotation speed was 2500 rpm, and the ultraviolet absorption masterbatch was obtained; the master batch was dried, the drying temperature was 130 ° C, and the time was 5 h; after that, it was uniformly mixed with the PET slice for 30 min, and the rotation speed was 90 rpm, wherein the mass ratio of the master batch was 20 %, fed into a spinning machine for melt spinning, spinning temperature of 290 ° C, speed of 3200 m / min, initial assembly pressure of 16 MPa, to obtain high anti-UV fiber (sample fiber 3);
  • the anti-UV fiber is used in the weft direction, and the mass ratio is 100%, and the target fabric 3 is obtained.
  • the 50 nm modified titanium dioxide ultraviolet absorber is uniformly mixed with the PBT powder, wherein the mass ratio of the ultraviolet absorber to the resin powder is 3:7; after mixing, the twin-screw extrusion blending is performed, and the extrusion temperature is 275.
  • the rotation speed is 2200rpm
  • the ultraviolet absorption masterbatch is obtained
  • the masterbatch is dried, the drying temperature is 130 ° C, the time is 5h; after mixing with the PET slice, the masterbatch mass ratio is 8%, fed to the spinning machine Melt spinning, spinning temperature is 282 ° C, speed is 2900 m / min, initial pressure of spinning assembly is 12 MPa, high anti-UV fiber is prepared, and short-cutting equipment is added to prepare short fiber with length of 3.5 cm. No Preparation of woven fabric.
  • the fiber fineness was measured by a microscope projector method.
  • a microscope projector with a magnification of 500 times, a wedge ruler, and a micrometer with a graduation value of 0.01 m were used. The measured results are shown in the table below.
  • the tensile mechanical properties of the fiber were measured by a YG001N type electronic single fiber strength meter.
  • the sample pretension was 0.2 cN
  • the clamping distance was 10 mm
  • the stretching speed was 10 mm/min.
  • the measured results are shown in the table below.
  • the fabric was tested for UV protection (wavelength of 200-400 nm) using a Lambda 35 UV/Vis spectrometer. The test results are shown in the table.
  • the far-infrared emissivity of the fabric was tested using an IR-2 emissivity meter.
  • the IR-2 specifications are as follows:
  • Display method LED digital display, last position 0.001
  • the optical lens of the instrument and the window of the infrared detector are all hot pressed zinc selenide, and the transmission band is 0.5-22 ⁇ m.
  • the black body temperature is 600K
  • the energy in the 0 ⁇ 1 ⁇ m band accounts for 1/107 of the total energy
  • the energy after 22 ⁇ m accounts for 3.8% of the total energy.
  • the black body temperature is 520 K
  • the energy after 22 ⁇ m accounts for 4.3% of the total energy. Therefore, it can be considered that the emissivity in the band of 1 to 22 ⁇ m without the filter can represent the full-band emissivity.
  • Different materials have different emissivity.
  • the same material has different surface conditions and its emissivity is different.
  • brass the polished surface can be used as a bronze mirror, the emissivity is only 0.04; the surface emissivity of the vehicle light is between 0.1 and 0.2; the surface emissivity with a fine sand spray can reach 0.3; the surface emissivity with a coarse sand spray can reach 0.5; The emissivity after oxidation blackening can reach 0.6 or more.
  • the sample to be tested must be flat, the convex surface measurement value is small, the concave surface measurement value is large, and the black body is made of a very concave surface.
  • the powder must be laid flat, preferably flattened.
  • the powder is preferably coated to facilitate comparison of ingredients on the same surface condition.
  • the thickness of the coating may be such that it is not permeable to the carrier.
  • Black body temperature control This instrument measures the head black body temperature control using 0 ⁇ 400.000 °C precision microcomputer temperature controller. When measuring 8 ⁇ 14 ⁇ m band, the black body temperature is set at 250 °C, the power control is 43%, and the instrument is turned on. The upper row on the upper right side of the box shows the black body temperature measurement value, and the lower row shows the previous set value. To change the black body temperature setting value, touch the function button. After a few seconds, the upper display window changes to the SU symbol. A certain number of digits in the lower display window starts to flash. Touch the shift button ⁇ , the add button ⁇ , the sub-key ⁇ , you can set as needed, press the button again to reset the completion. After one hour of starting, the black body temperature is stable and the instrument can be calibrated.
  • Instrument calibration The black body temperature is set at 250 °C. After starting for one hour, add 8 ⁇ 14 ⁇ m filter, place the aluminum-plated compensation reference plate on the bracket directly below the test head, and position the reference board. Align the center of the straight head of the measuring head and wait for 2 minutes for stabilization before correcting. Press the MR button, the lower indicator light is on, press the value on the back of the reference board, such as the aluminum plate, its emissivity is 0.05, adjust the corresponding knob, it should display 950, and the DR signal has an effect on it, to press DR The key, see what the value is displayed, 950 minus the value of DR, is the value we should adjust. Press E key, the lower indicator light is on, showing the emissivity is 0.05.
  • Sample test Place the sample to be tested on the measuring tray. Press the E button after 3 seconds. When the indicator below is on, the emissivity value of the sample can be read. This is the last 8 ⁇ 14 ⁇ m emissivity measurement.
  • Example 4 The short fibers obtained in Example 4 were placed in a disc machine for mechanical pulping, and the disc spacing was 0.55 mm and 0.45 mm, respectively. After the end, the ground slurry was taken out and poured into a wali beater to be beaten to obtain a mechanical pulp slurry of different beating degrees.
  • the nonwoven fabric is obtained by wet molding, drying, and hot rolling.
  • the fabric was tested for UV protection (wavelength of 200-400 nm) using a Lambda 35 UV/Vis spectrometer. The test results are shown in the table.
  • the far-infrared emissivity of the fabric was tested using an IR-2 emissivity meter.
  • the IR-2 specifications are as follows:
  • Display method LED digital display, last position 0.001
  • the optical lens of the instrument and the window of the infrared detector are all hot pressed zinc selenide, and the transmission band is 0.5-22 ⁇ m.
  • the black body temperature is 600K
  • the energy in the 0 ⁇ 1 ⁇ m band accounts for 1/107 of the total energy
  • 22 The energy after ⁇ m accounts for 3.8% of the total energy.
  • the black body temperature is 520 K
  • the energy after 22 ⁇ m accounts for 4.3% of the total energy. Therefore, it can be considered that the emissivity in the band of 1 to 22 ⁇ m without the filter can represent the full-band emissivity.
  • Different materials have different emissivity.
  • the same material has different surface conditions and its emissivity is different.
  • brass the polished surface can be used as a bronze mirror, the emissivity is only 0.04; the surface emissivity of the vehicle light is between 0.1 and 0.2; the surface emissivity with a fine sand spray can reach 0.3; the surface emissivity with a coarse sand spray can reach 0.5; The emissivity after oxidation blackening can reach 0.6 or more.
  • the sample to be tested must be flat, the convex surface measurement value is small, the concave surface measurement value is large, and the black body is made of a very concave surface.
  • the powder must be laid flat, preferably flattened.
  • the powder is preferably coated to facilitate comparison of ingredients on the same surface condition.
  • the thickness of the coating may be such that it is not permeable to the carrier.
  • Black body temperature control This instrument measures the head black body temperature control using 0 ⁇ 400.000 °C precision microcomputer temperature controller. When measuring 8 ⁇ 14 ⁇ m band, the black body temperature is set at 250 °C, the power control is 43%, and the instrument is turned on. The upper row on the upper right side of the box shows the black body temperature measurement value, and the lower row shows the previous set value. To change the black body temperature setting value, touch the function button. After a few seconds, the upper display window changes to the SU symbol. A certain number of digits in the lower display window starts to flash. Touch the shift button ⁇ , the add button ⁇ , the sub-key ⁇ , you can set as needed, press the button again to reset the completion. After one hour of starting, the black body temperature is stable and the instrument can be calibrated.
  • Instrument calibration The black body temperature is set at 250 °C. After starting for one hour, add 8 ⁇ 14 ⁇ m filter, place the aluminum-plated compensation reference plate on the bracket directly below the test head, and position the reference board. Align the center of the straight head of the measuring head and wait for 2 minutes for stabilization before correcting. Press the MR button, the lower indicator light is on, press the value on the back of the reference board, such as the aluminum plate, its emissivity is 0.05, adjust the corresponding knob, it should display 950, and the DR signal has an effect on it, to press DR The key, see what the value is displayed, 950 minus the value of DR, is the value we should adjust. Press E key, the lower indicator light is on, showing the emissivity is 0.05.
  • Sample test Place the sample to be tested on the measuring tray. Press the E button after 3 seconds. When the indicator below is on, the emissivity value of the sample can be read. This is the last 8 ⁇ 14 ⁇ m emissivity measurement.
  • the mechanical properties of the fibers and fabrics produced by the invention are extremely excellent, and can reach the standard of ordinary fibers, wherein the DTY fiber has a strength of 4 cN/dtex and an elongation at break of 21%, which fully satisfies the requirements of various weaving;
  • the fiber and the fabric are obtained, wherein after the dispersibility of the modified absorbent, the spinning and the fabric can be realized;
  • the functional fiber obtained by the invention has a fineness of 0.5 to 10D and a tow fineness of 10 to 150D, which can be used for development.
  • the fiber and fabric produced by this method have excellent far-infrared radiation performance; the method has excellent sterilization effect on fibers and fabrics; the invention adopts a new anti-ultraviolet mechanism to prepare new high-anti-UV fiber, and the fiber diameter can be achieved.
  • Microfiber, fiber can be made into white, with permanent UV resistance.

Abstract

本发明提供了一种高抗紫外功能纤维的制备方法及功能纤维与应用，其中方法包括，将二氧化钛与树脂粉体混合，共混造粒，得到紫外线吸收母粒，干燥后将其同树脂切片混合，将混合物进行熔体纺丝，得到高抗紫外纤维；所述共混造粒，其挤出温度设置为160～350℃，螺杆转速为150～2500rpm。本发明制得纤维及面料机械性能极其优秀，可以达到普通纤维的标准，同时具有很强的抗紫外性能，其中，DTY纤维强度达到4cN/dtex，断裂伸长为21％，完全满足各种织造的要求。

Description

一种高抗紫外功能纤维的制备方法及功能纤维与应用 技术领域
本发明属于功能纺织材料技术领域，具体涉及一种高抗紫外功能纤维的制备方法及功能纤维与应用。
背景技术
能够到达地表的UV的成分划分为波长为320～400nm的UVA和波长为290～320nm的UVB。紫外线对人类的危害，一般是由UVA和UVB的综合作用引起。
有效的抗紫外功能一直是生产服装和装饰面料产业上想解决的问题，目前从市场调研结果来看，真正有效并且能够满足国内外标准的抗紫外面料非常少，其成本也比较高。
目前市场上现有的抗紫外功能面料以后处理方式居多，把具有紫外吸收功能的助剂通过涂覆或者复合的方式添加到面料表面，如遮阳伞等产品，但是此种方式不耐洗涤和摩擦，效果不持久，并不能满足运动品牌尤其是户外运动服装的需求；也有通过添加紫外吸收剂的方式获得具有抗紫外功能的纤维，但是其紫外吸收功能有限，不能达到全棉防止紫外线透射，尤其是紫外线的透射，因此对人体的保护能力有限。现有技术中改性吸收剂添加不超过2.5％，因为添加量过大，无法解决分散性问题，无法纺丝。
因此，开发一种新型的抗紫外功能纤维并制造相应面料，具有很重要的意义。
发明内容
本部分的目的在于概述本发明的实施例的一些方面以及简要介绍一些较佳实施例。在本部分以及本申请的说明书摘要和发明名称中可能会做些简化或省略以避免使本部分、说明书摘要和发明名称的目的模糊，而这种简化或省略不能用于限制本发明的范围。
鉴于上述和/或现有制备抗紫外功能纤维并织造相应面料的技术空白，提出了本发明。
因此，本发明其中的一个目的是解决现有技术中的不足，提供一种高质量的高抗紫外功能纤维的制备方法。
为解决上述技术问题，本发明提供了如下技术方案：一种高抗紫外功能纤 维的制备方法，包括，将二氧化钛与树脂粉体混合，共混造粒，得到紫外线吸收母粒，干燥后将其同树脂切片混合，将混合物进行熔体纺丝，得到高抗紫外纤维；所述共混造粒，其挤出温度设置为160～350℃，螺杆转速为150～2500rpm。
作为本发明所述高抗紫外功能纤维的制备方法的一种优选方案，其中：所述改性紫外线吸收剂与树脂粉体的质量比为1:9～4:6。
作为本发明所述高抗紫外功能纤维的制备方法的一种优选方案，其中：所述混合物，其中紫外线吸收母粒的质量百分比为3％～20％。
作为本发明所述高抗紫外功能纤维的制备方法的一种优选方案，其中：所述改性紫外线吸收剂粒径为30～100nm。
作为本发明所述高抗紫外功能纤维的制备方法的一种优选方案，其中：所述熔体纺丝，其纺丝温度为270～290℃，纺丝速度为600～3200m/min，纺丝组件初始压力为8～16MPa。
作为本发明所述高抗紫外功能纤维的制备方法的一种优选方案，其中：所述干燥，其温度为125～135℃，时间为4～6h。
作为本发明所述高抗紫外功能纤维的制备方法的一种优选方案，其中：所述同树脂切片混合，其是以70～100rpm的转速混合20～40min。
本发明的另一个目的是提供一种机械性能佳的高抗紫外纤维。
为解决上述技术问题，本发明提供了如下技术方案：一种高抗紫外纤维，其单丝纤度为0.5～10D，丝束纤度为10～150D，长度为30～150mm。
本发明还有一个目的是提供一种高抗紫外纤维在制备面料方面的应用。
为解决上述技术问题，本发明提供了如下技术方案：将高抗紫外纤维在面丝或底丝中的一面使用，通过机织得到面料。
作为本发明所述高抗紫外纤维在制备面料方面的应用的一种优选方案，其中：所述高抗紫外纤维，其添加量为面料总质量的15％～100％。
本发明的有益效果：
(1)本发明制得纤维及面料机械性能极其优秀，可以达到普通纤维的标准，其中，DTY纤维强度达到4cN/dtex，断裂伸长为21％，完全满足各种织造的要求。
(2)本发明制得纤维及面料，其中改性吸收剂分散性后，能够实现纺丝并制成面料。
(3)本发明制得的功能纤维单丝纤度为0.5～10D，丝束纤度为10～150D，可用于开发轻薄面料。
(4)本法明制得纤维及面料远红外辐射性能优异。
(5)本法明制得纤维及面料杀菌效果优异。
(6)本发明采用全新的抗紫外机理制备新的高抗紫外纤维，纤维直径可以做到超细纤维，纤维可以做成白色，具有永久性抗紫外功能。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其它的附图。其中：
图1为本发明得到的抗紫外纤维的SEM图。从图中可以看到抗紫外颗粒在纤维中均匀分布，可以有效的吸收紫外线；
图2为本发明得到的抗紫外纤维作用机理图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合具体实施例对本发明的具体实施方式做详细的说明。
在下面的描述中阐述了很多具体细节以便于充分理解本发明，但是本发明还可以采用其他不同于在此描述的其它方式来实施，本领域技术人员可以在不违背本发明内涵的情况下做类似推广，因此本发明不受下面公开的具体实施例的限制。
其次，此处所称的“一个实施例”或“实施例”是指可包含于本发明至少一个实现方式中的特定特征、结构或特性。在本说明书中不同地方出现的“在一个实施例中”并非均指同一个实施例，也不是单独的或选择性的与其他实施例互相排斥的实施例。
实施例1：
将粒径100nm的改性二氧化钛紫外线吸收剂与树脂粉体PBT均匀混合，其中紫外吸收剂与树脂粉体质量比为3:7；混合后经双螺杆挤出共混造粒挤出，挤出温度为275℃，转速为300rpm，得到紫外吸收母粒；将母粒干燥，干燥温度为130摄氏度，时间为5小时；后同树脂PET切片均匀混合30min，转速为 80rpm，其中母粒质量占比为8％，喂入纺丝机进行熔体纺丝，纺丝温度为285℃，速度为2900m/min，纺丝组件初始压力12MPa，制得高抗紫外纤维(样品纤维1)；
采用机织方式，将抗紫外纤维在纬向使用，质量占比为25％，得到目标面料1。
实施例2
将粒径为80nm改性二氧化钛紫外线吸收剂与树脂粉体PBT均匀混合，其中紫外吸收剂与PBT粉体质量比为4:6；混合后经双螺杆挤出共混造粒，挤出温度为275℃，转速为2500rpm，得到紫外吸收母粒；将母粒干燥，干燥温度为130℃，时间为5h；后同PET切片均匀混合25min，转速为100rpm，其中母粒质量占比为6％，喂入纺丝机进行熔体纺丝，纺丝温度为290℃，速度为2900m/min，纺丝组件初始压力12MPa，制得高抗紫外纤维(样品纤维2)；
采用机织方式，将抗紫外纤维在径向使用，质量占比为33％，得到目标面料2。
实施例3
将粒径为100nm改性二氧化钛紫外线吸收剂与树脂粉体PBT均匀混合，其中紫外吸收剂与树脂粉体质量比为4:6；混合后经双螺杆挤出共混造粒挤出，挤出温度为350℃，转速为2500rpm，得到紫外吸收母粒；将母粒干燥，干燥温度为130℃，时间为5h；后同PET切片均匀混合30min，转速为90rpm，其中母粒质量占比为20％，喂入纺丝机进行熔体纺丝，纺丝温度为290℃，速度为3200m/min，纺丝组件初始压力16MPa，制得高抗紫外纤维(样品纤维3)；
采用机织方式，将抗紫外纤维在纬向使用，质量占比为100％，得到目标面料3。
实施例4
将粒径为50nm改性二氧化钛紫外吸收剂与PBT粉体均匀混合，其中紫外吸收剂与树脂粉体质量比为3:7；混合后经双螺杆挤出共混造粒，挤出温度为275℃，转速为2200rpm，得到紫外吸收母粒；将母粒干燥，干燥温度为130℃，时间为5h；后同PET切片混合纺丝，其中母粒质量占比为8％，喂入纺丝机进行熔体纺丝，纺丝温度为282℃，速度为2900m/min，纺丝组件初始压力12MPa，制得高抗紫外纤维，同时添加短切设备，制备长度为3.5cm的短纤维，用于无 纺布的制备。
实施例5
检测其相应的功能，将实施例1～3所制得的功能纤维，与对比纤维1(普通纤维)、对比纤维2(市售普通功能纤维)进行如下测试：
细度测试
采用显微镜投影仪法测量纤维细度。采用放大倍数为500倍的显微镜投影仪、楔形尺以及分度值为0.01m的测微尺。测得结果见下表
Figure PCTCN2016111002-appb-000001
强伸性测试
用YG001N型电子单纤维强力仪测试纤维的拉伸力学性能，试样预张力为0.2cN，夹持距离为10mm，拉伸速度为10mm/min。测得结果见下表
Figure PCTCN2016111002-appb-000002
实施例6
抗紫外线性能
用Lambda35型紫外/可见光光谱仪测试织物防紫外线(波长为200～400nm)性能，测试结果见表。
Figure PCTCN2016111002-appb-000003
Figure PCTCN2016111002-appb-000004
测试远红外发射率
使用IR-2发射率测量仪测试织物远红外发射率，IR-2规格如下：
1.测量波段：8～14μm
2.发射率测量范围：0.1～0.99
3.灵敏度：0.001
4.示值误差：±0.02(>0.50)
5.重复性：±0.01
6.样品温度：常温
7.样品尺寸：≤40mm
8.测量时间：3秒后按轻触开关E，即显示测量值。
9.显示方法：LED数字显示，末位0.001
10.电源：交流220V 50HZ
测试说明
1.仪器中的光学镜头及红外探测器的窗口均采用热压硒化锌，其透过波段为0.5～22μm。当黑体温度为600K时，0～1μm波段能量占总能量的1/107，22μm以后的能量占总能量的3.8％。当黑体温度为520K时，22μm以后的能量占总能量的4.3％。所以，可认为不加滤光片时1～22μm波段的发射率可代表全波段发射率。
2.不同材料有不同的发射率。同一种材料表面状况不同，其发射率也不同。例如黄铜，抛光表面可作铜镜，发射率只有0.04；车光表面发射率在0.1～0.2之间；用细沙喷表面发射率可达0.3；用粗沙喷表面发射率可达0.5；氧化发黑后发射率可达0.6以上。
3.被测样品必须是平面，凸面测量值小，凹面测量值大，黑体就是利用非常凹的面做成的。
4.对粉料必需铺平整，最好压平。粉料最好做成涂层，便于在同等表面状况作配料对比。
5.用车光黄铜表面做载体，均匀涂上被测物可较好测出物质的发射率。涂层厚度以不透载体辐射即可。
使用方法
1.黑体控温：本仪器测量头部黑体控温采用0～400.000℃精密微机控温仪，其测8～14μm波段时，黑体温度设定在250℃，功率控制在43％，开机后仪器箱右上方上排显示黑体温度测量值，下排显示前一次的设定值。如要改变黑体温度设定值，轻触功能键，几秒钟后，上排显示窗变为SU符号，下排显示窗的某一位数开始闪烁，轻触移位键﹤，加数键△，减数键▽，即可按需设定，再按一下键，重新设定完成。开机一小时后黑体温度稳定，即可进行仪器校正。
2.仪器校正：黑体温度设置在250℃，开机一小时后，加8～14μm滤光片，把镀铝的补偿参考板置于测试头正下方托架上，并将参考板上的位置点对准测量头部直杆的中心位置，等待2分钟稳定后在行校正。按MR键,其下方指示灯亮，按参考板背面的数值，如镀铝板它的发射率为0.05，调节对应的旋扭，应该显示950，而DR这路信号对它有影响，要按DR的键，看其显示的数值为多少，950减去DR的值，才是我们应该调的值。按E键，下方指示灯亮，显示发射率为0.05。
3.样品测试：把被测样品置于测量托盘上，3秒钟后按E键，待下方指示灯亮，即可读出试样的发射率值。即为最后8～14μm发射率测量值。
测定五组面料远红外发射率，波长范围：8～14μm
Figure PCTCN2016111002-appb-000005
抗菌检测
用美国测试与材料协会ASTM E2149-2001固着性抗菌活性的动态测试法，采用金黄色葡萄球菌ATCC No.6538(革兰氏阳性菌)作实验菌种，测试单面针织物抗菌功能，测试结果见表
Figure PCTCN2016111002-appb-000006
实施例7
将实施例4所制得的短纤维放入磨盘机中进行机械法制浆，磨盘间距分别为0.55mm、0.45mm。结束后取出所磨的浆，将其倒入瓦利打浆机中打浆，以获得不同的打浆度的机械浆浆料。经湿法成型、干燥、热轧加固，制得无纺布。
抗紫外线性能
用Lambda35型紫外/可见光光谱仪测试织物防紫外线(波长为200～400nm)性能，测试结果见表
Figure PCTCN2016111002-appb-000007
测试远红外发射率
使用IR-2发射率测量仪测试织物远红外发射率，IR-2规格如下：
1.测量波段：8～14μm
2.发射率测量范围：0.1～0.99
3.灵敏度：0.001
4.示值误差：±0.02(>0.50)
5.重复性：±0.01
6.样品温度：常温
7.样品尺寸：≤40mm
8.测量时间：3秒后按轻触开关E，即显示测量值。
9.显示方法：LED数字显示，末位0.001
10.电源：交流220V 50HZ
测试说明
1.仪器中的光学镜头及红外探测器的窗口均采用热压硒化锌，其透过波段为0.5～22μm。当黑体温度为600K时，0～1μm波段能量占总能量的1/107，22 μm以后的能量占总能量的3.8％。当黑体温度为520K时，22μm以后的能量占总能量的4.3％。所以，可认为不加滤光片时1～22μm波段的发射率可代表全波段发射率。
2.不同材料有不同的发射率。同一种材料表面状况不同，其发射率也不同。例如黄铜，抛光表面可作铜镜，发射率只有0.04；车光表面发射率在0.1～0.2之间；用细沙喷表面发射率可达0.3；用粗沙喷表面发射率可达0.5；氧化发黑后发射率可达0.6以上。
3.被测样品必须是平面，凸面测量值小，凹面测量值大，黑体就是利用非常凹的面做成的。
4.对粉料必需铺平整，最好压平。粉料最好做成涂层，便于在同等表面状况作配料对比。
5.用车光黄铜表面做载体，均匀涂上被测物可较好测出物质的发射率。涂层厚度以不透载体辐射即可。
使用方法
1.黑体控温：本仪器测量头部黑体控温采用0～400.000℃精密微机控温仪，其测8～14μm波段时，黑体温度设定在250℃，功率控制在43％，开机后仪器箱右上方上排显示黑体温度测量值，下排显示前一次的设定值。如要改变黑体温度设定值，轻触功能键，几秒钟后，上排显示窗变为SU符号，下排显示窗的某一位数开始闪烁，轻触移位键﹤，加数键△，减数键▽，即可按需设定，再按一下键，重新设定完成。开机一小时后黑体温度稳定，即可进行仪器校正。
2.仪器校正：黑体温度设置在250℃，开机一小时后，加8～14μm滤光片，把镀铝的补偿参考板置于测试头正下方托架上，并将参考板上的位置点对准测量头部直杆的中心位置，等待2分钟稳定后在行校正。按MR键,其下方指示灯亮，按参考板背面的数值，如镀铝板它的发射率为0.05，调节对应的旋扭，应该显示950，而DR这路信号对它有影响，要按DR的键，看其显示的数值为多少，950减去DR的值，才是我们应该调的值。按E键，下方指示灯亮，显示发射率为0.05。
3.样品测试：把被测样品置于测量托盘上，3秒钟后按E键，待下方指示灯亮，即可读出试样的发射率值。即为最后8～14μm发射率测量值。
测定所述无纺布面料远红外发射率，波长范围：8～14μm
Figure PCTCN2016111002-appb-000008
抗菌检测
用美国测试与材料协会ASTM E2149-2001固着性抗菌活性的动态测试法，采用金黄色葡萄球菌ATCC No.6538(革兰氏阳性菌)作实验菌种，测试单面针织物抗菌功能，测试结果见表
Figure PCTCN2016111002-appb-000009
由此可见，本发明制得纤维及面料机械性能极其优秀，可以达到普通纤维的标准，其中，DTY纤维强度达到4cN/dtex，断裂伸长为21％，完全满足各种织造的要求；本发明制得纤维及面料，其中改性吸收剂分散性后，能够实现纺丝并制成面料；本发明制得的功能纤维单丝纤度为0.5～10D，丝束纤度为10～150D，可用于开发轻薄面料；本法明制得纤维及面料远红外辐射性能优异；本法明制得纤维及面料杀菌效果优异；本发明采用全新的抗紫外机理制备新的高抗紫外纤维，纤维直径可以做到超细纤维，纤维可以做成白色，具有永久性抗紫外功能。
应说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围当中。

Claims (10)

  1. 一种高抗紫外功能纤维的制备方法，其特征在于：包括，
    将二氧化钛与树脂粉体混合，共混造粒，得到紫外线吸收母粒，干燥后将其同树脂切片混合，将混合物进行熔体纺丝，得到高抗紫外纤维；
    所述共混造粒，其挤出温度设置为160～350℃，螺杆转速为150～2500rpm。
  2. 根据权利要求1所述高抗紫外功能纤维及面料的制备方法，其特征在于：所述改性紫外线吸收剂与树脂粉体的质量比为1:9～4:6。
  3. 根据权利要求1或2所述高抗紫外功能纤维及面料的制备方法，其特征在于：所述混合物，其中紫外线吸收母粒的质量百分比为3％～20％。
  4. 根据权利要求1所述高抗紫外功能纤维及面料的制备方法，其特征在于：所述改性紫外线吸收剂粒径为30～100nm。
  5. 根据权利要求1、2或4中任一项所述高抗紫外功能纤维及面料的制备方法，其特征在于：所述熔体纺丝，其纺丝温度为270～290℃，纺丝速度为600～3200m/min，纺丝组件初始压力为8～16MPa。
  6. 根据权利要求1所述高抗紫外功能纤维及面料的制备方法，其特征在于：所述干燥，其温度为125～135℃，时间为4～6h。
  7. 根据权利要求1、2、4或6中任一项所述高抗紫外功能纤维及面料的制备方法，其特征在于：所述同树脂切片混合，其是以70～100rpm的转速混合20～40min。
  8. 一种高抗紫外纤维，其特征在于：一种高抗紫外纤维，其单丝纤度为0.5～10D，丝束纤度为10～150D，长度为30～150mm。
  9. 一种利用权利要求8所述高抗紫外纤维在制备面料方面的应用，其特征在于：将高抗紫外纤维在面丝或底丝中的一面使用，通过机织得到面料。
  10. 根据权利要求9所述制备面料的方法，其特征在于：所述高抗紫外纤维，其添加量为面料总质量的15％～100％。
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CN114481454A (zh) * 2022-01-20 2022-05-13 苏州沐兮新材料科技有限公司 一种射线防护用pet织物的制备方法及防护织物
CN114953628A (zh) * 2022-04-02 2022-08-30 江苏洁瑞雅纺织品有限公司 一种抗紫外线面料及其加工方法

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