CN110685027B - Preparation method of polymer optical fiber - Google Patents
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- CN110685027B CN110685027BCN201910831732.8ACN201910831732ACN110685027BCN 110685027 BCN110685027 BCN 110685027BCN 201910831732 ACN201910831732 ACN 201910831732ACN 110685027 BCN110685027 BCN 110685027B
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
- 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
- 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
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
- 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
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
- 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
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- Textile Engineering (AREA)
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- Multicomponent Fibers (AREA)
Abstract
Translated fromChinese
Description
Translated fromChinese技术领域technical field
本发明属于光信息材料与纺织材料交叉领域，尤其涉及装饰用面料所涉及的光纤材料，具体涉及一种聚合物光纤的制备方法。The invention belongs to the cross field of optical information materials and textile materials, in particular to an optical fiber material related to decorative fabrics, and in particular to a preparation method of a polymer optical fiber.
背景技术Background technique
目前纺织领域已有人采用光纤(光导纤维)作为一种原料进行制备发光织物，例如通过将光纤与棉纱相交织，同时对织物中的光纤进行集束处理，并将集束后的光纤与一定光源进行耦连，形成光纤发光织物，但是目前的光纤基本是由玻璃或者塑料聚合物制成的纤维，即以聚甲基丙烯酸甲酯(PMMA)为芯层，氟树脂作为包裹芯层的皮层，例如中国发明CN104164734A(其公开了一种聚甲基丙烯酸甲酯光纤纱线，包括内芯和外裹层，内芯为聚甲基丙烯酸甲酯，外裹层为氟树脂)，又如中国发明专利CN103380240A(其公开了一种光照织物、一种光照皮肤设备、一种成套设备及其实施方法，公开了其采用的光纤为：光纤纤芯为聚甲基丙烯酸甲酯，光纤包层为氟化高聚物)，上述光纤的制备方法主要是预制件-拉伸法，即先将材料通过一定方法制成具有一定外观结，然后将预制件置于拉伸装置中加热并拉伸成上千米的光导纤维；然而此类光纤传输效率高，可用作光传导工具，但是性脆、弹性和柔软性等性能较差，在纺织领域的编织和应用过程中易断裂、舒适性不够，同时氟树脂成本高昂，因此较难以在装饰用面料中得到大规模的应用。At present, some people in the textile field have used optical fibers (optical fibers) as a raw material to prepare light-emitting fabrics. For example, by interweaving the optical fibers with cotton yarn, the fibers in the fabric are bundled, and the bundled optical fibers are coupled with a certain light source. However, the current optical fiber is basically a fiber made of glass or plastic polymer, that is, with polymethyl methacrylate (PMMA) as the core layer and fluororesin as the skin layer surrounding the core layer, such as China Invention CN104164734A (which discloses a polymethyl methacrylate optical fiber yarn, including an inner core and an outer coating, the inner core is polymethyl methacrylate, and the outer coating is fluororesin), another example is Chinese invention patent CN103380240A (It discloses a lighted fabric, a lighted skin device, a complete set of equipment and its implementation method, and discloses that the optical fiber used is: the optical fiber core is polymethyl methacrylate, and the optical fiber cladding is fluorinated high (polymer), the preparation method of the above-mentioned optical fiber is mainly the preform-stretching method, that is, the material is first made into a knot with a certain appearance by a certain method, and then the preform is placed in a stretching device and heated and stretched to thousands of meters. However, this type of optical fiber has high transmission efficiency and can be used as a light transmission tool, but has poor performance such as brittleness, elasticity and softness, and is easy to break and is not comfortable enough during weaving and application in the textile field. The high cost of resin makes it difficult to obtain large-scale application in decorative fabrics.
发明内容SUMMARY OF THE INVENTION
本发明所要解决的技术问题是克服现有技术中的不足，提供一种兼具较低的光损、极佳的韧性并能够适用于装饰用面料的聚合物光纤的制备方法。The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, and to provide a method for preparing a polymer optical fiber with low light loss, excellent toughness and suitable for decorative fabrics.
为解决以上技术问题，本发明采取的技术方案如下：In order to solve the above technical problems, the technical scheme adopted by the present invention is as follows:
一种聚合物光纤的制备方法，所述聚合物光纤包括芯层、设置于所述芯层外周的皮层，所述芯层的材料包括聚碳酸酯，所述皮层的材料包括改性聚对苯二甲酸乙二酯和/或透明尼龙，所述改性聚对苯二甲酸乙二酯的全光线透过率为88％-90％、折射率为1.45-1.50，所述透明尼龙的全光线透过率为90％-92％、折射率为1.47-1.52，所述聚碳酸酯的折射率为1.55-1.59，所述聚碳酸酯的折射率与所述改性聚对苯二甲酸乙二酯的折射率的差值占所述聚碳酸酯的折射率的百分含量为5％-8％，所述聚碳酸酯的折射率与所述透明尼龙的折射率的差值占所述聚碳酸酯的折射率的百分含量为4％-6％；A preparation method of a polymer optical fiber, the polymer optical fiber comprises a core layer and a skin layer arranged on the outer periphery of the core layer, the material of the core layer comprises polycarbonate, and the material of the skin layer comprises modified polyparaphenylene Ethylene dicarboxylate and/or transparent nylon, the modified polyethylene terephthalate has a total light transmittance of 88%-90% and a refractive index of 1.45-1.50, and the transparent nylon has a total light transmittance of 88%-90%. The transmittance is 90%-92%, the refractive index is 1.47-1.52, the refractive index of the polycarbonate is 1.55-1.59, and the refractive index of the polycarbonate is the same as that of the modified polyethylene terephthalate. The difference in the refractive index of the ester accounts for 5%-8% of the refractive index of the polycarbonate, and the difference between the refractive index of the polycarbonate and the transparent nylon accounts for the polycarbonate. The percentage of refractive index of carbonate is 4%-6%;
所述聚合物光纤的制备方法包括如下步骤：The preparation method of the polymer optical fiber comprises the following steps:
(1)将所述芯层的材料与所述皮层的材料分别进行干燥处理；(1) drying the material of the core layer and the material of the skin layer respectively;
(2)将步骤(1)处理后的所述芯层的材料与所述皮层的材料分别加入双螺杆熔融纺丝机的两个螺杆中经喷丝板在真空条件下挤出，制成粗品；(2) The material of the core layer and the material of the skin layer treated in step (1) are respectively added to the two screws of the twin-screw melt spinning machine and extruded under vacuum conditions through a spinneret to make a crude product ;
(3)将所得的所述粗品经水冷，再经不同速度的牵伸辊牵伸，制成所述聚合物光纤。(3) The obtained crude product is water-cooled, and then drawn by drawing rollers with different speeds to prepare the polymer optical fiber.
根据本发明的一些优选且具体的方面，步骤(2)中，当所述皮层的材料为改性聚对苯二甲酸乙二酯时，设定所述皮层的材料所在的螺杆后区温度为275-285℃，前区温度为280-290℃，箱体温度为280-290℃；当所述皮层的材料为透明尼龙时，设定所述皮层的材料所在的螺杆后区温度为220-225℃，前区温度为225-230℃，箱体温度为225-230℃。According to some preferred and specific aspects of the present invention, in step (2), when the material of the skin layer is modified polyethylene terephthalate, the temperature of the rear area of the screw where the material of the skin layer is located is set to be 275-285°C, the temperature of the front zone is 280-290°C, and the temperature of the box is 280-290°C; when the material of the skin layer is transparent nylon, the temperature of the rear zone of the screw where the material of the skin layer is located is set to 220- 225℃, the temperature of the front zone is 225-230℃, and the temperature of the box is 225-230℃.
根据本发明的一些优选且具体的方面，步骤(2)中，设定所述芯层的材料所在的螺杆后区温度为275-280℃，前区温度为280-285℃，箱体温度为285-290℃。According to some preferred and specific aspects of the present invention, in step (2), the temperature of the rear area of the screw where the material of the core layer is located is set to be 275-280°C, the temperature of the front area to be 280-285°C, and the temperature of the box body to be 285-290℃.
根据本发明的一些优选且具体的方面，步骤(2)中，设定所述喷丝板的温度为280-290℃。According to some preferred and specific aspects of the present invention, in step (2), the temperature of the spinneret is set to be 280-290°C.
根据本发明的一些优选方面，步骤(2)中，所述双螺杆熔融纺丝机的两个螺杆分别设置与其自身配合的真空泵，所述真空泵用于抽出空气及由于高温而从原料切片内散发出的水蒸气，从而使生成的材料内气泡减少，可提高光传输效率。According to some preferred aspects of the present invention, in step (2), the two screws of the twin-screw melt-spinning machine are respectively provided with vacuum pumps that cooperate with themselves, and the vacuum pumps are used to extract air and emit air from the raw material chips due to high temperature. The outgoing water vapor can reduce the air bubbles in the generated material, which can improve the light transmission efficiency.
根据本发明的一些优选且具体的方面，步骤(3)中，所述水冷的温度为50-60℃。According to some preferred and specific aspects of the present invention, in step (3), the temperature of the water cooling is 50-60°C.
根据本发明的一些优选且具体的方面，步骤(3)中，所述牵伸辊牵伸后的牵伸比为1∶1.5-4。According to some preferred and specific aspects of the present invention, in step (3), the drafting ratio after drafting by the drafting roller is 1:1.5-4.
根据本发明的一些优选方面，所述改性聚对苯二甲酸乙二酯通过如下方法制备而得：将聚对苯二甲酸乙二酯、苯乙烯和丙烯酸酯的共聚物、环烯烃聚合物和聚苯乙烯混合、熔融挤出而制成。According to some preferred aspects of the present invention, the modified polyethylene terephthalate is prepared by combining polyethylene terephthalate, a copolymer of styrene and acrylate, a cyclic olefin polymer It is mixed with polystyrene and made by melt extrusion.
根据本发明的一些优选且具体的方面，所述聚对苯二甲酸乙二酯、所述苯乙烯和丙烯酸酯的共聚物、所述环烯烃聚合物和所述聚苯乙烯的投料质量比为1∶0.018-0.048∶0.018-0.036∶0.027-0.048。According to some preferred and specific aspects of the present invention, the mass ratio of the polyethylene terephthalate, the copolymer of styrene and acrylate, the cyclic olefin polymer and the polystyrene is: 1: 0.018-0.048: 0.018-0.036: 0.027-0.048.
根据本发明的一些优选且具体的方面，所述改性聚对苯二甲酸乙二酯的制备过程中，所述熔融挤出采用螺杆挤出机进行，熔融挤出的温度为：一区275～280℃，二区280-285℃，三区285-290℃，箱体温度285-290℃，模头温度285-290℃。According to some preferred and specific aspects of the present invention, in the preparation process of the modified polyethylene terephthalate, the melt extrusion is carried out by a screw extruder, and the temperature of the melt extrusion is: 275 in the first zone ～280℃, the second zone is 280-285℃, the third zone is 285-290℃, the box temperature is 285-290℃, and the die temperature is 285-290℃.
根据本发明的一些优选且具体的方面，所述改性聚对苯二甲酸乙二酯以ISO1133标准在280℃条件下、载荷37.3N时测定的熔融指数为44-59g/10min。According to some preferred and specific aspects of the present invention, the modified polyethylene terephthalate has a melt index of 44-59 g/10min measured according to ISO1133 at 280° C. and a load of 37.3 N.
根据本发明的一些优选且具体的方面，所述透明尼龙以ISO 1133标准在230℃条件下、载荷37.3N时测定的熔融指数为20-26g/10min。According to some preferred and specific aspects of the present invention, the transparent nylon has a melt index of 20-26 g/10min measured according to ISO 1133 at 230° C. under a load of 37.3 N.
根据本发明的一些优选且具体的方面，所述聚碳酸酯以ISO 1133标准在300℃条件下、载荷37.3N时测定的熔融指数为19-23g/10min。According to some preferred and specific aspects of the present invention, the polycarbonate has a melt index of 19-23 g/10min measured according to ISO 1133 at 300°C and a load of 37.3N.
根据本发明的一些优选方面，所述聚碳酸酯的折射率与所述改性聚对苯二甲酸乙二酯的折射率的差值占所述聚碳酸酯的折射率的百分含量为5.5％-7.6％，所述聚碳酸酯的折射率与所述透明尼龙的折射率的差值占所述聚碳酸酯的折射率的百分含量为4.5％-5.5％。According to some preferred aspects of the present invention, the difference between the refractive index of the polycarbonate and the refractive index of the modified polyethylene terephthalate accounts for 5.5 percent of the refractive index of the polycarbonate. %-7.6%, the difference between the refractive index of the polycarbonate and the refractive index of the transparent nylon accounts for 4.5%-5.5% of the refractive index of the polycarbonate.
根据本发明，全光线指的是可见光(近红外线到近紫外线)，全光线透过率就是指这所有的光的透过率。According to the present invention, total light refers to visible light (near-infrared to near-ultraviolet), and total light transmittance refers to the transmittance of all light.
由于以上技术方案的采用，本发明与现有技术相比具有如下优点：Due to the adoption of the above technical solutions, the present invention has the following advantages compared with the prior art:
本发明制备的聚合物光纤采用特定的材料作为皮层材料，并控制皮层材料与芯层材料的折射率关系，制成后不仅能够兼具极佳的韧性、较低的光损耗，同时基于材质的特殊性使其能够采用熔融纺丝法进行制备，克服了现有技术中采用预制件-拉伸法制备存在效率较低的缺陷，同时兼具价格更低廉，使得本发明方法制备的聚合物光纤尤为适用于装饰用面料这种较短程光传输的发光织物中。The polymer optical fiber prepared by the invention adopts a specific material as the skin layer material, and controls the refractive index relationship between the skin layer material and the core layer material. The particularity makes it possible to use the melt spinning method for preparation, overcoming the defect of low efficiency in the preparation of the preform-drawing method in the prior art, and at the same time, the price is lower, making the polymer optical fiber prepared by the method of the present invention. Especially suitable for luminous fabrics with short-range light transmission such as decorative fabrics.
附图说明Description of drawings
图1是本发明聚合物光纤制备工艺结构示意图；1 is a schematic structural diagram of the preparation process of the polymer optical fiber of the present invention;
图2为本发明聚合物光纤的其中一种结构示意图；FIG. 2 is a schematic structural diagram of one of the polymer optical fibers of the present invention;
图3为本发明聚合物光纤的其中一种结构的横截面示意图；3 is a schematic cross-sectional view of one of the structures of the polymer optical fiber of the present invention;
图4为本发明聚合物光纤的其中一种结构的横截面示意图；4 is a schematic cross-sectional view of one of the structures of the polymer optical fiber of the present invention;
图5为本发明聚合物光纤的其中一种结构的横截面示意图；5 is a schematic cross-sectional view of one of the structures of the polymer optical fiber of the present invention;
图6为本发明聚合物光纤的其中一种结构的横截面示意图；6 is a schematic cross-sectional view of one of the structures of the polymer optical fiber of the present invention;
图7为本发明聚合物光纤的其中一种结构的横截面示意图。7 is a schematic cross-sectional view of one of the structures of the polymer optical fiber of the present invention.
具体实施方式Detailed ways
以下结合具体实施例对上述方案做进一步说明；应理解，这些实施例是用于说明本发明的基本原理、主要特征和优点，而本发明不受以下实施例的范围限制；实施例中采用的实施条件可以根据具体要求做进一步调整，未注明的实施条件通常为常规实验中的条件。下述中，如无特殊说明，所有的原料均来自于商购或者通过本领域的常规方法制备而得。The above scheme will be further described below in conjunction with specific examples; it should be understood that these examples are used to illustrate the basic principles, main features and advantages of the present invention, and the present invention is not limited by the scope of the following examples; The implementation conditions can be further adjusted according to specific requirements, and the unspecified implementation conditions are usually those in routine experiments. In the following, unless otherwise specified, all raw materials are commercially available or prepared by conventional methods in the art.
下述中，改性聚对苯二甲酸乙二酯的熔融指数以ISO 1133标准在280℃条件下、载荷37.3N时测定；透明尼龙的熔融指数以ISO 1133标准在230℃条件下、载荷37.3N时测定；聚碳酸酯的熔融指数以ISO 1133标准在300℃条件下、载荷37.3N时测定。In the following, the melt index of modified polyethylene terephthalate is measured according to ISO 1133 at 280°C and a load of 37.3N; the melt index of transparent nylon is measured according to ISO 1133 at 230°C and a load of 37.3 N. Measured at N; the melt index of polycarbonate is measured according to ISO 1133 at 300°C and a load of 37.3N.
实施例1Example 1
如图1所示，下述实施例中各聚合物光纤的制备所采用的结构系统包括分别分列于两侧的两个料斗(11)、两个计量泵(12)、两个螺杆(13)(即双螺杆挤出机的两个螺杆)、两个分别与所述两个螺杆配合抽真空的真空泵(14)(真空泵(14)用于抽出空气及由于高温而从切片内散发出的水蒸气，从而使材料内气泡减少，提高光传输效率)，以及分别与所述两个螺杆出口连通的纺丝模头(15)，水冷池(16)、牵拉辊(17)、收卷装置(18)；在物料材料进入纺丝模头(15)前，两组装置均为料斗(11)与计量泵(12)相连，然后接入螺杆(13)，每个螺杆(13)上安装有一个真空泵(14)；原料切片后经过螺杆(13)的加热，进入纺丝模头(15)，挤出，接着挤出的粗品纤维经过水冷池(16)水冷，再经过多个配速不同的牵拉辊(17)的拉伸，将光纤拉细并使纤维内大分子取向度提高，最后由一个收卷装置(18)收集。As shown in FIG. 1 , the structural system used in the preparation of each polymer optical fiber in the following embodiments includes two hoppers (11), two metering pumps (12), two screws (13), which are respectively arranged on both sides. ) (that is, the two screws of the twin-screw extruder), two vacuum pumps (14) which are respectively cooperated with the two screws to evacuate (the vacuum pump (14) is used for drawing out the air and the air emitted from the slice due to the high temperature. water vapor, so as to reduce the bubbles in the material and improve the light transmission efficiency), and the spinning die head (15), the water cooling pool (16), the pulling roller (17), the winding and A device (18); before the material enters the spinning die head (15), the two sets of devices are connected to the hopper (11) and the metering pump (12), and then connected to the screw (13), and each screw (13) is connected to the A vacuum pump (14) is installed; after the raw material is sliced, it is heated by the screw (13), enters the spinning die head (15), and is extruded, and then the extruded crude fiber is cooled by the water cooling pool (16), and then passed through a number of dispensing processes. The stretching of the pulling rollers (17) with different speeds makes the optical fibers thin and increases the orientation degree of macromolecules in the fibers, and finally is collected by a winding device (18).
实施例2Example 2
本例提供一种聚合物光纤，如图2所示，包括芯层(32)、包覆在芯层(32)外表面的皮层(31)，芯层(32)的材料为聚碳酸酯(PC，折射率为1.59，熔融指数为22g/10min)，皮层(31)的材料为改性聚对苯二甲酸乙二酯(改性PET，全光线透过率为90％，折射率为1.49，熔融指数为44g/10min)，其横截面如图3所示。This example provides a polymer optical fiber, as shown in FIG. 2, comprising a core layer (32), a skin layer (31) covering the outer surface of the core layer (32), and the material of the core layer (32) is polycarbonate (32). PC, the refractive index is 1.59, the melt index is 22g/10min), the material of the skin layer (31) is modified polyethylene terephthalate (modified PET, the total light transmittance is 90%, the refractive index is 1.49) , the melt index is 44g/10min), and its cross-section is shown in Figure 3.
上述的改性聚对苯二甲酸乙二酯通过如下方法制备而得：其由以下重量份的原料组成：聚对苯二甲酸乙二酯100份、苯乙烯和丙烯酸酯的共聚物(NAS)2份、环烯烃聚合物(COP)3份、聚苯乙烯3份；制备方法为：The above-mentioned modified polyethylene terephthalate is prepared by the following method: it is made up of the raw materials of the following parts by weight: 100 parts of polyethylene terephthalate, styrene and acrylate copolymer (NAS) 2 parts, 3 parts of cycloolefin polymer (COP), 3 parts of polystyrene; the preparation method is:
(1)在高速混合机里添加各原料，搅拌20分钟，得预混料；(1) Add each raw material in a high-speed mixer, and stir for 20 minutes to obtain a premix;
(2)将所得预混料置于螺杆挤出机中进行熔融共混(温度参数：一区275～280℃，二区280℃，三区285℃，箱体温度285℃，模头温度285℃)、挤出，冷却，切片，即可得到所述改性聚对苯二甲酸乙二酯。(2) The obtained premix is placed in a screw extruder for melt blending (temperature parameters: 275 to 280°C in the first zone, 280°C in the second zone, 285°C in the third zone, 285°C in the box, and 285°C in the die head. ℃), extrusion, cooling, and slicing to obtain the modified polyethylene terephthalate.
聚合物光纤的制备方法包括如下步骤：The preparation method of polymer optical fiber includes the following steps:
(1)将上述制备的改性PET切片在120℃的真空干燥箱中干燥8小时，将PC切片在120℃的真空干燥箱中干燥8小时，分别得到干燥后的改性PET和PC切片；(1) The modified PET chips prepared above were dried in a vacuum drying oven at 120°C for 8 hours, and the PC chips were dried in a vacuum drying oven at 120°C for 8 hours to obtain respectively dried modified PET and PC chips;
(2)将干燥后的改性PET和PC切片分别加入双螺杆熔融纺丝机的两个螺杆中，改性PET组分设定螺杆后区温度280℃、前区温度285℃、箱体温度285℃，PC组分设定螺杆后区温度280℃、前区温度285℃、箱体温度285℃，喷丝板温度285℃；(2) The dried modified PET and PC chips were added to the two screws of the twin-screw melt spinning machine respectively, and the modified PET component was set to a temperature of 280°C in the rear area of the screw, a temperature of 285°C in the front area, and a temperature of the box body. 285℃, PC component set the temperature of the rear area of the screw to 280℃, the temperature of the front area to 285℃, the temperature of the box body to 285℃, and the temperature of the spinneret to be 285℃;
(3)经过皮芯结构(核壳结构)的纺丝模头纺丝成型；(3) Spinning through a spinning die with a skin-core structure (core-shell structure);
(4)经过水冷池55℃冷却，由牵拉辊牵伸，牵伸比1：3，并由收卷装置收集成卷。(4) After cooling in a water-cooled pool at 55°C, it is drawn by a drawing roller with a draw ratio of 1:3, and collected into a roll by a winding device.
该光纤截面接LED光源，皮层(31)可侧发光，芯层(32)的厚度为600μm，皮层(31)的厚度为60μm，将此纤维与常用的纺织纤维经针织或机织等工艺，可以获得发光织物。The cross section of the optical fiber is connected to an LED light source, the skin layer (31) can emit light from the side, the thickness of the core layer (32) is 600 μm, and the thickness of the skin layer (31) is 60 μm. Luminous fabrics are available.
实施例3Example 3
本例提供一种聚合物光纤，包括芯层(34)、第一聚合物材料层、第二聚合物材料层、第一聚合物材料层、第二聚合物材料层和皮层(33)，第一聚合物材料层、皮层(33)的材料分别为改性聚对苯二甲酸乙二酯(改性PET，全光线透过率为90％，折射率为1.50，熔融指数为59g/10min)，第二聚合物材料层、芯层(34)的材料分别为聚碳酸酯(PC，折射率为1.59，熔融指数为23g/10min)，其横截面如图4所示。This example provides a polymer optical fiber, comprising a core layer (34), a first polymer material layer, a second polymer material layer, a first polymer material layer, a second polymer material layer, and a skin layer (33). A polymer material layer and a skin layer (33) are respectively made of modified polyethylene terephthalate (modified PET, with a total light transmittance of 90%, a refractive index of 1.50, and a melt index of 59g/10min) , the materials of the second polymer material layer and the core layer (34) are respectively polycarbonate (PC, refractive index is 1.59, melt index is 23g/10min), and the cross section is shown in FIG. 4 .
上述的改性聚对苯二甲酸乙二酯通过如下方法制备而得：其由以下重量份的原料组成：聚对苯二甲酸乙二酯100份、苯乙烯和丙烯酸酯的共聚物(NAS)2份、环烯烃聚合物(COP)2份、聚苯乙烯3份；制备方法为：The above-mentioned modified polyethylene terephthalate is prepared by the following method: it is made up of the raw materials of the following parts by weight: 100 parts of polyethylene terephthalate, styrene and acrylate copolymer (NAS) 2 parts, 2 parts of cycloolefin polymer (COP), 3 parts of polystyrene; the preparation method is:
(1)在高速混合机里添加各原料，搅拌20分钟，得预混料；(1) Add each raw material in a high-speed mixer, and stir for 20 minutes to obtain a premix;
(2)将所得预混料置于螺杆挤出机中进行熔融共混(温度参数：一区275～280℃，二区280℃，三区285℃，箱体温度285℃，模头温度285℃)、挤出，冷却，切片，即可得到所述改性聚对苯二甲酸乙二酯。(2) The obtained premix is placed in a screw extruder for melt blending (temperature parameters: 275 to 280°C in the first zone, 280°C in the second zone, 285°C in the third zone, 285°C in the box, and 285°C in the die head. ℃), extrusion, cooling, and slicing to obtain the modified polyethylene terephthalate.
聚合物光纤的制备方法包括如下步骤：The preparation method of polymer optical fiber includes the following steps:
(1)将上述制备的改性PET切片在120℃的真空干燥箱中干燥8小时，将PC切片在120℃的真空干燥箱中干燥8小时，分别得到干燥后的改性PET和PC切片；(1) The modified PET chips prepared above were dried in a vacuum drying oven at 120°C for 8 hours, and the PC chips were dried in a vacuum drying oven at 120°C for 8 hours to obtain respectively dried modified PET and PC chips;
(2)将干燥后的改性PET和PC切片分别加入双螺杆熔融纺丝机的两个螺杆中，PET组分设定螺杆后区温度283℃、前区温度288℃、箱体温度288℃，PC组分设定螺杆后区温度280℃、前区温度285℃、箱体温度290℃，喷丝板温度290℃；(2) Add the dried modified PET and PC chips to the two screws of the twin-screw melt-spinning machine respectively, and the PET component is set to have a temperature of 283°C in the rear area of the screw, a temperature of 288°C in the front area, and a temperature of 288°C in the box. , PC components set the temperature of the rear area of the screw to 280℃, the temperature of the front area to 285℃, the temperature of the box body to 290℃, and the temperature of the spinneret to 290℃;
(3)经过多层皮芯结构的纺丝模头纺丝成型；(3) Spinning through a spinning die with a multi-layer skin-core structure;
(4)经过水冷池60℃冷却，由牵拉辊牵伸，牵伸比1：2，并由收卷装置收集成卷。(4) After cooling in a water-cooled pool at 60°C, it is drawn by a drawing roller with a draw ratio of 1:2, and collected into a roll by a winding device.
皮层(33)的厚度为650nm，第一聚合物材料层、第二聚合物材料层的厚度分别为110nm，芯层(34)的直径为600nm，该光纤截面接LED光源，皮层可侧发光，且发光效果优于实施例2中所述纤维，将此纤维与常用的纺织纤维经针织或机织等工艺，可以获得发光效果更好的织物。The thickness of the skin layer (33) is 650 nm, the thicknesses of the first polymer material layer and the second polymer material layer are respectively 110 nm, the diameter of the core layer (34) is 600 nm, the cross section of the optical fiber is connected to the LED light source, and the skin layer can emit light from the side, And the luminous effect is better than that of the fiber described in Example 2. By knitting or weaving this fiber with common textile fibers, a fabric with better luminous effect can be obtained.
实施例4Example 4
本例提供一种聚合物光纤，包括芯层(36)、包覆在芯层(36)外表面的皮层(35)，芯层(36)的材料为聚碳酸酯(PC，折射率为1.59，熔融指数为22g/10min)，皮层(35)的材料为改性聚对苯二甲酸乙二酯(改性PET，全光线透过率为89％，折射率为1.47，熔融指数为49g/10min)，其横截面如图5所示。This example provides a polymer optical fiber, comprising a core layer (36), a skin layer (35) covering the outer surface of the core layer (36), and the material of the core layer (36) is polycarbonate (PC, with a refractive index of 1.59). , the melt index is 22g/10min), the material of the skin layer (35) is modified polyethylene terephthalate (modified PET, the total light transmittance is 89%, the refractive index is 1.47, and the melt index is 49g/ 10 min), and its cross-section is shown in Figure 5.
上述的改性聚对苯二甲酸乙二酯通过如下方法制备而得：其由以下重量份的原料组成：聚对苯二甲酸乙二酯100份、苯乙烯和丙烯酸酯的共聚物(NAS)4份、环烯烃聚合物(COP)3份、聚苯乙烯3份；制备方法为：The above-mentioned modified polyethylene terephthalate is prepared by the following method: it is made up of the raw materials of the following parts by weight: 100 parts of polyethylene terephthalate, styrene and acrylate copolymer (NAS) 4 parts, 3 parts of cycloolefin polymer (COP), 3 parts of polystyrene; the preparation method is:
(1)在高速混合机里添加各原料，搅拌20分钟，得预混料；(1) Add each raw material in a high-speed mixer, and stir for 20 minutes to obtain a premix;
(2)将所得预混料置于螺杆挤出机中进行熔融共混(温度参数：一区275～280℃，二区280℃，三区285℃，箱体温度285℃，模头温度285℃)、挤出，冷却，切片，即可得到所述改性聚对苯二甲酸乙二酯。(2) The obtained premix is placed in a screw extruder for melt blending (temperature parameters: 275 to 280°C in the first zone, 280°C in the second zone, 285°C in the third zone, 285°C in the box, and 285°C in the die head. ℃), extrusion, cooling, and slicing to obtain the modified polyethylene terephthalate.
聚合物光纤的制备方法包括如下步骤：The preparation method of polymer optical fiber includes the following steps:
(1)将上述制备的改性PET切片在120℃的真空干燥箱中干燥8小时，将PC切片在120℃的真空干燥箱中干燥8小时，分别得到干燥后的改性PET和PC切片；(1) The modified PET chips prepared above were dried in a vacuum drying oven at 120°C for 8 hours, and the PC chips were dried in a vacuum drying oven at 120°C for 8 hours to obtain respectively dried modified PET and PC chips;
(2)将干燥后的改性PET和PC切片分别加入双螺杆熔融纺丝机的两个螺杆中，PET组分设定螺杆后区温度275℃、前区温度280℃、箱体温度285℃，PC组分设定螺杆后区温度275℃、前区温度280℃、箱体温度285℃，喷丝板温度285℃；(2) The dried modified PET and PC chips are respectively added to the two screws of the twin-screw melt spinning machine, and the temperature of the PET component is set to 275°C in the rear area of the screw, 280°C in the front area, and 285°C in the box. , PC components set the temperature of the rear area of the screw to 275 °C, the temperature of the front area to 280 °C, the temperature of the box to 285 °C, and the temperature of the spinneret to 285 °C;
(3)经过皮层为三角形，芯层为圆形的纺丝模头纺丝成型；(3) through the skin layer is a triangle, the core layer is a circular spinning die spinning molding;
(4)经过水冷池55℃冷却，由牵拉辊牵伸，牵伸比1:3，并由收卷装置收集成卷。(4) After cooling in a water-cooled pool at 55°C, it is drawn by a drawing roller with a draw ratio of 1:3, and collected into a roll by a winding device.
皮层(35)为三角形，芯层(36)为圆形，芯层(36)的厚度为670μm，皮层(35)的最小厚度为80μm，该光纤截面接LED光源，皮层可侧发光，将此纤维与常用的纺织纤维经针织或机织等工艺，可以获得发光织物；且由于该种光纤的皮层截面为三角形，在纤维的三个角上形成了天然的三棱镜，光线在此处发生色散，该种纤维制成的纺织品在阳光下，可形成天然的彩虹色。The skin layer (35) is triangular, the core layer (36) is circular, the thickness of the core layer (36) is 670 μm, and the minimum thickness of the skin layer (35) is 80 μm. Fibers and commonly used textile fibers can be knitted or woven to obtain light-emitting fabrics; and because the cross-section of the cortex of this fiber is triangular, a natural triangular prism is formed at the three corners of the fiber, where the light is dispersed, Textiles made of this fiber can form a natural iridescent color in sunlight.
实施例5Example 5
本例提供一种聚合物光纤，包括芯层(38)、包覆在芯层(38)外表面的皮层(37)，芯层(38)的材料为聚碳酸酯(PC，折射率为1.57，熔融指数为19g/10min)，皮层(37)的材料为改性聚对苯二甲酸乙二酯(改性PET，全光线透过率为90％，折射率为1.46，熔融指数为53g/10min)，其横截面如图6所示。This example provides a polymer optical fiber, comprising a core layer (38), a skin layer (37) covering the outer surface of the core layer (38), and the material of the core layer (38) is polycarbonate (PC, with a refractive index of 1.57). , the melt index is 19g/10min), the material of the skin layer (37) is modified polyethylene terephthalate (modified PET, the total light transmittance is 90%, the refractive index is 1.46, and the melt index is 53g/ 10 min), and its cross-section is shown in Figure 6.
上述的改性聚对苯二甲酸乙二酯通过如下方法制备而得：其由以下重量份的原料组成：聚对苯二甲酸乙二酯100份、苯乙烯和丙烯酸酯的共聚物(NAS)4份、环烯烃聚合物(COP)3份、聚苯乙烯4份；制备方法为：The above-mentioned modified polyethylene terephthalate is prepared by the following method: it is made up of the raw materials of the following parts by weight: 100 parts of polyethylene terephthalate, styrene and acrylate copolymer (NAS) 4 parts, 3 parts of cycloolefin polymer (COP), 4 parts of polystyrene; the preparation method is:
(1)在高速混合机里添加各原料，搅拌20分钟，得预混料；(1) Add each raw material in a high-speed mixer, and stir for 20 minutes to obtain a premix;
(2)将所得预混料置于螺杆挤出机中进行熔融共混(温度参数：一区275～280℃，二区280℃，三区285℃，箱体温度285℃，模头温度285℃)、挤出，冷却，切片，即可得到所述改性聚对苯二甲酸乙二酯。(2) The obtained premix is placed in a screw extruder for melt blending (temperature parameters: 275 to 280°C in the first zone, 280°C in the second zone, 285°C in the third zone, 285°C in the box, and 285°C in the die head. ℃), extrusion, cooling, and slicing to obtain the modified polyethylene terephthalate.
聚合物光纤的制备方法包括如下步骤：The preparation method of polymer optical fiber includes the following steps:
(1)将上述制备的改性PET切片在120℃的真空干燥箱中干燥8小时，将PC切片在105℃的真空干燥箱中干燥8小时，分别得到干燥后的改性PET和PC切片；(1) the modified PET chips prepared above were dried in a vacuum drying oven at 120°C for 8 hours, and the PC chips were dried in a vacuum drying oven at 105°C for 8 hours to obtain respectively dried modified PET and PC chips;
(2)将干燥后的改性PET和PC切片分别加入双螺杆熔融纺丝机的两个螺杆中，PET组分设定螺杆后区温度280℃、前区温度285℃、箱体温度285℃，PC组分设定螺杆后区温度280℃、前区温度285℃、箱体温度288℃，喷丝板温度290℃；(2) Add the dried modified PET and PC chips to the two screws of the twin-screw melt-spinning machine, respectively, and the PET component is set at a temperature of 280°C in the rear area of the screw, 285°C in the front area, and 285°C in the box. , PC components set the temperature of the rear area of the screw to 280°C, the temperature of the front area to 285°C, the temperature of the box to 288°C, and the temperature of the spinneret to 290°C;
(3)经过芯层为五角星形，皮层为圆形的纺丝模头纺丝成型。(3) The core layer is a five-pointed star, and the skin layer is a circular spinning die.
(4)经过水冷池60℃冷却，由牵拉辊牵伸，牵伸比1:2.5，并由收卷装置收集成卷。(4) After cooling in a water-cooled pool at 60°C, it is drawn by a drawing roller with a draw ratio of 1:2.5, and collected into a roll by a winding device.
皮层(37)为圆形，芯层(38)为五角星形，芯层(38)的最大直径为630μm，皮层(37)的最小厚度为100μm，该光纤截面接LED光源，皮层可侧发光，将此纤维与常用的纺织纤维经针织或机织等工艺，可以获得发光织物，且光线在芯层五角星形的五个顶角上聚集，从光线的侧面能看到5条更亮的光线。The skin layer (37) is circular, the core layer (38) is a five-pointed star, the maximum diameter of the core layer (38) is 630 μm, and the minimum thickness of the skin layer (37) is 100 μm. , by knitting or weaving this fiber with common textile fibers, a luminous fabric can be obtained, and the light is concentrated on the five top corners of the five-pointed star of the core layer, and five brighter lines can be seen from the side of the light. light.
实施例6Example 6
本例提供一种聚合物光纤，包括多个并列设置的芯层(40)、包覆在多个并列设置的芯层(40)外表面的皮层(39)，芯层(40)的材料为聚碳酸酯(PC，折射率为1.55，熔融指数为23g/10min)，皮层(39)的材料为透明尼龙(全光线透过率为92％，折射率为1.47，熔融指数为22g/10min)，其横截面如图7所示。This example provides a polymer optical fiber, comprising a plurality of core layers (40) arranged in parallel, a skin layer (39) covering the outer surfaces of the plurality of core layers (40) arranged in parallel, and the material of the core layer (40) is Polycarbonate (PC, refractive index is 1.55, melt index is 23g/10min), and the material of the skin layer (39) is transparent nylon (total light transmittance is 92%, refractive index is 1.47, melt index is 22g/10min) , and its cross section is shown in Figure 7.
聚合物光纤的制备方法包括如下步骤：The preparation method of polymer optical fiber includes the following steps:
(1)将透明尼龙切片在100℃的真空干燥箱中干燥8小时，将PC切片在120℃的真空干燥箱中干燥8小时，分别得到干燥后的透明尼龙和PC切片；(1) drying the transparent nylon slices in a vacuum drying oven at 100°C for 8 hours, and drying the PC slices in a vacuum drying oven at 120°C for 8 hours to obtain dried transparent nylon and PC slices;
(2)将干燥后的透明尼龙和PC切片分别加入双螺杆熔融纺丝机的两个螺杆中，透明尼龙组分设定螺杆后区温度225℃、前区温度230℃、箱体温度230℃，PC组分设定螺杆后区温度275℃、前区温度280℃、箱体温度285℃，喷丝板温度285℃；(2) Add the dried transparent nylon and PC slices to the two screws of the twin-screw melt spinning machine, respectively. The transparent nylon component is set to a temperature of 225°C in the rear area of the screw, a temperature of 230°C in the front area, and a temperature of 230°C in the box. , PC components set the temperature of the rear area of the screw to 275 °C, the temperature of the front area to 280 °C, the temperature of the box to 285 °C, and the temperature of the spinneret to 285 °C;
(3)经过海岛形结构(即多个芯层)的纺丝模头纺丝成型；(3) spinning through the spinning die head of the sea-island structure (ie, multiple core layers);
(4)经过水冷池60℃冷却，由牵拉辊牵伸，牵伸比1:2，并由收卷装置收集成卷。(4) After cooling in a water-cooled pool at 60°C, it is drawn by a drawing roller with a draw ratio of 1:2, and collected into a roll by a winding device.
多个芯层(40)并列分布于皮层(39)内，每个芯层(40)的直径分别为50μm，皮层(39)的外径为800μm，该光纤截面接LED光源，皮层可侧发光，且光的分布较为均一，将此纤维与常用的纺织纤维经针织或机织等工艺，可以获得发光织物。A plurality of core layers (40) are arranged side by side in the skin layer (39), the diameter of each core layer (40) is 50 μm respectively, and the outer diameter of the skin layer (39) is 800 μm, the cross section of the optical fiber is connected to the LED light source, and the skin layer can emit light from the side , and the distribution of light is relatively uniform, and the luminous fabric can be obtained by knitting or weaving this fiber with commonly used textile fibers.
实施例7Example 7
本例提供一种聚合物光纤，如图2所示，包括芯层(32)、包覆在芯层(32)外表面的皮层(31)，芯层(32)的材料为聚碳酸酯(PC，折射率为1.55，熔融指数为19g/10min)，皮层(31)的材料为透明尼龙(透光度为90％，折射率为1.47，熔融指数为22g/10min)，其横截面如图3所示。This example provides a polymer optical fiber, as shown in FIG. 2, comprising a core layer (32), a skin layer (31) covering the outer surface of the core layer (32), and the material of the core layer (32) is polycarbonate (32). PC, the refractive index is 1.55, the melt index is 19g/10min), and the material of the skin layer (31) is transparent nylon (transparency is 90%, the refractive index is 1.47, and the melt index is 22g/10min). Its cross section is shown in the figure 3 shown.
聚合物光纤的制备方法包括如下步骤：The preparation method of polymer optical fiber includes the following steps:
(1)将透明尼龙切片在100℃的真空干燥箱中干燥8小时，将PC切片在120℃的真空干燥箱中干燥8小时，分别得到干燥后的透明尼龙切片和PC切片；(1) drying the transparent nylon slices in a vacuum drying oven at 100°C for 8 hours, and drying the PC slices in a vacuum drying oven at 120°C for 8 hours to obtain the dried transparent nylon slices and PC slices respectively;
(2)将干燥后的透明尼龙切片和PC切片分别加入双螺杆熔融纺丝机的两个螺杆中，透明尼龙组分设定螺杆后区温度225℃、前区温度230℃、箱体温度230℃，PC组分设定螺杆后区温度275℃、前区温度280℃、箱体温度285℃，喷丝板温度285℃；(2) Add the dried transparent nylon slices and PC slices to the two screws of the twin-screw melt spinning machine, respectively. The transparent nylon component is set to the screw rear temperature of 225 ° C, the front temperature of 230 ° C, and the box temperature of 230 ° C. ℃, the PC component set the temperature of the rear area of the screw to 275℃, the temperature of the front area to 280℃, the temperature of the box body to 285℃, and the temperature of the spinneret to 285℃;
(3)经过皮芯结构(核壳结构)的纺丝模头纺丝成型；(3) Spinning through a spinning die with a skin-core structure (core-shell structure);
(4)经过水冷池60℃冷却，由牵拉辊牵伸，牵伸比1:3.5，并由收卷装置收集成卷。(4) After cooling in a water-cooled pool at 60°C, it is drawn by a drawing roller with a draw ratio of 1:3.5, and collected into a roll by a winding device.
该光纤截面接LED光源，皮层(31)可侧发光，芯层(32)的直径为720μm，皮层(31)的厚度为70μm，将此纤维与常用的纺织纤维经针织或机织等工艺，可以获得发光织物。The cross section of the optical fiber is connected to an LED light source, the skin layer (31) can emit light from the side, the diameter of the core layer (32) is 720 μm, and the thickness of the skin layer (31) is 70 μm. Luminous fabrics are available.
对比例1Comparative Example 1
基本同实施例2，其区别仅在于，皮层的材料为市售的常规PET材料，其折射率为1.56，全光线透过率为87％。Basically the same as Example 2, the difference is only that the material of the skin layer is a commercially available conventional PET material, the refractive index is 1.56, and the total light transmittance is 87%.
对比例2Comparative Example 2
市售的聚碳酸酯(PC)/氟树脂光纤。Commercially available polycarbonate (PC)/fluororesin optical fibers.
性能测试Performance Testing
将上述实施例2-7、对比例1所制得的聚合物光纤以及对比例2提供的光纤进行如下一些性能测试，具体结果参见表1。The polymer optical fibers prepared in the above Examples 2-7, Comparative Example 1, and the optical fiber provided in Comparative Example 2 were subjected to some performance tests as follows, and the specific results are shown in Table 1.
表1Table 1
上述的各性能测试标准如下：The above performance test standards are as follows:
断裂伸长、断裂强力：GB/T 14337-2008Elongation at break, breaking strength: GB/T 14337-2008
衰减系数：GB/T 15972.40-2008Attenuation coefficient: GB/T 15972.40-2008
阳离子染色上色率：FZ/T 50020-2013。Cationic dyeing rate: FZ/T 50020-2013.
由上述实施例可知，本发明的聚合物光纤采用特定的材料作为皮层材料，并控制皮层材料与芯层材料的折射率关系，制成后不仅能够兼具极佳的韧性、较低的光损耗，而且价格更低廉，使其尤为适用于装饰用面料这种较短程光传输的发光织物中；同时本发明的聚合物光纤能够采用熔融挤出，纺丝的方法制成，避免了现有技术仅能采用预制件-拉伸法生产效率较低的缺陷，能够实现连续生产，有利于规模性的扩大化。It can be seen from the above examples that the polymer optical fiber of the present invention adopts a specific material as the skin layer material, and controls the refractive index relationship between the skin layer material and the core layer material. , and the price is lower, making it especially suitable for decorative fabrics such as light-emitting fabrics with short-range light transmission; at the same time, the polymer optical fiber of the present invention can be made by melt extrusion and spinning, avoiding the need for existing technology. Only the preform-stretching method can be used for the defect of low production efficiency, which can realize continuous production and is conducive to the expansion of scale.
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围，凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。The above-mentioned embodiments are only to illustrate the technical concept and characteristics of the present invention, and their purpose is to enable those who are familiar with the art to understand the content of the present invention and implement them accordingly, and cannot limit the scope of protection of the present invention with this. Equivalent changes or modifications made in the spirit and spirit should all be included within the protection scope of the present invention.
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