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CN100390332C - Electric device and method for spinning generation and collection - Google Patents

Electric device and method for spinning generation and collection Download PDF

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CN100390332C
CN100390332C CNB2005100869855A CN200510086985A CN100390332C CN 100390332 C CN100390332 C CN 100390332C CN B2005100869855 A CNB2005100869855 A CN B2005100869855A CN 200510086985 A CN200510086985 A CN 200510086985A CN 100390332 C CN100390332 C CN 100390332C
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fibers
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CN1766181A (en
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李路明
潘焕
胡龙
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Tsinghua University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin

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Abstract

一种电纺丝发生和收集的装置及方法,属于一维纳米材料制备领域,本发明所述装置主要包括喷射装置、液体供给装置、高压电源和收集装置四个部分,利用两根或两组正对的分别连接正、负极性高电压的喷嘴作为喷射系统,喷嘴喷出的带相反电荷的纤维在空中互相吸引、相撞、电中和,成为飞行速度急速降低的纺丝束,收集为高度单向排列的纤维。本发明可以在很大的面积上收集连续的高度单向排列的纳米或微米纤维,能制备出均匀混合的双组分或者多组分纤维结构;可以直接在绝缘表面收集纤维。本发明拓展了传统电纺丝方法的概念,扩大了使用灵活性,特别在收集连续高度单向排列纤维方面提供了一种很有效的手段,赋予了电纺丝纤维更广阔的应用前景。

Figure 200510086985

A device and method for generating and collecting electrospinning, belonging to the field of preparation of one-dimensional nanomaterials, the device of the present invention mainly includes four parts: injection device, liquid supply device, high-voltage power supply and collection device, using two or two sets of Positively connected nozzles with positive and negative polarity high voltage are used as the injection system, and the oppositely charged fibers ejected from the nozzles attract, collide, and neutralize each other in the air, and become spinning bundles with rapidly reduced flying speeds, which are collected as Highly unidirectional fibers. The invention can collect continuous and highly unidirectionally arranged nanometer or micrometer fibers in a large area, and can prepare evenly mixed two-component or multi-component fiber structures; the fibers can be directly collected on the insulating surface. The invention expands the concept of the traditional electrospinning method, expands the flexibility of use, especially provides a very effective means for collecting continuous and highly unidirectionally arranged fibers, and endows the electrospun fibers with broader application prospects.

Figure 200510086985

Description

一种电纺丝发生和收集的装置及方法 A device and method for generating and collecting electrospinning

技术领域 technical field

本发明涉及一种电纺丝发生和收集的装置及方法,具体为一种制备和排列连续微/纳米尺度纤维的电纺丝方法和装置,属于一维纳米材料制备领域。The invention relates to a device and method for generating and collecting electrospinning, in particular to an electrospinning method and device for preparing and arranging continuous micro/nano-scale fibers, belonging to the field of one-dimensional nanomaterial preparation.

背景技术 Background technique

电纺丝技术目前引起了越来越多的重视,在过滤材料、伤口敷料、生物组织工程材料、纳米复合材料和传感器等方面获得了广泛的应用,它被认为是一种制备连续微/纳米尺度纤维的理想方法。电纺丝装置一般包括高压电源、液体供给装置、喷射装置和收集装置四个部分。液体供给装置向喷射装置供给高分子聚合物或其它材料的溶液或熔融液体,高压电源向喷嘴提供几百到几万伏的直流电压。在电场力作用下,喷口的液体被拉出形成很细的射流飞向的收集装置,射流在飞行过程中固化、细化,最后成为纳米或微米尺度的纤维。接收装置一般为接地或接负电压的平板电极。由于射流在飞行过程中的高速随机甩动,上面的电纺丝过程获得的是纤维方向随机分布的无纺布,它只能应用于过滤材料和伤口敷料等领域。Electrospinning technology has attracted more and more attention, and has been widely used in filter materials, wound dressings, biological tissue engineering materials, nanocomposites and sensors. It is considered to be a method for preparing continuous micro/nano Ideal way to scale fibers. The electrospinning device generally includes four parts: a high-voltage power supply, a liquid supply device, a spray device and a collection device. The liquid supply device supplies the solution or molten liquid of polymer or other materials to the injection device, and the high-voltage power supply provides a DC voltage of hundreds to tens of thousands of volts to the nozzle. Under the action of the electric field force, the liquid in the nozzle is pulled out to form a very thin jet and flies to the collecting device. The jet solidifies and refines during the flight, and finally becomes nano or micron-scale fibers. The receiving device is generally a flat electrode that is grounded or connected to a negative voltage. Due to the high-speed random swing of the jet during flight, the above electrospinning process obtains non-woven fabrics with randomly distributed fiber directions, which can only be applied to fields such as filter materials and wound dressings.

在纳米增强材料、传感器等很多应用中,需要的是取向性很好的纤维,目前为止主要有以下三种电纺丝纤维排列工艺:1)使用高速旋转的圆筒作为接收装置,当圆筒的旋转速度足够快时,可以获得一定取向程度的纤维排布。但如果速度过高又将会导致纤维被拉断,所以这种收集方法获得的纤维排布远未达到理想效果。2)使用边缘尖锐的薄圆盘作为收集装置,由于圆盘边缘对电场的聚焦作用,当圆盘高速旋转时,纤维被吸引到其边缘并获得很好的单向排列。这种方法的缺点在于纤维只能收集到圆盘边缘很狭小的范围内。3)使用两块导电平板作为接收装置,其间形成几毫米宽的绝缘区域,喷射一段时间后可以在绝缘区域上获得取向很好的纤维。这种方法的缺点是收集范围很小,当绝缘区域的宽度大于1cm后,纤维取向逐渐变差。因为绝大部分纤维喷射到两块导电极板上了,随着纤维层对极板的覆盖,绝缘区域纤维的取向也会变差。In many applications such as nano-reinforced materials and sensors, fibers with good orientation are needed. So far, there are mainly the following three electrospun fiber alignment processes: 1) Use a high-speed rotating cylinder as a receiving device. When the cylinder When the rotation speed is fast enough, the fiber arrangement with a certain degree of orientation can be obtained. However, if the speed is too high, the fibers will be broken, so the fiber arrangement obtained by this collection method is far from ideal. 2) A thin disk with sharp edges is used as a collection device. Due to the focusing effect of the electric field on the edge of the disk, when the disk rotates at high speed, the fibers are attracted to its edge and a good unidirectional arrangement is obtained. The disadvantage of this method is that the fibers can only be collected to a very narrow extent at the edge of the disc. 3) Two conductive flat plates are used as the receiving device, and an insulating area with a width of several millimeters is formed between them, and well-oriented fibers can be obtained on the insulating area after spraying for a period of time. The disadvantage of this method is that the collection range is very small, and when the width of the insulating area is greater than 1 cm, the fiber orientation gradually becomes poor. Because most of the fibers are sprayed onto the two conductive plates, as the fiber layer covers the plates, the orientation of the fibers in the insulating area will also become poor.

发明内容 Contents of the invention

本发明的目的在于提供一种电纺丝发生和收集的装置,包括:The object of the present invention is to provide a kind of electrospinning generation and collection device, comprising:

液体供给装置,其向喷射装置提供工作液体;所述液体供给装置可控制所述喷射装置的流量;供给流量为0.01μl/min~5000μl/min;A liquid supply device, which provides working liquid to the injection device; the liquid supply device can control the flow rate of the injection device; the supply flow rate is 0.01μl/min-5000μl/min;

两个喷射装置,连接所述液体供给装置并接收工作液体,并且分别喷射出带有正、负电荷的纤维;所述喷射装置包括喷嘴;所述喷射装置加载电压可分别调节;所述两个喷射装置喷嘴相对,两个喷射装置之间的距离为2cm~60cm;Two injection devices are connected to the liquid supply device and receive the working liquid, and respectively eject fibers with positive and negative charges; the injection device includes a nozzle; the loading voltage of the injection device can be adjusted separately; the two The nozzles of the spraying devices are opposite, and the distance between the two spraying devices is 2cm to 60cm;

高压电源,分别向两个喷射装置提供正、负极性的加载电压;电压调节范围为2kV~20kV和-2kV~-20kV;High-voltage power supply provides positive and negative loading voltages to the two injection devices respectively; the voltage adjustment range is 2kV~20kV and -2kV~-20kV;

收集装置,其用来收集所述纤维束,以获得所需纤维;所述收集装置位于与两个喷射装置垂直距离为0-500cm的位置;控制收集装置的表面速度,以获得不同取向程度的纤维结构。Collecting device, it is used for collecting described fiber bundle, obtains desired fiber; Said collecting device is positioned at the position that is 0-500cm perpendicular distance with two injection devices; Controls the surface speed of collecting device, obtains the different degree of orientation Fibrous structure.

其中,液体供给装置为注射泵或气压控制系统;每个喷射装置分别具有1个或多个喷嘴,喷嘴为玻璃毛细管或金属针头;为了聚焦电场,喷嘴上可以固定有薄平板电极,收集装置为旋转装置或皮带传动装置,收集装置的表面采用导电或绝缘材料。Among them, the liquid supply device is a syringe pump or an air pressure control system; each injection device has one or more nozzles, and the nozzles are glass capillaries or metal needles; in order to focus the electric field, thin flat electrodes can be fixed on the nozzles, and the collection device is Rotary device or belt drive, the surface of the collection device is made of conductive or insulating material.

此外,本发明目的还在于提供一种电纺丝发生和收集的方法,该方法包括如下步骤:In addition, the object of the present invention is also to provide a method for generating and collecting electrospinning, which method includes the following steps:

1)将电纺丝的工作溶液装入液体供给装置,并将其与两个喷射装置相连;1) Fill the electrospinning working solution into the liquid supply device and connect it with the two injection devices;

2)调节两个喷射装置的供给流量为0.1μl/min~50μl/min;2) Adjust the supply flow rate of the two injection devices to 0.1μl/min~50μl/min;

3)调整使两种喷射装置相对,并调节它们相互之间的距离为2cm~60cm;3) Adjust to make the two injection devices face each other, and adjust the distance between them to be 2cm to 60cm;

4)调节收集装置的位置,使其与两个喷嘴的垂直距离为0~500cm;4) Adjust the position of the collecting device so that the vertical distance from the two nozzles is 0-500cm;

5)调节收集装置的表面速度0.01m/s~50m/s;5) Adjust the surface velocity of the collecting device to 0.01m/s~50m/s;

6)分别调节两个喷射装置的加载电压为2kV~20kV和-2kV~-20kV;喷射装置分别喷射出带有正、负电荷的纤维,所述纤维在空中相遇并吸附在一起形成速度急剧降低的纤维束;使用气流或绝缘棒牵引所述纤维束到收集装置表面,开始收集。6) Adjust the loading voltage of the two injection devices to 2kV~20kV and -2kV~-20kV respectively; the injection devices eject fibers with positive and negative charges respectively, and the fibers meet in the air and are adsorbed together to form a sharp decrease in speed fiber bundles; using air flow or insulating rods to draw the fiber bundles to the surface of the collection device to start collection.

本发明还包括如下特征:1)当收集装置位于两个喷嘴中间时,能在直径较小的导电或者绝缘材料表面收集均匀的纤维材料。2)当收集装置距离喷嘴一定垂直距离时,能在各种大小的导电或者绝缘装置上收集高度单向排列的纤维。3)对两个喷嘴分别供给不同的高分子聚合物或其它材料溶液或熔融液体,并单独控制流量,能获得均匀混合的双组分纤维结构。4)把上述两个喷嘴扩展为两组喷嘴,每组喷嘴可以包含不同数量的喷嘴并排列成不同的几何结构;能对以上喷嘴供给同种高分子聚合物或其它材料溶液熔融液体,也可以供给不同的液体,从而获得均匀的多组分纤维结构。5)收集装置包括各种形状的运动装置,除了使用圆筒收集,还使用皮带传动装置来进行收集。控制收集装置的表面速度,能获得不同取向程度的纤维结构。The present invention also includes the following features: 1) When the collecting device is located between the two nozzles, uniform fiber materials can be collected on the surface of conductive or insulating materials with smaller diameters. 2) When the collection device is at a certain vertical distance from the nozzle, highly unidirectionally arranged fibers can be collected on conductive or insulating devices of various sizes. 3) Different high molecular polymer or other material solutions or molten liquids are supplied to the two nozzles respectively, and the flow rate is controlled separately, so that a uniformly mixed bicomponent fiber structure can be obtained. 4) Expand the above two nozzles into two groups of nozzles, each group of nozzles can contain different numbers of nozzles and be arranged in different geometric structures; the above nozzles can be supplied with the same polymer or other material solution molten liquid, or Different liquids are supplied to obtain a homogeneous multicomponent fiber structure. 5) The collecting device includes moving devices of various shapes. In addition to using a cylinder for collecting, a belt transmission device is also used for collecting. By controlling the surface velocity of the collecting device, fiber structures with different degrees of orientation can be obtained.

上面所述的电纺丝发生和收集的方法及装置适用于传统的电纺丝方法和装置所使用的各种高分子聚合物或其它材料溶液和熔融液体。The method and device for generating and collecting electrospinning described above are applicable to various polymer or other material solutions and molten liquids used in traditional electrospinning methods and devices.

本发明的有益效果是:使用该方法和装置可以在很大的面积上收集连续的高度单向排列的纳米或微米纤维,能制备出均匀混合的双组分或者多组分纤维结构;还可以直接在绝缘表面收集纤维,而传统方法需要收集装置导电并接地或接负电。本发明所述方法和装置,拓展了传统电纺丝方法的概念,扩大了使用灵活性,特别在收集连续高度单向排列纤维方面提供了一种很有效的手段,赋予了电纺丝纤维更广阔的应用前景。The beneficial effects of the present invention are: the method and device can be used to collect continuous highly unidirectionally arranged nanometer or micrometer fibers on a large area, and can prepare a uniformly mixed bicomponent or multicomponent fiber structure; Fibers are collected directly on insulating surfaces, whereas conventional methods require collection devices to be conductive and grounded or negatively charged. The method and device of the present invention expand the concept of the traditional electrospinning method, expand the flexibility of use, especially provide a very effective means for collecting continuous and highly unidirectionally arranged fibers, and endow the electrospun fibers with more Broad application prospects.

附图说明 Description of drawings

图1是本发明的装置示意图。Figure 1 is a schematic diagram of the device of the present invention.

图2是喷射装置的喷嘴排列的四个例子。Figure 2 shows four examples of nozzle arrangements of the spraying device.

图3是接收装置放置于喷嘴中间时的喷射示意图。Figure 3 is a schematic diagram of spraying when the receiving device is placed in the middle of the nozzle.

图4是使用皮带传动装置作为接收装置的示意图。Figure 4 is a schematic diagram of using a belt drive as a receiving device.

图5是用本发明所述方法和装置收集的高度单向排列纤维的扫描电镜图。Figure 5 is a scanning electron micrograph of highly unidirectionally aligned fibers collected using the method and apparatus of the present invention.

具体实施方式 Detailed ways

下面结合附图对本发明进行说明。The present invention will be described below in conjunction with the accompanying drawings.

图1是本发明的装置示意图,其中1和2为分别连接正、负电源的喷射喷嘴,3和4分别为喷嘴1和喷嘴2喷射出的纤维,5是纤维3和4相互吸引,聚集在一起形成的纤维束,6是收集装置,7是最后收集得到的高度单方向性的纳米纤维。喷嘴1和2组成喷射装置,位置可以单独调节。通过液体供给装置向它们供给上述同一种工作液体,也可以分别供给不同的工作液体。从喷嘴1和2喷出的分别带有正、负电荷的纤维3和4在空中相遇并吸附在一起形成速度急剧降低的纤维束,将该纤维束牵引到高速转动的收集装置6上,就可以把它拉伸成更细的纤维束5,此后可以在收集装置6上收集到连续的高度单向排列的纤维7。上述拉伸过程提供了纺丝取向排列的机械动力,收集装置的表面速度越大,获得的纤维单向性越好。但为了防止收集过程中纤维断裂,收集装置表面速度一般不大于50m/s。Fig. 1 is a schematic view of the device of the present invention, wherein 1 and 2 are spray nozzles connected to positive and negative power supplies respectively, 3 and 4 are respectively the fibers ejected from nozzle 1 and nozzle 2, and 5 is that fibers 3 and 4 attract each other and gather in The fiber bundles formed together, 6 is the collection device, 7 is the highly unidirectional nanofibers collected at last. Nozzles 1 and 2 form the injection unit, the positions of which can be adjusted individually. The above-mentioned same working fluid may be supplied to them by the liquid supply device, or different working fluids may be supplied respectively. The positively and negatively charged fibers 3 and 4 ejected from the nozzles 1 and 2 meet in the air and are adsorbed together to form a fiber bundle with a sharply reduced speed. The fiber bundle is drawn to the high-speed rotating collecting device 6, just It can be drawn into finer fiber bundles 5, after which a continuous highly unidirectional fiber 7 can be collected on a collecting device 6. The above-mentioned drawing process provides the mechanical power for the alignment of the spinning orientation, and the higher the surface speed of the collecting device, the better the unidirectionality of the obtained fibers. However, in order to prevent fiber breakage during the collection process, the surface speed of the collection device is generally not greater than 50m/s.

本发明所述装置主要包括喷射装置、液体供给装置、高压电源和收集装置四个部分。The device of the present invention mainly includes four parts: spraying device, liquid supply device, high-voltage power supply and collecting device.

1)高压电源1) High voltage power supply

使用两套直流高压电源,电源的输出电压分别为正、负2kV~20kV。它们分别与两个喷射装置连接并提供高电压,两个喷嘴上的加载电压可以分别调节。Two sets of DC high-voltage power supplies are used, and the output voltages of the power supplies are positive and negative 2kV to 20kV respectively. They are respectively connected with two injection devices and provide high voltage, and the loading voltage on the two nozzles can be adjusted separately.

2)液体供给装置2) Liquid supply device

液体供给装置使用注射泵,还可以使用气压控制系统。可以控制每个喷嘴的流量为0.01μl/min~5000μl/min。The liquid supply unit uses a syringe pump, and an air pressure control system can also be used. The flow rate of each nozzle can be controlled from 0.01μl/min to 5000μl/min.

3)喷射装置3) Injection device

图2是喷射装置的喷嘴排列的四个例子。喷射装置可以使用玻璃毛细管,也可以使用医用注射器针头,内径为10μm-5mm。两个喷嘴的内径可以相同,也可以不同。为了聚集电场,还可以在喷嘴上固定“刀片状”薄平板电极8、9,如图2(a)所示,平板电极与喷嘴同时与高压电源连接。还可以把两个喷嘴都旋转一个角度,如图2(b)所示,这种结构可以使中和后的纤维束很容易被牵引出来。Figure 2 shows four examples of nozzle arrangements of the spraying device. The injection device can use a glass capillary or a medical syringe needle with an inner diameter of 10 μm-5 mm. The inner diameters of the two nozzles can be the same or different. In order to gather the electric field, "blade-shaped" thin plate electrodes 8 and 9 can also be fixed on the nozzle, as shown in Figure 2(a), the plate electrode and the nozzle are connected to a high-voltage power supply at the same time. The two nozzles can also be rotated at an angle, as shown in Figure 2(b), this structure can make the neutralized fiber bundles easily pulled out.

可以把上述带正、负高电压的两根喷嘴用两组喷嘴阵列来代替,它们分别连接正、负性直流高电压。两组喷嘴相对放置,保证它们喷射的纺丝能够相遇并相互吸附。每组喷嘴可以包含不同数量的喷嘴,并能排列成不同的几何形状和空间结构。图2(c)、(d)是每组包括两个喷嘴的喷射装置的两个排列例子。The above two nozzles with positive and negative high voltages can be replaced by two sets of nozzle arrays, which are respectively connected with positive and negative DC high voltages. The two groups of nozzles are placed opposite to each other to ensure that the spinning fibers they spray can meet and adsorb each other. Each group of nozzles can contain different numbers of nozzles and can be arranged in different geometric shapes and spatial structures. Fig. 2(c), (d) are two arrangement examples of spraying devices including two nozzles in each group.

在多喷嘴的情况下,可以对所有的喷嘴供给同种高工作液体,也可以分组供给不同的液体,还可以对每个喷嘴单独供给不同液体。此外,可以控制每个喷嘴使用相同的流量或者不同的流量。用这种方法可以获得混合均匀的多组分纤维制品。In the case of multiple nozzles, the same high-level working fluid may be supplied to all the nozzles, different fluids may be supplied in groups, or different fluids may be individually supplied to each nozzle. In addition, each nozzle can be controlled to use the same flow rate or a different flow rate. In this way, homogeneously mixed multicomponent fiber products can be obtained.

4)收集装置4) Collection device

图1所示为高速旋转的圆筒距离两喷嘴一定距离进行收集,还可以将较小的圆筒放置于喷嘴之间进行收集,如图3是接收装置放置于喷嘴中间时的喷射示意图。这种方式收集的纤维排列同传统旋转圆筒的方法差不多,不同之处在于这种方法可以直接在绝缘圆筒上收集纺丝,传统方法需要圆筒导电并需要接负电或者接地。此外,由于本方法的收集过程中,对收集装置的放置位置和角度没有特别限制,可位于与两个喷嘴垂直距离为几毫米到几百厘米的任意位置。收集装置的尺寸也没有限制,使用直径很大的圆筒收集,可以在很大的面积上获得纤维排列,这是目前的很多纤维排列方法所不能实现的。为了使收集到的纤维沿收集圆筒轴向均匀分布,可以使圆筒或者喷嘴沿着圆筒轴向缓慢往复运动。收集装置可以是各种形状的运动装置,除了圆筒,还可以使用图4所示的皮带传动装置作为收集装置。Figure 1 shows that the high-speed rotating cylinder is collected at a certain distance from the two nozzles, and a smaller cylinder can also be placed between the nozzles for collection. Figure 3 is a schematic diagram of the spraying when the receiving device is placed in the middle of the nozzles. The arrangement of fibers collected in this way is similar to that of the traditional rotating cylinder method. The difference is that this method can directly collect and spin on the insulating cylinder. The traditional method requires the cylinder to be conductive and needs to be connected to negative electricity or grounded. In addition, during the collection process of this method, there are no special restrictions on the location and angle of the collection device, and it can be located at any position with a vertical distance from several millimeters to hundreds of centimeters from the two nozzles. There is no limit to the size of the collection device. Using a cylinder with a large diameter to collect can obtain fiber arrangement on a large area, which cannot be achieved by many current fiber arrangement methods. In order to distribute the collected fibers evenly along the axial direction of the collecting cylinder, the cylinder or the nozzle can be slowly reciprocated along the axial direction of the cylinder. The collection device can be a moving device of various shapes, except the cylinder, the belt drive shown in Figure 4 can also be used as the collection device.

本发明提供一种电纺丝发生和收集的新方法和装置,能制备连续的高度单向排布的微纳米纤维。其中,使用两个或两组相对的分别连接正、负极性高电压的喷嘴1和2作为喷射系统,喷嘴喷出的带相反电荷的纤维在空中互相吸引、相撞、电中和,成为飞行速度急剧降低的纤维束,从而提供了一种新的电纺丝发生和收集方法,其步骤如下:The invention provides a new method and device for generating and collecting electrospinning, which can prepare continuous highly unidirectionally arranged micro-nano fibers. Among them, two or two sets of opposite nozzles 1 and 2 respectively connected to positive and negative high voltages are used as the injection system, and the oppositely charged fibers ejected from the nozzles attract, collide and electrically neutralize each other in the air, forming a flying Fiber bundles with dramatically reduced velocity, thus providing a new method of electrospinning generation and collection with the following steps:

1)将电纺丝的工作溶液装入液体供给装置,并将其与两个喷射装置相连;1) Fill the electrospinning working solution into the liquid supply device and connect it with the two injection devices;

2)调节两个喷射装置的供给流量为0.1μl/min~50μl/min;2) Adjust the supply flow rate of the two injection devices to 0.1μl/min~50μl/min;

3)调整使两种喷射装置相对,并调节它们相互之间的距离为2cm-60cm;3) Adjust to make the two injection devices face each other, and adjust the distance between them to be 2cm-60cm;

4)调节收集装置的位置,使其与两个喷嘴的垂直距离为0~500cm;4) Adjust the position of the collecting device so that the vertical distance from the two nozzles is 0-500cm;

5)调节收集装置的表面速度0.01m/s~50m/s5) Adjust the surface speed of the collecting device to 0.01m/s~50m/s

6)分别调节两个喷射装置的加载电压为2kV~20kV和-2kV~-20kV;喷射装置分别喷射出带有正、负电荷的纤维,所述纤维在空中相遇并吸附在一起形成速度急剧降低的纤维束;使用气流或绝缘棒牵引所述纤维束到收集装置表面,开始收集。6) Adjust the loading voltage of the two injection devices to 2kV~20kV and -2kV~-20kV respectively; the injection devices eject fibers with positive and negative charges respectively, and the fibers meet in the air and are adsorbed together to form a sharp decrease in speed fiber bundles; using air flow or insulating rods to draw the fiber bundles to the surface of the collection device to start collection.

上面所述的电纺丝发生和收集的方法及装置适用于传统的电纺丝装置所使用的各种高分子聚合物或其它材料溶液和熔融液体。The method and device for generating and collecting electrospinning described above are applicable to various high molecular polymer or other material solutions and molten liquids used in traditional electrospinning devices.

图5是用本发明所述方法和装置收集到的高度单向排列纤维的扫描电镜图,其中纤维材料为PVA,直径约为320纳米。Fig. 5 is a scanning electron micrograph of highly unidirectionally aligned fibers collected by the method and device of the present invention, wherein the fiber material is PVA with a diameter of about 320 nanometers.

下面通过例子对本发明进行说明。The present invention is illustrated below by way of examples.

例1:example 1:

1.以质量百分数为7%的PVA水溶液为工作液体,将其装入气压供液装置并与两根喷嘴相连;1. Use the PVA aqueous solution with a mass percentage of 7% as the working liquid, put it into the air pressure liquid supply device and connect it with two nozzles;

2.调节两根喷嘴的供给流量均为0.1μl/min;2. Adjust the supply flow rate of the two nozzles to 0.1μl/min;

3.使两根喷嘴正对,调节它们之间的距离为30cm;3. Make the two nozzles face each other, and adjust the distance between them to 30cm;

4.使用直径为6mm的聚四氟乙烯管作为收集装置,调节其与两根喷嘴垂直距离为5cm。4. Use a polytetrafluoroethylene tube with a diameter of 6mm as the collection device, and adjust the vertical distance between it and the two nozzles to be 5cm.

5.调节圆筒的转速为3000rpm;5. Adjust the rotating speed of the cylinder to 3000rpm;

6.开启正、负高压电源,分别调节电压为7kV和-7kV。使用绝缘棒将喷射出的纤维束牵引到聚四氟乙烯管表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 7kV and -7kV respectively. Use an insulating rod to draw the ejected fiber bundle to the surface of the Teflon tube and start collecting and spinning.

例2:Example 2:

1.以质量百分数为10%的PVA水溶液为工作液体,将其装入双通道注射泵中并与两根喷嘴相连;1. Take 10% PVA aqueous solution as the working liquid, put it into a dual-channel syringe pump and connect it with two nozzles;

2.调节两根喷嘴的供给流量均为3μl/min;2. Adjust the supply flow rate of the two nozzles to be 3μl/min;

3.使两根喷嘴正对,调节它们之间的距离为2cm;3. Make the two nozzles face each other, and adjust the distance between them to 2cm;

4.使用直径为40mm的金属圆筒作为收集装置,调节其与两根喷嘴垂直距离为15cm。4. Use a metal cylinder with a diameter of 40mm as the collection device, and adjust the vertical distance between it and the two nozzles to be 15cm.

5.调节圆筒的转速为1000rpm;5. Adjust the rotation speed of the cylinder to 1000rpm;

6.开启正、负高压电源,分别调节电压为2kV和-2kV。使用绝缘棒将喷射出的纤维束牵引到金属圆筒表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 2kV and -2kV respectively. The ejected fiber bundles are drawn to the surface of the metal cylinder using insulating rods to start collecting and spinning.

例3:Example 3:

1.以质量百分数为10%的PVA水溶液为工作液体,将其装入双通道注射泵中并与两根喷嘴连通;1. Use 10% PVA aqueous solution as the working liquid, put it into a dual-channel syringe pump and communicate with two nozzles;

2.调节正、负极喷嘴的流量分别为2μl/min和7μl/min;2. Adjust the flow rates of the positive and negative nozzles to 2μl/min and 7μl/min respectively;

3.使两根喷嘴正对,调节它们之间的距离为20cm;3. Make the two nozzles face each other, and adjust the distance between them to 20cm;

4.使用直径为40mm的金属圆筒作为收集装置,调节其与两根喷嘴垂直距离为20cm。4. Use a metal cylinder with a diameter of 40mm as the collection device, and adjust the vertical distance between it and the two nozzles to be 20cm.

5.调节圆筒的转速为1000rpm;5. Adjust the rotation speed of the cylinder to 1000rpm;

6.开启正、负高压电源,分别调节电压为7kV和-7kV。使用气流控制的方法将喷射出的纤维束牵引到金属圆筒表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 7kV and -7kV respectively. The ejected fiber bundle is drawn to the surface of the metal cylinder by means of airflow control, and the collection and spinning are started.

例4:Example 4:

1.以质量百分数为8%的PVA水溶液为工作液体,将其装入气压供液装置并与两根喷嘴连通;1. Use 8% PVA aqueous solution as the working liquid, put it into the pneumatic liquid supply device and communicate with the two nozzles;

2.调节两根喷嘴的供给流量均为50μl/min;2. Adjust the supply flow rate of the two nozzles to 50μl/min;

3.使两根喷嘴正对,在喷嘴上固定正对的平板电极,调节它们之间的距离为60cm;3. Make the two nozzles face each other, fix the face plate electrodes on the nozzles, and adjust the distance between them to 60cm;

4.使用直径为8mm的聚四氟乙烯管作为收集装置,放置于两根喷嘴中间。4. Use a polytetrafluoroethylene tube with a diameter of 8mm as a collection device and place it between the two nozzles.

5.调节聚四氟乙烯管的转速为4000rpm;5. Adjust the rotation speed of the PTFE tube to 4000rpm;

6.开启正、负高压电源,分别调节电压为20kV和-20kV,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, adjust the voltage to 20kV and -20kV respectively, and start collecting and spinning.

例5:Example 5:

1.以质量百分数为16%的PS的氯仿溶液为工作液体,将其装入气压供液装置与两根喷嘴连通;1. Use the chloroform solution of PS with a mass percentage of 16% as the working liquid, put it into the air pressure liquid supply device and communicate with the two nozzles;

2.调节两根喷嘴的供给流量均为5μl/min;2. Adjust the supply flow rate of the two nozzles to 5μl/min;

3.使两根喷嘴正对,调节它们之间的距离为30cm;3. Make the two nozzles face each other, and adjust the distance between them to 30cm;

4.使用皮带传动装置收集纤维,调节其与两根喷嘴垂直距离为10cm。4. Use the belt drive to collect the fiber, and adjust the vertical distance between it and the two nozzles to be 10cm.

5.调节皮带传动装置的表面速度为2m/s;5. Adjust the surface speed of the belt drive to 2m/s;

6.开启正、负高压电源,分别调节电压为9kV和-9kV。使用绝缘棒将喷射出的纤维束牵引到皮带传动装置表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 9kV and -9kV respectively. Insulation rods are used to draw the ejected fiber bundles to the surface of the belt drive to start the collection spinning.

例6:Example 6:

1.以质量百分数为10%的PEO水溶液为工作液体,将其装入气压供液装置并与两根喷嘴连通;1. Use 10% PEO aqueous solution as the working liquid, put it into the pneumatic liquid supply device and communicate with the two nozzles;

2.分别调节正负极喷嘴的流量为3μl/min和6μl/min;2. Adjust the flow rate of the positive and negative nozzles to 3μl/min and 6μl/min respectively;

3.使两根喷嘴正对,调节它们之间的距离为30cm;3. Make the two nozzles face each other, and adjust the distance between them to 30cm;

4.使用皮带传动装置收集纤维,调节其与两根喷嘴垂直距离为10cm。4. Use the belt drive to collect the fiber, and adjust the vertical distance between it and the two nozzles to be 10cm.

5.调节皮带传动装置的表面速度为1.5m/s;5. Adjust the surface speed of the belt drive to 1.5m/s;

6.开启正、负高压电源,分别调节电压为10kV和-13kV。使用绝缘棒将喷射出的纤维束牵引到皮带传动装置表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 10kV and -13kV respectively. Insulation rods are used to draw the ejected fiber bundles to the surface of the belt drive to start the collection spinning.

例7:Example 7:

1.配制质量百分数为7%和10%的PVA水溶液,将溶液加入双通道注射泵中,正极喷嘴供给7%PVA水溶液,负极喷嘴供给10%PVA水溶液;1. Prepare PVA aqueous solutions with mass percentages of 7% and 10%, add the solutions to a dual-channel syringe pump, supply 7% PVA aqueous solution to the positive nozzle, and supply 10% PVA aqueous solution to the negative nozzle;

2.分别调节正、负极喷嘴的供给流量为10μl/min和4μl/min;2. Adjust the supply flow of positive and negative nozzles to 10μl/min and 4μl/min respectively;

3.使两根喷嘴正对,调节它们之间的距离为30cm;3. Make the two nozzles face each other, and adjust the distance between them to 30cm;

4.使用直径为40mm的金属圆筒作为收集装置,调节其与两根喷嘴垂直距离为15cm。4. Use a metal cylinder with a diameter of 40mm as the collection device, and adjust the vertical distance between it and the two nozzles to be 15cm.

5.调节圆筒的转速为800rpm;5. Adjust the rotating speed of the cylinder to 800rpm;

6.开启正、负高压电源,分别调节电压为11kV和-11kV。使用绝缘棒牵引喷射出的纤维束到金属圆筒表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 11kV and -11kV respectively. Use an insulating rod to draw the ejected fiber bundles to the surface of the metal cylinder, and start collecting and spinning.

例8:Example 8:

1.配制PVDF质量百分数为20%的DMAc溶液和PVC质量百分数为25%的DMAc溶液,将溶液加入双通道注射泵中,并分别与正、负极喷嘴连接;1. Prepare a DMAc solution with a PVDF mass percentage of 20% and a PVC mass percentage of 25% DMAc solution, add the solutions to a dual-channel syringe pump, and connect them to the positive and negative nozzles respectively;

2.分别调节正、负极喷嘴的流量为12μl/min和15μl/min;2. Adjust the flow rates of positive and negative nozzles to 12μl/min and 15μl/min respectively;

3.使两根喷嘴正对,调节它们之间的距离为30cm;3. Make the two nozzles face each other, and adjust the distance between them to 30cm;

4.使用直径为30mm的金属圆筒作为收集装置,调节其与两根喷嘴垂直距离为20cm。4. Use a metal cylinder with a diameter of 30mm as the collection device, and adjust the vertical distance between it and the two nozzles to be 20cm.

5.调节圆筒的转速为800rpm;5. Adjust the rotating speed of the cylinder to 800rpm;

6.开启正、负高压电源,分别调节电压为15kV和-15kV。使用气流控制的方法牵引喷射出的纤维束到金属圆筒表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 15kV and -15kV respectively. Use the method of airflow control to draw the jetted fiber bundle to the surface of the metal cylinder, and start to collect and spin.

例9:Example 9:

1.配制PVDF质量百分数为20%的DMAc溶液和PVC质量百分数为25%的DMAc溶液,将溶液加入双通道注射泵中,并分别与正、负极喷嘴连接;1. Prepare a DMAc solution with a PVDF mass percentage of 20% and a PVC mass percentage of 25% DMAc solution, add the solutions to a dual-channel syringe pump, and connect them to the positive and negative nozzles respectively;

2.分别调节正、负极喷嘴的流量为10μl/min和12μl/min;2. Adjust the flow rate of positive and negative nozzles to 10μl/min and 12μl/min respectively;

3.使两根喷嘴正对,调节它们之间的距离为30cm;3. Make the two nozzles face each other, and adjust the distance between them to 30cm;

4.使用直径为8mm的聚四氟乙烯管作为收集装置,调节其与两根喷嘴垂直距离为20cm。4. Use a polytetrafluoroethylene tube with a diameter of 8mm as the collection device, and adjust the vertical distance between it and the two nozzles to be 20cm.

5.调节聚四氟乙烯管的转速为3000rpm;5. Adjust the rotation speed of the PTFE tube to 3000rpm;

6.开启正、负高压电源,分别调节电压为12kV和-12kV。使用绝缘棒将喷射出的纤维束牵引到聚四氟乙烯管表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 12kV and -12kV respectively. Use an insulating rod to draw the ejected fiber bundle to the surface of the Teflon tube and start collecting and spinning.

例10:Example 10:

1.配制PVDF质量百分数为20%的DMAc溶液和PVC质量百分数为25%的DMAc溶液,将溶液加入双通道注射泵中,并分别与正、负极喷嘴连接;1. Prepare a DMAc solution with a PVDF mass percentage of 20% and a PVC mass percentage of 25% DMAc solution, add the solutions to a dual-channel syringe pump, and connect them to the positive and negative nozzles respectively;

2.分别调节正、负极喷嘴的流量为15μl/min和8μl/min;2. Adjust the flow rate of positive and negative nozzles to 15μl/min and 8μl/min respectively;

3.使两根喷嘴正对,调节它们之间的距离为35cm;3. Make the two nozzles face each other, and adjust the distance between them to 35cm;

4.用皮带传动装置收集纤维,调节其与两根喷嘴垂直距离为20cm。4. Use a belt drive to collect fibers, and adjust the vertical distance between them and the two nozzles to be 20cm.

5.调节皮带传动装置的表面速度为3m/s;5. Adjust the surface speed of the belt drive to 3m/s;

6.开启正、负高压电源,分别调节电压为15kV和-15kV。使用气流控制的方法将喷射出的纤维束牵引到皮带传动装置表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 15kV and -15kV respectively. The jetted fiber bundles are drawn to the surface of the belt drive by means of airflow control, and the spinning begins.

例11:Example 11:

1.配制质量比为2∶1的PVDF和PVC的质量百分数为20%的DMAc溶液,将溶液加入气压供液装置中并与两根喷嘴连接;1. Prepare a 20% DMAc solution with a mass percentage of 2:1 PVDF and PVC, add the solution to the air pressure liquid supply device and connect it with two nozzles;

2.调节两根喷嘴的流量均为13μl/min;2. Adjust the flow rate of the two nozzles to 13μl/min;

3.使两根喷嘴正对,调节它们之间的距离为20cm;3. Make the two nozzles face each other, and adjust the distance between them to 20cm;

4.使用直径为30mm的金属圆筒作为收集装置,调节其与两根喷嘴垂直距离为25cm。4. Use a metal cylinder with a diameter of 30mm as the collection device, and adjust the vertical distance between it and the two nozzles to be 25cm.

5.调节金属圆筒的转速为1200rpm;5. Adjust the speed of the metal cylinder to 1200rpm;

6.开启正、负高压电源,分别调节电压为6kV和-6kV。使用玻璃棒将喷射出的纤维束牵引到金属圆筒表面,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, and adjust the voltages to 6kV and -6kV respectively. A glass rod is used to draw the ejected fiber bundle to the surface of a metal cylinder to start collecting and spinning.

例12:Example 12:

1.配制质量比为1∶3的PVDF和PVC的质量百分数为20%的DMAc溶液,将溶液加入气压供液装置中并与两根喷嘴连接;1. Prepare a DMAc solution with a mass percentage of 1:3 of PVDF and PVC with a mass percentage of 20%, and add the solution to the air pressure liquid supply device and connect it with two nozzles;

2.调节流量均为10μl/min;2. Adjust the flow rate to 10μl/min;

3.使两根喷嘴正对,调节它们之间的距离为35cm;3. Make the two nozzles face each other, and adjust the distance between them to 35cm;

4.使用直径为6mm的聚四氟乙烯管作为收集装置,放置于两根喷嘴中间并调节为同样高度;4. Use a polytetrafluoroethylene tube with a diameter of 6mm as the collection device, place it between the two nozzles and adjust it to the same height;

5.调节聚四氟乙烯管的转速为1500rpm;5. Adjust the rotation speed of the PTFE tube to 1500rpm;

6.开启正、负高压电源,分别调节电压为10kV和-10kV,开始收集纺丝。6. Turn on the positive and negative high-voltage power supplies, adjust the voltage to 10kV and -10kV respectively, and start collecting and spinning.

上述方式只是本发明优选的实施方式,对于本领域内的普通技术人员而言,在本发明公开了使用两种相对的且电压极性相反的喷射装置的基础上,很容易作出各种类型的改进或变形,而不仅限于本发明上述具体实施方式所描述的装置和方法,因此前面描述的方式只是优选地,而并不具有限制性的意义。The above-mentioned method is only a preferred embodiment of the present invention. For those of ordinary skill in the art, on the basis of the present invention disclosing the use of two opposite injection devices with opposite voltage polarities, it is easy to make various types of injection devices. Improvements or modifications are not limited to the devices and methods described in the above specific embodiments of the present invention, so the foregoing descriptions are only preferred rather than limiting.

Claims (8)

1. the electrospinning silk device that takes place and collect is characterized in that: this electrospinning silk takes place and the device collected comprises:
Fluid Supplying apparatus, it provides hydraulic fluid to injection apparatus; Described fluid Supplying apparatus can be controlled the flow of described injection apparatus; Supply flow rate is 0.01 μ l/min~5000 μ l/min;
Two injection apparatus connect described fluid Supplying apparatus and receive hydraulic fluid, and eject the fiber that has positive and negative electric charge respectively; Described injection apparatus comprises nozzle; Described injection apparatus on-load voltage can be regulated respectively; Described two injection apparatus nozzles are relative, and the distance between two injection apparatus is 2cm~60cm;
High voltage source provides the on-load voltage of positive and negative polarity respectively to two injection apparatus; The voltage-regulation scope be 2kV~20kV and-2kV~-20kV;
Gathering-device is used for collecting described fibre bundle, to obtain required fiber; Described gathering-device be positioned at two injection apparatus vertical ranges be 0~500cm position; The superficial velocity of control gathering-device is to obtain the fibre structure of different orientation degree.
2. the device that electrospinning silk as claimed in claim 1 takes place and collects is characterized in that described fluid Supplying apparatus is syringe pump or pneumatic control system.
3. the device that electrospinning silk as claimed in claim 1 takes place and collects is characterized in that each injection apparatus has one or more nozzles respectively.
4. the device that electrospinning silk as claimed in claim 1 takes place and collects is characterized in that described nozzle is capillary glass tube or syringe needle.
5. the device that electrospinning silk as claimed in claim 1 takes place and collects is characterized in that, is fixed with the thin flat plate electrode on the described nozzle.
6. the device that electrospinning silk as claimed in claim 1 takes place and collects is characterized in that described gathering-device is whirligig or belt drive unit.
7. the device that electrospinning silk as claimed in claim 1 takes place and collects is characterized in that, conduction or insulating materials are adopted in the surface of described gathering-device.
8. the electrospinning silk method that takes place and collect, it comprises the steps:
1) working solution of electrospinning silk is packed into fluid Supplying apparatus, and it is linked to each other with two injection apparatus;
2) supply flow rate of two injection apparatus of adjusting is 0.1 μ l/min~50 μ l/min;
3) adjust and to make two kinds of injection apparatus relative, and to regulate their distances each other be 2cm~60cm;
4) regulate the position of gathering-device, making the vertical range of itself and two nozzles is 0~500cm;
5) the superficial velocity 0.01m/s~50m/s of adjusting gathering-device;
6) on-load voltage of regulating two injection apparatus respectively be 2kV~20kV and-2kV~-20kV; Injection apparatus ejects the fiber that has positive and negative electric charge respectively, the described fiber fibre bundle that formation speed sharply reduces that aloft meets and be attached together; Use air-flow or insulating bar to draw described fibre bundle, begin to collect spinning to the gathering-device surface.
CNB2005100869855A 2005-11-25 2005-11-25 Electric device and method for spinning generation and collection Expired - Fee Related CN100390332C (en)

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