CN116371084A - A kind of degradable spun-bonded filter material and preparation method thereof - Google Patents
A kind of degradable spun-bonded filter material and preparation method thereof Download PDFInfo
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical class O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 82
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 16
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- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0028—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions provided with antibacterial or antifungal means
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Abstract
本发明涉及一种可降解的纺黏过滤材料及其制备方法,属于非织造技术领域。本发明的可降解纺黏过滤材料包括三层纤维直径大小不一的纤维网;纤维网中的纤维为皮芯型复合纤维。本发明通过双螺杆造粒技术得到改性聚己二酸对苯二甲酸丁二醇酯和改性二氧化碳基聚氨酯,再分别与常规PBAT颗粒和二氧化碳基聚氨酯颗粒混合,经过双组分纺黏工艺,得到三层纤维网。将三层纤维网自上而下依次排列,进行热黏合加固,再进行电晕驻极处理,得到可降解的纺黏过滤材料。本发明的可降解纺黏过滤材料不仅具有较好的过滤和抗菌性能,而且均采用可降解材料,避免不可降解物质对环境造成污染,一定程度上保护了环境。
The invention relates to a degradable spunbonded filter material and a preparation method thereof, belonging to the technical field of nonwovens. The degradable spun-bonded filter material of the present invention comprises three layers of fiber nets with different fiber diameters; the fibers in the fiber nets are sheath-core composite fibers. The present invention obtains modified polybutylene adipate terephthalate and modified carbon dioxide-based polyurethane through twin-screw granulation technology, and then mixes them with conventional PBAT particles and carbon dioxide-based polyurethane particles respectively, and undergoes a two-component spun-bonding process. , to obtain a three-layer fiber web. The three-layer fiber net is arranged in sequence from top to bottom, thermally bonded and reinforced, and then subjected to corona electret treatment to obtain a degradable spun-bonded filter material. The degradable spun-bonded filter material of the present invention not only has better filtering and antibacterial properties, but also uses degradable materials to avoid environmental pollution caused by non-degradable substances and protect the environment to a certain extent.
Description
技术领域technical field
本发明属于非织造技术领域,尤其涉及一种可降解的纺黏过滤材料及其制备方法。The invention belongs to the field of non-woven technology, and in particular relates to a degradable spun-bonded filter material and a preparation method thereof.
背景技术Background technique
现有常见的过滤材料及其制备方法:Existing common filter materials and their preparation methods:
现有技术中公开了一种采用静电纺丝与熔喷纺丝相结合的方法制备具有梯度纤维直径的复合无纺布层,同时在熔喷材料中添加抗静电剂、抗菌剂,以及在静电纺丝液中添加抗菌剂,其使用工艺为静电纺丝和熔喷纺丝工艺,但该方法制备所得复合无纺布过滤阻力较高。还有将多层纤维网层叠后,依次经过针刺加固处理、烘焙处理、电晕驻极处理制成多层纺熔驻极过滤材料。但其滤料的纤维为单组分纤维,且采用的材料均为不可降解材料,过度使用不利于环境保护。The prior art discloses a method of combining electrospinning and melt-blown spinning to prepare a composite non-woven fabric layer with gradient fiber diameters, and at the same time add antistatic agents and antibacterial agents to the melt-blown materials, and The antimicrobial agent is added to the spinning liquid, and its application process is electrospinning and melt blown spinning process, but the filtration resistance of the composite nonwoven fabric prepared by this method is relatively high. In addition, after laminating the multi-layer fiber webs, the multi-layer spunmelt electret filter material is made into sequentially through acupuncture reinforcement treatment, baking treatment, and corona electret treatment. However, the fiber of the filter material is a single-component fiber, and the materials used are all non-degradable materials, and excessive use is not conducive to environmental protection.
发明内容Contents of the invention
为解决上述技术问题,本发明提供了一种可降解的纺黏过滤材料及其制备方法。本发明的过滤材料包括三层纤维直径大小不一的纤维网;纤维网中的纤维为皮芯型复合纤维。通过双螺杆造粒技术得到改性PBAT和改性二氧化碳基聚氨酯,再分别与常规PBAT颗粒和二氧化碳基聚氨酯颗粒混合,经过双组分纺黏工艺,得到三层纤维网。将三层纤维直径不一的纤维网自上而下依次排列,进行热黏合加固,再对其进行电晕驻极处理,得到可降解的纺黏过滤材料。本发明所述滤料不仅具有较好的过滤和抗菌性能,而且均采用可降解材料,避免不可降解物质对环境造成污染,一定程度上保护了环境。In order to solve the above technical problems, the present invention provides a degradable spunbonded filter material and a preparation method thereof. The filter material of the invention comprises three layers of fiber nets with different fiber diameters; the fibers in the fiber nets are sheath-core composite fibers. Modified PBAT and modified carbon dioxide-based polyurethane were obtained through twin-screw granulation technology, and then mixed with conventional PBAT particles and carbon dioxide-based polyurethane particles respectively, and a three-layer fiber web was obtained through a two-component spun-bonding process. Three layers of fiber webs with different fiber diameters are arranged sequentially from top to bottom, thermally bonded and reinforced, and then subjected to corona electret treatment to obtain a degradable spunbond filter material. The filter material of the present invention not only has better filtering and antibacterial properties, but also uses degradable materials to avoid environmental pollution caused by non-degradable substances and protect the environment to a certain extent.
本发明是通过以下技术方案实现的:The present invention is achieved through the following technical solutions:
本发明第一个目的是提供一种可降解的纺黏过滤材料,所述纺黏过滤材料从上到下依次包括上层纤维网、中层纤维网和下层纤维网;所述上层纤维网中纤维的直径为16μm~19μm;中层纤维网中纤维的直径为12μm~15μm;所述下层纤维网中纤维的直径为9μm~11μm。The first object of the present invention is to provide a degradable spunbond filter material, which comprises an upper fiber web, a middle fiber web and a lower fiber web from top to bottom; The diameter is 16 μm to 19 μm; the diameter of the fiber in the middle fiber web is 12 μm to 15 μm; the diameter of the fiber in the lower fiber web is 9 μm to 11 μm.
在本发明的一个实施例中,所述上、中、下三层纤维网的克重分别为25g/m2~35g/m2、30g/m2~40g/m2、40g/m2~60g/m2。In one embodiment of the present invention, the weights of the upper, middle and lower layers of fiber webs are respectively 25g/m 2 to 35g/m 2 , 30g/m 2 to 40g/m 2 , 40g/m 2 to 60g/m 2 .
在本发明的一个实施例中,所述纤维为皮芯型复合纤维;所述纤维的皮层为改性二氧化碳基聚氨酯与二氧化碳基聚氨酯的混合物;所述纤维的芯层为改性聚己二酸对苯二甲酸丁二醇酯与聚己二酸对苯二甲酸丁二醇酯的混合物。In one embodiment of the present invention, the fiber is a sheath-core composite fiber; the skin layer of the fiber is a mixture of modified carbon dioxide-based polyurethane and carbon dioxide-based polyurethane; the core layer of the fiber is modified polyadipic acid A mixture of butylene terephthalate and polybutylene adipate terephthalate.
在本发明的一个实施例中,所述改性二氧化碳基聚氨酯通过以下方法制备得到:In one embodiment of the present invention, the modified carbon dioxide-based polyurethane is prepared by the following method:
将抗菌颗粒与二氧化碳基聚氨酯混合,双螺杆挤出机加热熔融,冷却干燥后得到所述改性二氧化碳基聚氨酯;所述抗菌颗粒选自纳米氧化锌。The antibacterial particles are mixed with carbon dioxide-based polyurethane, heated and melted by a twin-screw extruder, and cooled and dried to obtain the modified carbon dioxide-based polyurethane; the antibacterial particles are selected from nanometer zinc oxide.
在本发明的一个实施例中,所述抗菌颗粒与二氧化碳基聚氨酯的质量比为3~4:15~16。In one embodiment of the present invention, the mass ratio of the antibacterial particles to carbon dioxide-based polyurethane is 3-4:15-16.
在本发明的一个实施例中,所述改性聚己二酸对苯二甲酸丁二醇酯通过以下方法制备得到:In one embodiment of the present invention, described modified polybutylene adipate terephthalate is prepared by the following method:
将增能助剂与聚己二酸对苯二甲酸丁二醇酯混合,计量、双螺杆挤出机加热熔融,冷却干燥后得到所述改性聚己二酸对苯二甲酸丁二醇酯;所述增能助剂为硬脂酸钙、硬脂酸镁与氮化硅的混合物;所述硬脂酸钙、硬脂酸镁与氮化硅的质量百分比分别为40%~50%、30%~40%与10%~30%。Mix the energy-enhancing additive with polybutylene adipate terephthalate, measure, heat and melt with a twin-screw extruder, and obtain the modified polybutylene adipate terephthalate after cooling and drying The energizer is a mixture of calcium stearate, magnesium stearate and silicon nitride; the mass percentages of the calcium stearate, magnesium stearate and silicon nitride are respectively 40% to 50%, 30% to 40% and 10% to 30%.
在本发明的一个实施例中,所述增能助剂与聚己二酸对苯二甲酸丁二醇酯的质量比为2~3:7~8。In one embodiment of the present invention, the mass ratio of the energizer to polybutylene adipate terephthalate is 2-3:7-8.
本发明的第二个目的是提供一种可降解的纺黏过滤材料的制备方法,包括以下步骤:Second object of the present invention is to provide a kind of preparation method of degradable spun-bonded filter material, comprising the following steps:
(1)将改性二氧化碳基聚氨酯与二氧化碳基聚氨酯混合,经螺杆挤出机加热熔融、冷却、干燥、切断得到皮层料;将改性聚己二酸对苯二甲酸丁二醇酯与聚己二酸对苯二甲酸丁二醇酯混合,经螺杆挤出机加热熔融、冷却、干燥、切断得到芯层料;(1) Mix modified carbon dioxide-based polyurethane with carbon dioxide-based polyurethane, heat and melt through a screw extruder, cool, dry, and cut off to obtain a skin layer material; modify polybutylene adipate terephthalate and polyhexamethylene Butylene glycol terephthalate is mixed, heated and melted by a screw extruder, cooled, dried, and cut to obtain a core layer material;
(2)将所述步骤(1)所得皮层料与芯层料在纺丝组件中通过喷丝孔挤出,经侧吹风冷却和调节牵伸时气流的初始速度,进而分丝后形成不同直径的纤维,分别铺设到多孔传输带上得到上层纤维网、中层纤维网和下层纤维网;(2) Extrude the cortex material and core layer material obtained in the step (1) through the spinneret holes in the spinning assembly, cool and adjust the initial velocity of the airflow during drafting by side blowing, and then form different diameters after the filaments are separated. The fibers are respectively laid on the porous conveyor belt to obtain the upper fiber web, the middle layer fiber web and the lower layer fiber web;
(3)将步骤(2)所得上层纤维网、中层纤维网和下层纤维网自上而下排列,通过热黏合加固,固结成布,进行电晕驻极,得到所述可降解的纺黏过滤材料。(3) Arrange the upper layer fiber web, the middle layer fiber web and the lower layer fiber web obtained in step (2) from top to bottom, reinforce by thermal bonding, consolidate into a cloth, and perform corona electret to obtain the degradable spunbond filter material.
在本发明的一个实施例中,步骤(2)中,将皮层料加入料斗1,经过螺杆挤出机1加热熔融、过滤器1过滤杂质、计量泵1计量;将芯层料加入料斗2,经过螺杆挤出机2加热熔融、过滤器2过滤杂质、计量泵2计量,二者到达纺丝组件,形成皮芯复合结构的熔体细流,再由侧吹风冷空气冷却、调节气流的初始速度拉伸形成连续长丝后,得到不同直径的纤维,分别随机铺设到多孔传输带上形成上层纤维网、中层纤维网和下层纤维网。In one embodiment of the present invention, in step (2), the skin layer material is added to the
在本发明的一个实施例中,步骤(2)中,所述纺丝组件的纺丝速度为2400/min以上,单丝纤度1.6dtex以下。In one embodiment of the present invention, in step (2), the spinning speed of the spinning assembly is above 2400/min, and the fineness of single filament is below 1.6 dtex.
在本发明的一个实施例中,步骤(2)中,所述侧吹风装置为一种左右两端对称的新型侧吹风装置。所述新型侧吹风装置左右两端对称,每端都包括侧吹风箱,两个侧吹风箱体之间形成冷却纤维的空间。其中,侧吹风箱设置有多层多孔板与L形导流板进行分风导流,每层多孔板孔型为蜂窝形设计进行分风整流。In one embodiment of the present invention, in step (2), the side blowing device is a new type of side blowing device with symmetrical left and right ends. The left and right ends of the novel side blowing device are symmetrical, and each end includes a side blowing box, and a space for cooling fibers is formed between the two side blowing boxes. Among them, the side blowing box is equipped with multi-layer perforated plates and L-shaped deflectors for air distribution and flow diversion, and the hole pattern of each layer of perforated plates is honeycomb-shaped design for air distribution and rectification.
在本发明的一个实施例中,步骤(2)中,所述气流的初始速度为70m/s~80m/s时制备得到直径为16μm~19μm的纤维;所述气流初始速度为90m/s~105m/s时制备得到直径为12μm~15μm的纤维;所述气流初始速度为110m/s~120m/s时制备得到直径为9μm~11μm的纤维。In one embodiment of the present invention, in step (2), fibers with a diameter of 16 μm to 19 μm are prepared when the initial velocity of the airflow is 70 m/s to 80 m/s; the initial velocity of the airflow is 90 m/s to 80 m/s. Fibers with a diameter of 12 μm to 15 μm are prepared at 105 m/s; fibers with a diameter of 9 μm to 11 μm are prepared when the initial air velocity is 110 m/s to 120 m/s.
在本发明的一个实施例中,步骤(2)中,所述分丝是以静电分丝器作为分丝装置;其中,静电电压为26kV,电流为1mA,放电针板与接地辊之间距离为50mm。In one embodiment of the present invention, in step (2), the said splitting device is an electrostatic splitter as the splitting device; wherein, the electrostatic voltage is 26kV, the current is 1mA, and the distance between the discharge needle plate and the ground roller is 50mm.
在本发明的一个实施例中,步骤(2)中,所述牵伸是以整体式宽狭缝牵伸器作为拉伸装置,狭缝宽度为7mm。In one embodiment of the present invention, in step (2), the drafting uses an integral wide slit drafter as the stretching device, and the slit width is 7mm.
在本发明的一个实施例中,步骤(3)中,所述热黏合加固的热轧辊温度为170℃~180℃。In one embodiment of the present invention, in step (3), the temperature of the thermally bonded and reinforced hot roll is 170°C-180°C.
在本发明的一个实施例中,所述电晕驻极的放电针尖的材质为钨;所述针尖的密度为900枚/m2~1000枚/m2。In one embodiment of the present invention, the discharge tip of the corona electret is made of tungsten; the density of the tip is 900 pieces/m 2 -1000 pieces/m 2 .
在本发明的一个实施例中,步骤(3)中,所述电晕驻极的条件:驻极直流电压为7kv~18kv,驻极时间为50s~90s,驻极距离为15cm~20cm,驻极温度为25℃~35℃。In one embodiment of the present invention, in step (3), the conditions of the corona electret: the electret DC voltage is 7kv-18kv, the electret time is 50s-90s, the electret distance is 15cm-20cm, the electret Extreme temperature is 25℃~35℃.
在本发明的一个实施例中,步骤(3)中,将制成的纤维直径不一的上、中、下三层纤维网自上而下依次排列,使用热轧辊进行热黏合加固,固结成布、卷绕成型,最后将其经过导辊、高压电源放电针尖电极、接地金属辊等进行电晕驻极,即得到该可降解的纺黏过滤材料。In one embodiment of the present invention, in step (3), the upper, middle and lower three-layer fiber webs with different fiber diameters are arranged sequentially from top to bottom, and hot rollers are used for thermal bonding and reinforcement. Fabrication, winding and molding, and finally corona electret through guide rollers, high-voltage power supply discharge needle-point electrodes, grounded metal rollers, etc., to obtain the degradable spunbonded filter material.
在本发明的一个实施例中,步骤(3)中,所述热粘合的热轧辊温度为170℃~180℃。In one embodiment of the present invention, in step (3), the temperature of the thermally bonded hot roll is 170°C-180°C.
在本发明的一个实施例中,所述纤维的皮层添加的抗菌颗粒含量为3%~8%。所述皮层组分的二氧化碳基聚氨酯和抗菌颗粒纳米氧化锌能够产生协同作用。具有很强吸水性的二氧化碳基聚氨酯能够促进纳米氧化锌产生更多的氢氧自由基,而高化学活性的氢氧自由基能与有机物反应,杀死绝大多数的病毒和细菌。皮层组分中两种物质的协同作用大大地增强了该滤料的抗菌功能。In one embodiment of the present invention, the content of antibacterial particles added to the skin layer of the fiber is 3%-8%. The carbon dioxide-based polyurethane of the skin layer component and the antibacterial particle nano-zinc oxide can produce a synergistic effect. Carbon dioxide-based polyurethane with strong water absorption can promote nano-zinc oxide to generate more hydroxyl radicals, and highly chemically active hydroxyl radicals can react with organic matter and kill most viruses and bacteria. The synergistic effect of the two substances in the cortex component greatly enhances the antibacterial function of the filter material.
在本发明的一个实施例中,所述纤维的芯层添加的增能助剂含量为5%~10%。所述增能助剂中硬脂酸钙、硬脂酸镁、氮化硅的比例为5:3:2。特殊配比的增能助剂的加入改变了聚合物结晶粒径的大小,形成了无数多个小粒径,增大了粒径的总表面积,使电荷聚集在无数多个小粒径的表面,从而增大了电荷的储存空间,明显提高了该纺黏滤料的过滤效率。In one embodiment of the present invention, the content of the energizing additive added to the core layer of the fiber is 5%-10%. The ratio of calcium stearate, magnesium stearate and silicon nitride in the energizer is 5:3:2. The addition of a special ratio of energy-enhancing additives changes the size of the polymer crystal particle size, forming countless small particle sizes, increasing the total surface area of the particle size, and making the charge gather on the surface of countless small particle sizes , thereby increasing the charge storage space and significantly improving the filtration efficiency of the spunbond filter material.
在本发明的一个实施例中,所述增能助剂占PBAT增能母粒的质量比为20%~30%;所述PBAT增能母粒占芯层原料的质量比为5%~10%。In one embodiment of the present invention, the mass ratio of the energizing agent to the PBAT energizing masterbatch is 20% to 30%; the mass ratio of the PBAT energizing masterbatch to the core layer raw material is 5% to 10% %.
在本发明的一个实施例中,所述抗菌颗粒占改性二氧化碳基聚氨酯母粒的质量比为15%~20%;所述改性二氧化碳基聚氨酯母粒占皮层原料的质量比为3%~8%。In one embodiment of the present invention, the mass ratio of the antibacterial particles to the modified carbon dioxide-based polyurethane masterbatch is 15% to 20%; the mass ratio of the modified carbon dioxide-based polyurethane masterbatch to the cortex raw material is 3% to 3%. 8%.
本发明的技术方案具有以下优点:The technical solution of the present invention has the following advantages:
(1)本发明所述的一种可降解的纺黏过滤材料设置上、中、下三层纤维直径不一的纤维网,逐步过滤颗粒物,大大增强了滤料的过滤功能。(1) The degradable spunbonded filter material of the present invention is provided with three layers of fiber webs with different fiber diameters in the upper, middle and lower layers to gradually filter particulate matter, greatly enhancing the filtering function of the filter material.
(2)本发明所述的一种可降解的纺黏过滤材料采用双组分纺黏工艺,其纤维为皮芯型复合纤维,且皮层纤维的二氧化碳基聚氨酯、芯层纤维的PBAT均为可降解材料,即该滤料为可降解过滤材料,避免不可降解物质对环境造成污染,一定程度上保护了环境。(2) A kind of degradable spunbond filter material of the present invention adopts two-component spunbond technology, and its fiber is sheath-core type composite fiber, and the carbon dioxide base polyurethane of cortex fiber, the PBAT of core layer fiber all can Degradable material, that is, the filter material is a degradable filter material, which avoids non-degradable substances from polluting the environment and protects the environment to a certain extent.
(3)本发明所述的一种可降解的纺黏过滤材料的纤维为皮芯型复合纤维。其中,皮层组分包括二氧化碳基聚氨酯和抗菌颗粒纳米氧化锌,具有很强吸水性的二氧化碳基聚氨酯能够促进纳米氧化锌产生更多的氢氧自由基,而高化学活性的氢氧自由基能与有机物反应,杀死绝大多数的病毒和细菌。皮层组分中两种物质的协同作用大大地增强了该滤料的抗菌功能。其中,芯层组分添加以硬脂酸钙、硬脂酸镁、氮化硅的混合物为主要成分的增能助剂,特殊配比的增能助剂的加入改变了聚合物结晶粒径的大小,形成了无数多个小粒径,增大了粒径的总表面积,使电荷聚集在无数多个小粒径的表面,从而增大了电荷的储存空间,明显提高了该纺黏滤料的过滤效率及稳定性。同时,材料中储存的高密度静电荷可刺激细菌的蛋白质变性,进一步起到抗菌作用,因此增能助剂与抗菌颗粒纳米氧化锌也可以产生协同作用,大大提高了该滤料的抗菌效率。(3) The fibers of the degradable spunbonded filter material of the present invention are sheath-core composite fibers. Among them, the cortex components include carbon dioxide-based polyurethane and antibacterial particle nano-zinc oxide. Carbon dioxide-based polyurethane with strong water absorption can promote nano-zinc oxide to generate more hydroxyl radicals, and highly chemically active hydroxyl radicals can interact with The organic matter reacts, killing most viruses and bacteria. The synergistic effect of the two substances in the cortex component greatly enhances the antibacterial function of the filter material. Among them, the core layer component is added with a mixture of calcium stearate, magnesium stearate, and silicon nitride as the main component of the energy-enhancing additive, and the addition of the special proportion of the energy-enhancing additive changes the particle size of the polymer crystal. Size, forming countless small particle sizes, increasing the total surface area of the particle size, making the charge gather on the surface of countless small particle sizes, thereby increasing the storage space of the charge, and significantly improving the performance of the spunbond filter material. Filtration efficiency and stability. At the same time, the high-density electrostatic charge stored in the material can stimulate the protein denaturation of the bacteria and further play an antibacterial effect. Therefore, the energizing agent and the antibacterial particle nano-zinc oxide can also produce a synergistic effect, which greatly improves the antibacterial efficiency of the filter material.
(4)在该滤料制备的最后,将其经过导辊、高压电源放电针尖电极、接地金属辊等进行电晕驻极,通过所设置的超高电压、超大距离及特殊钨材质的放电针尖,大大提高了该滤料的过滤效率。同时,与抗菌颗粒纳米氧化锌产生协同作用,进一步增强抗菌功能。(4) At the end of the preparation of the filter material, corona electret is carried out through guide rollers, high-voltage power supply discharge needle-tip electrodes, grounded metal rollers, etc., through the set ultra-high voltage, super-large distance and special tungsten discharge needle tip , greatly improving the filtration efficiency of the filter material. At the same time, it has a synergistic effect with antibacterial particle nano zinc oxide to further enhance the antibacterial function.
(5)本发明提供了一种可降解的纺黏过滤材料,其制备原理图如图1所示,本发明的滤料结合双螺杆造粒技术、皮芯型双组分纺黏工艺、热黏合加固技术和电晕驻极技术制成。由双螺杆造粒技术得到PBAT增能母粒、改性二氧化碳基聚氨酯母粒,由皮芯型双组分纺黏工艺得到纤维直径不一的上、中、下三层纤维网,将三层纤维网自上而下依次排列,使用热轧辊进行热黏合加固后,进行电晕驻极,四种工艺缺一不可,共同组合后才可制得该可降解的纺黏过滤材料。(5) The present invention provides a degradable spunbond filter material, the principle diagram of which is shown in Figure 1. The filter material of the present invention combines twin-screw granulation technology, skin-core two-component spunbond process, thermal Adhesive reinforcement technology and corona electret technology. PBAT energized masterbatch and modified carbon dioxide-based polyurethane masterbatch were obtained by twin-screw granulation technology, and upper, middle and lower three-layer fiber webs with different fiber diameters were obtained by skin-core two-component spunbond technology. The fiber webs are arranged in order from top to bottom. After thermal bonding and reinforcement with hot rolls, corona electret is carried out. The four processes are indispensable, and the degradable spunbond filter material can be obtained only after they are combined together.
(6)该滤料的制备过程中采用一种左右两端对称的新型侧吹风装置,使冷风气流均匀一致、温度一致,极大地减少了断丝、并丝现象,提高纺丝的均匀性和稳定性,有利于生产出更高品质、更高质量的纺黏滤料。此外,以静电分丝器作为分丝装置,明显改善该纺黏滤料产品的均匀度;以整体式宽狭缝牵伸器作为拉伸装置,明显改善纺黏长丝的长度、线密度、强度、伸长率等物理机械性能。(6) In the preparation process of the filter material, a new type of side blowing device with symmetrical left and right ends is adopted to make the cold air flow uniform and the temperature consistent, which greatly reduces the phenomenon of broken filaments and parallel filaments, and improves the uniformity and stability of spinning It is conducive to the production of higher quality and higher quality spunbond filter materials. In addition, the electrostatic separator is used as the separating device to significantly improve the uniformity of the spunbonded filter material; the integral wide slit drafter is used as the stretching device to significantly improve the length, linear density, and Physical and mechanical properties such as strength and elongation.
附图说明Description of drawings
为了使本发明的内容更容易被清楚地理解,下面根据本发明的具体实施例并结合附图,对本发明作进一步详细的说明,其中:In order to make the content of the present invention more easily understood, the present invention will be described in further detail below according to specific embodiments of the present invention in conjunction with the accompanying drawings, wherein:
图1是本发明中一种可降解的纺黏过滤材料的制备原理图;Fig. 1 is the preparation schematic diagram of a kind of degradable spunbonded filter material among the present invention;
图2是本发明实施例中的三层纤维网的结构示意图;Fig. 2 is the structural representation of the three-layer fiber net in the embodiment of the present invention;
图3是本发明实施例中的皮芯型双组分纤维的截面示意图;Fig. 3 is a schematic cross-sectional view of a sheath-core bicomponent fiber in an embodiment of the present invention;
其中:1,上层纤维网;2,中层纤维网;3,下层纤维网;4,纤维芯层;5,纤维皮层;Among them: 1, upper fiber web; 2, middle fiber web; 3, lower fiber web; 4, fiber core layer; 5, fiber cortex;
图4是本发明实施例中的设备工艺流程图;Fig. 4 is the equipment process flowchart in the embodiment of the present invention;
图5是本发明实施例中皮芯型双组分纺黏设备的纺丝组件的剖面图;Fig. 5 is a cross-sectional view of the spinning assembly of the sheath-core type two-component spunbond equipment in an embodiment of the present invention;
其中:6,料斗;7,螺杆挤出机;8,过滤器;9,计量泵;10,纺丝组件;11,新型侧吹风装置;12,整体式宽狭缝牵伸器;13,热黏合加固;14,卷绕装置;15,电晕驻极装置;16,高压电源;17,放电针尖电极;18,接地金属辊。Among them: 6, hopper; 7, screw extruder; 8, filter; 9, metering pump; 10, spinning assembly; 11, new side blowing device; 12, integral wide slit drafter; 13, heat Adhesive reinforcement; 14, winding device; 15, corona electret device; 16, high-voltage power supply; 17, discharge needle-point electrode; 18, grounded metal roller.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明作进一步说明,以使本领域的技术人员可以更好地理解本发明并能予以实施,但所举实施例不作为对本发明的限定。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments, so that those skilled in the art can better understand the present invention and implement it, but the examples given are not intended to limit the present invention.
下述实施例和对比例中,所使用的实验方法无特殊说明,均为常规方法,所用的材料、试剂等,如无特殊说明,均可从商业途径得到。In the following examples and comparative examples, the experimental methods used are conventional methods unless otherwise specified, and the materials and reagents used can be obtained from commercial sources unless otherwise specified.
本发明PBAT颗粒购于宁波百福得环保科技有限公司,规格:密度:1.15g/cm3~1.28g/cm3,熔点:115℃~130℃,透明度:30%~60%;硬脂酸钙颗粒购于江山市艺天科技有限公司,规格:熔点:150℃~160℃,钙含量:6.4~7.4%;硬脂酸镁粉末购于拓亿新材料(广州)有限公司,规格:熔点:108℃~115℃,密度:1.02g/cm3~1.13g/cm3;氮化硅粉末购于苏州赛隆纳诺新材料实业有限公司,规格:平均粒径:20nm,比表面积:93m2/g,密度:3.4g/cm3;二氧化碳基聚氨酯购于杭州普力材料科技有限公司,规格:二氧化碳基聚氨酯的含量为99.1%;纳米氧化锌购于南京保克特新材料有限公司,规格:粒径15nm~20nm,ZnO含量:99%,比表面积:55m2/g。The PBAT granules of the present invention were purchased from Ningbo Baifude Environmental Protection Technology Co., Ltd. Specifications: density: 1.15g/cm 3 -1.28g/cm 3 , melting point: 115°C-130°C, transparency: 30%-60%; stearic acid Calcium particles were purchased from Jiangshan Yitian Technology Co., Ltd. Specifications: melting point: 150°C-160°C, calcium content: 6.4-7.4%; magnesium stearate powder was purchased from Tuoyi New Materials (Guangzhou) Co., Ltd. Specifications: melting point : 108℃~115℃, density: 1.02g/cm 3 ~1.13g/cm 3 ; silicon nitride powder was purchased from Suzhou Sailon Nano New Material Industry Co., Ltd., specifications: average particle size: 20nm, specific surface area: 93m 2 /g, density: 3.4g/cm 3 ; carbon dioxide-based polyurethane was purchased from Hangzhou Puli Material Technology Co., Ltd., specifications: the content of carbon dioxide-based polyurethane is 99.1%; nano-zinc oxide was purchased from Nanjing Baoket New Material Co., Ltd. Specifications: particle size 15nm~20nm, ZnO content: 99%, specific surface area: 55m 2 /g.
实施例1Example 1
本实施例提供一种兼具增能/抗菌功能的可降解纺黏过滤材料的制备方法,包括以下步骤:This embodiment provides a method for preparing a degradable spun-bonded filter material with energy-enhancing/antibacterial functions, including the following steps:
将增能助剂与PBAT颗粒分别加入双螺杆造粒机的两个料斗,在180℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到PBAT增能母粒。其中,增能助剂占PBAT增能母粒的质量比为20%;增能助剂为硬脂酸钙、硬脂酸镁、氮化硅的混合物,且增能助剂中硬脂酸钙、硬脂酸镁、氮化硅的质量比为5:3:2。Add the energizing agent and PBAT granules to the two hoppers of the twin-screw granulator respectively, blend and melt in the twin-screw extruder at a temperature of 180°C, extrude, cool in a water bath, dry, and cut into granules to obtain PBAT Energizing Masterbatch. Among them, the mass ratio of the energy-enhancing additive to the PBAT energy-enhancing masterbatch is 20%; the energy-enhancing additive is a mixture of calcium stearate, magnesium stearate, and silicon nitride, and the calcium stearate in the energy-enhancing additive , magnesium stearate, and silicon nitride in a mass ratio of 5:3:2.
将抗菌颗粒与二氧化碳基聚氨酯颗粒分别加入双螺杆造粒机的两个料斗,在200℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到改性二氧化碳基聚氨酯母粒。其中,抗菌颗粒占改性二氧化碳基聚氨酯母粒的质量比为15%,且抗菌颗粒为纳米氧化锌。The antibacterial granules and carbon dioxide-based polyurethane granules were added to the two hoppers of the twin-screw granulator respectively, blended and melted in the twin-screw extruder at a temperature of 200°C, extruded, cooled in a water bath, dried, and cut into granules to obtain Modified carbon dioxide-based polyurethane masterbatch. Wherein, the mass ratio of the antibacterial particles to the modified carbon dioxide-based polyurethane masterbatch is 15%, and the antibacterial particles are nanometer zinc oxide.
将改性二氧化碳基聚氨酯母粒与常规二氧化碳基聚氨酯颗粒混合作为皮层原料,改性二氧化碳基聚氨酯母粒占皮层原料的质量比为3%;将PBAT增能母粒与常规PBAT混合作为芯层原料,PBAT增能母粒占芯层原料的质量比为5%。The modified carbon dioxide-based polyurethane masterbatch is mixed with conventional carbon dioxide-based polyurethane particles as the raw material of the skin layer, and the mass ratio of the modified carbon dioxide-based polyurethane masterbatch to the raw material of the skin layer is 3%; the PBAT energized masterbatch is mixed with conventional PBAT as the core layer raw material , the mass ratio of PBAT energized masterbatch to the core material is 5%.
制备兼具增能/抗菌功能的可降解纺黏过滤材料的具体设备工艺流程图4所示;皮芯型双组分纺黏设备的纺丝组件的剖面图如图5所示;由图4和图5可以看出:将皮层原料与芯层原料分别加入皮芯型双组分纺黏设备的两个料斗中,分别经各自的螺杆挤出机加热熔融、过滤器过滤杂质、计量泵计量后,到达纺丝组件形成皮芯复合结构的熔体细流,经侧吹风冷却,调节牵伸时气流的初始速度,分丝,制备得到皮芯结构的纤维(皮芯型双组分纤维的截面示意图如图2所示),皮芯结构的纤维到达成网帘,分别制备出纤维直径不同的上、中、下三层纤维网。当牵伸时气流的初始速度为80m/s时制备得到纤维直径为16μm、克重为25g/m2的上层纤维网;当牵伸时气流的初始速度为105m/s时制备得到纤维直径为12μm、克重为30g/m2的中层纤维网;当牵伸时气流的初始速度为120m/s时制备得到纤维直径为9μm、克重为40g/m2的下层纤维网.将制成的上、中、下三层纤维网(三层纤维网的结构示意图如图2所示)自上而下依次排列,使用温度为175℃的热轧辊进行热黏合加固,固结成布、卷绕成型,最后将其在8kV/cm的静电场中电晕驻极55秒,即得到兼具增能/抗菌功能的可降解纺黏过滤材料。The specific equipment process flow chart for preparing degradable spunbond filter materials with energy-enhancing/antibacterial functions is shown in Figure 4; the cross-sectional view of the spinning assembly of the skin-core two-component spunbond equipment is shown in Figure 5; It can be seen from Figure 5 that the raw materials for the skin layer and the core layer are added to the two hoppers of the skin-core type two-component spunbond equipment, heated and melted by the respective screw extruders, filtered by the filter, and metered by the metering pump. Finally, the thin stream of melt that reaches the spinning assembly to form a skin-core composite structure is cooled by side blowing, the initial velocity of the airflow is adjusted during drafting, and the fibers are separated to prepare fibers with a skin-core structure (skin-core bicomponent fibers) The cross-sectional schematic diagram is shown in Figure 2), the fibers of the skin-core structure reach the web curtain, and the upper, middle and lower three-layer fiber webs with different fiber diameters are prepared respectively. When the initial velocity of air-flow is 80m/s when drafting, it is 16 μ m that fiber diameter is prepared, and the grammage is 25g/m 2 upper fiber web; 12 μm, grammage is 30g/m 2 middle layer fiber net; When the initial velocity of airflow is 120m/s when drafting, the lower layer fiber web with fiber diameter 9μm, grammage is 40g/m 2 is prepared. Will make The upper, middle, and lower three-layer fiber webs (the structural diagram of the three-layer fiber web is shown in Figure 2) are arranged sequentially from top to bottom, and are thermally bonded and reinforced by hot rolls at a temperature of 175°C, consolidated into cloth, and wound molding, and finally corona electret in an electrostatic field of 8kV/cm for 55 seconds to obtain a degradable spunbonded filter material with both energy-enhancing and antibacterial functions.
采用TSI8130滤料综合性能测试台测试所得兼具增能/抗菌功能的可降解纺黏过滤材料的过滤效率和过滤阻力:在流速为32L/min,氯化钠气溶胶质量中值直径为0.26μm时,其过滤阻力为36Pa,过滤效率为81%。The filtration efficiency and filtration resistance of the degradable spunbond filter material with energy-enhancing/antibacterial functions tested by the TSI8130 filter material comprehensive performance test bench: at a flow rate of 32L/min, the mass median diameter of sodium chloride aerosol is 0.26μm When the filter resistance is 36Pa, the filter efficiency is 81%.
实施例2Example 2
本实施例提供一种兼具增能/抗菌功能的可降解纺黏过滤材料的制备方法,包括以下步骤:This embodiment provides a method for preparing a degradable spun-bonded filter material with energy-enhancing/antibacterial functions, including the following steps:
将增能助剂与PBAT颗粒分别加入双螺杆造粒机的两个料斗,在180℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到PBAT增能母粒。其中,增能助剂占PBAT增能母粒的质量比为24%;增能助剂为硬脂酸钙、硬脂酸镁、氮化硅的混合物,且增能助剂中硬脂酸钙、硬脂酸镁、氮化硅的比例为5:3:2。Add the energizing agent and PBAT granules to the two hoppers of the twin-screw granulator respectively, blend and melt in the twin-screw extruder at a temperature of 180°C, extrude, cool in a water bath, dry, and cut into granules to obtain PBAT Energizing Masterbatch. Among them, the mass ratio of the energy-enhancing additive to the PBAT energy-enhancing masterbatch is 24%; the energy-enhancing additive is a mixture of calcium stearate, magnesium stearate, and silicon nitride, and the calcium stearate in the energy-enhancing additive , magnesium stearate, silicon nitride ratio is 5:3:2.
将抗菌颗粒与二氧化碳基聚氨酯颗粒分别加入双螺杆造粒机的两个料斗,在200℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到改性二氧化碳基聚氨酯母粒。其中,抗菌颗粒占改性二氧化碳基聚氨酯母粒的质量比为16%,且抗菌颗粒为纳米氧化锌。The antibacterial granules and carbon dioxide-based polyurethane granules were added to the two hoppers of the twin-screw granulator respectively, blended and melted in the twin-screw extruder at a temperature of 200°C, extruded, cooled in a water bath, dried, and cut into granules to obtain Modified carbon dioxide-based polyurethane masterbatch. Wherein, the mass ratio of the antibacterial particles to the modified carbon dioxide-based polyurethane masterbatch is 16%, and the antibacterial particles are nanometer zinc oxide.
将改性二氧化碳基聚氨酯母粒与常规二氧化碳基聚氨酯颗粒混合作为皮层原料,改性二氧化碳基聚氨酯母粒占皮层原料的质量比为6%;将PBAT增能母粒与常规PBAT混合作为芯层原料,PBAT增能母粒占芯层原料的质量比为4%。The modified carbon dioxide-based polyurethane masterbatch is mixed with conventional carbon dioxide-based polyurethane particles as the raw material of the skin layer, and the mass ratio of the modified carbon dioxide-based polyurethane masterbatch to the raw material of the skin layer is 6%; the PBAT energized masterbatch is mixed with conventional PBAT as the core layer raw material , the mass ratio of PBAT energized masterbatch to the core material is 4%.
制备兼具增能/抗菌功能的可降解纺黏过滤材料的具体设备工艺流程图4所示;皮芯型双组分纺黏设备的纺丝组件的剖面图如图5所示;由图4和图5可以看出:将皮层原料与芯层原料分别加入皮芯型双组分纺黏设备的两个料斗中,分别经各自的螺杆挤出机加热熔融、过滤器过滤杂质、计量泵计量后,到达纺丝组件形成皮芯复合结构的熔体细流,经侧吹风冷却,调节牵伸时气流的初始速度,分丝,制备得到皮芯结构的纤维,皮芯结构的纤维到达成网帘,分别制备出上、中、下三层纤维网。当牵伸时气流的初始速度为76m/s时制备得到纤维直径为17μm、克重为28g/m2的上层纤维网;当牵伸时气流的初始速度为100m/s时制备得到纤维直径为13μm、克重为33g/m2的中层纤维网;当牵伸时气流的初始速度为115m/s时制备得到纤维直径为10μm、克重为48g/m2的下层纤维网,将制成的纤维直径不一的上、中、下三层纤维网(三层纤维网的结构示意图如图2所示)自上而下依次排列,使用温度为175℃的热轧辊进行热黏合加固,固结成布、卷绕成型,最后将其在12kV/cm的静电场中电晕驻极60秒,即得到兼具增能/抗菌功能的可降解纺黏过滤材料。The specific equipment process flow chart for preparing degradable spunbond filter materials with energy-enhancing/antibacterial functions is shown in Figure 4; the cross-sectional view of the spinning assembly of the skin-core two-component spunbond equipment is shown in Figure 5; It can be seen from Figure 5 that the raw materials for the skin layer and the core layer are added to the two hoppers of the skin-core type two-component spunbond equipment, heated and melted by the respective screw extruders, filtered by the filter, and metered by the metering pump. Finally, the thin stream of melt that reaches the spinning assembly to form a skin-core composite structure is cooled by side blowing, the initial velocity of the airflow is adjusted during drafting, and the fibers are divided to prepare fibers with a skin-core structure. The fibers of the skin-core structure reach the net For the curtain, the upper, middle and lower layers of fiber webs were prepared respectively. When the initial velocity of the air-flow was 76m/s when drawing, the fiber diameter of 17 μm and the grammage were 28g/ m2 ; when the initial velocity of the air-flow was 100m/s, the fiber diameter was prepared as 13 μm, grammage is the middle layer fiber web of 33g/m 2 ; When the initial speed of airflow is 115m/s when drafting, the lower layer fiber web that the fiber diameter is 10 μm, grammage is 48g/m 2 is prepared, will make The upper, middle and lower three-layer fiber webs with different fiber diameters (the structural diagram of the three-layer fiber web is shown in Figure 2) are arranged sequentially from top to bottom, and are thermally bonded and reinforced by using a hot roll at a temperature of 175 °C. Fabrication, winding and molding, and finally corona electret in an electrostatic field of 12kV/cm for 60 seconds, a degradable spunbond filter material with both energy-enhancing and antibacterial functions can be obtained.
采用TSI8130滤料综合性能测试台测试所得兼具增能/抗菌功能的可降解纺黏过滤材料的过滤效率和过滤阻力:在流速为32L/min,氯化钠气溶胶质量中值直径为0.26m时,其过滤阻力为39Pa,过滤效率为83%。The filtration efficiency and filtration resistance of the degradable spunbond filter material with energy-enhancing/antibacterial functions tested by TSI8130 filter material comprehensive performance test bench: at a flow rate of 32L/min, the mass median diameter of sodium chloride aerosol is 0.26m When the filter resistance is 39Pa, the filter efficiency is 83%.
实施例3Example 3
本实施例提供一种兼具增能/抗菌功能的可降解纺黏过滤材料的制备方法,包括以下步骤:This embodiment provides a method for preparing a degradable spun-bonded filter material with energy-enhancing/antibacterial functions, including the following steps:
将增能助剂与PBAT颗粒分别加入双螺杆造粒机的两个料斗,在180℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到PBAT增能母粒。其中,增能助剂占PBAT增能母粒的质量比为27%;增能助剂为硬脂酸钙、硬脂酸镁、氮化硅的混合物,且增能助剂中硬脂酸钙、硬脂酸镁、氮化硅的比例为5:3:2。Add the energizing agent and PBAT granules to the two hoppers of the twin-screw granulator respectively, blend and melt in the twin-screw extruder at a temperature of 180°C, extrude, cool in a water bath, dry, and cut into granules to obtain PBAT Energizing Masterbatch. Among them, the mass ratio of the energy-enhancing additive to the PBAT energy-enhancing masterbatch is 27%; the energy-enhancing additive is a mixture of calcium stearate, magnesium stearate, and silicon nitride, and the calcium stearate in the energy-enhancing additive , magnesium stearate, silicon nitride ratio is 5:3:2.
将抗菌颗粒与二氧化碳基聚氨酯颗粒分别加入双螺杆造粒机的两个料斗,在200℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到改性二氧化碳基聚氨酯母粒。其中,抗菌颗粒占改性二氧化碳基聚氨酯母粒的质量比为17%,且抗菌颗粒为纳米氧化锌。The antibacterial granules and carbon dioxide-based polyurethane granules were added to the two hoppers of the twin-screw granulator respectively, blended and melted in the twin-screw extruder at a temperature of 200°C, extruded, cooled in a water bath, dried, and cut into granules to obtain Modified carbon dioxide-based polyurethane masterbatch. Wherein, the mass ratio of the antibacterial particles to the modified carbon dioxide-based polyurethane masterbatch is 17%, and the antibacterial particles are nanometer zinc oxide.
将改性二氧化碳基聚氨酯母粒与常规二氧化碳基聚氨酯颗粒混合作为皮层原料,改性二氧化碳基聚氨酯母粒占皮层原料的质量比为5%;将PBAT增能母粒与常规PBAT混合作为芯层原料,PBAT增能母粒占芯层原料的质量比为7%。The modified carbon dioxide-based polyurethane masterbatch is mixed with conventional carbon dioxide-based polyurethane particles as the raw material of the skin layer, and the mass ratio of the modified carbon dioxide-based polyurethane masterbatch to the raw material of the skin layer is 5%; the PBAT energized masterbatch is mixed with conventional PBAT as the core layer raw material , the mass ratio of PBAT energized masterbatch to the core material is 7%.
制备兼具增能/抗菌功能的可降解纺黏过滤材料的具体设备工艺流程图4所示;皮芯型双组分纺黏设备的纺丝组件的剖面图如图5所示;由图4和图5可以看出:将皮层原料与芯层原料分别加入皮芯型双组分纺黏设备的两个料斗中,分别经各自的螺杆挤出机加热熔融、过滤器过滤杂质、计量泵计量后,到达纺丝组件形成皮芯复合结构的熔体细流,经侧吹风冷却,调节牵伸时气流的初始速度、分丝,制备得到皮芯结构的纤维,皮芯结构的纤维到达成网帘,分别制备出上、中、下三层纤维网。当牵伸时气流的初始速度为73m/s时制备得到纤维直径为18μm、克重为30g/m2的上层纤维网;当牵伸时气流的初始速度为95m/s时制备得到纤维直径为14μm、克重为36g/m2的中层纤维网;当牵伸时气流的初始速度为110m/s时制备得到纤维直径为11μm、克重为55g/m2的下层纤维网,将制成的纤维直径不一的上、中、下三层纤维网(三层纤维网的结构示意图如图2所示)自上而下依次排列,使用温度为175℃的热轧辊进行热黏合加固,固结成布、卷绕成型,最后将其在12kV/cm的静电场中电晕驻极70秒,即得到兼具增能/抗菌功能的可降解纺黏过滤材料。The specific equipment process flow chart for preparing degradable spunbond filter materials with energy-enhancing/antibacterial functions is shown in Figure 4; the cross-sectional view of the spinning assembly of the skin-core two-component spunbond equipment is shown in Figure 5; It can be seen from Figure 5 that the raw materials for the skin layer and the core layer are added to the two hoppers of the skin-core type two-component spunbond equipment, heated and melted by the respective screw extruders, filtered by the filter, and metered by the metering pump. Finally, the thin stream of melt that reaches the spinning assembly to form a skin-core composite structure is cooled by side blowing, and the initial speed and splitting of the airflow during drafting are adjusted to prepare fibers with a skin-core structure. The fibers of the skin-core structure reach the net For the curtain, the upper, middle and lower layers of fiber webs were prepared respectively. When the initial velocity of the air-flow was 73m/s when drawing, the fiber diameter was 18 μm and the grammage was 30g/m The upper fiber web was prepared; when the initial velocity of the air-flow was 95m/s, the fiber diameter was prepared as 14 μm, grammage is the middle layer fiber web of 36g/m 2 ; When the initial velocity of airflow is 110m/s when drafting, the fiber diameter is 11 μm, the grammage is the lower layer fiber web of 55g/m 2 prepared, will make The upper, middle and lower three-layer fiber webs with different fiber diameters (the structural diagram of the three-layer fiber web is shown in Figure 2) are arranged sequentially from top to bottom, and are thermally bonded and reinforced by using a hot roll at a temperature of 175 °C. Fabrication, winding and molding, and finally corona electret in an electrostatic field of 12kV/cm for 70 seconds, a degradable spunbond filter material with both energy-enhancing and antibacterial functions can be obtained.
采用TSI8130滤料综合性能测试台测试所得兼具增能/抗菌功能的可降解纺黏过滤材料的过滤效率和过滤阻力:在流速为32L/min,氯化钠气溶胶质量中值直径为0.26m时,其过滤阻力为45Pa,过滤效率为89%。The filtration efficiency and filtration resistance of the degradable spunbond filter material with energy-enhancing/antibacterial functions tested by TSI8130 filter material comprehensive performance test bench: at a flow rate of 32L/min, the mass median diameter of sodium chloride aerosol is 0.26m When the filter resistance is 45Pa, the filter efficiency is 89%.
实施例4Example 4
本实施例提供一种兼具增能/抗菌功能的可降解纺黏过滤材料的制备方法,包括以下步骤:This embodiment provides a method for preparing a degradable spun-bonded filter material with energy-enhancing/antibacterial functions, including the following steps:
将增能助剂与PBAT颗粒分别加入双螺杆造粒机的两个料斗,在180℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到PBAT增能母粒。其中,增能助剂占PBAT增能母粒的质量比为29%;增能助剂为硬脂酸钙、硬脂酸镁、氮化硅的混合物,且增能助剂中硬脂酸钙、硬脂酸镁、氮化硅的比例为5:3:2。Add the energizing agent and PBAT granules to the two hoppers of the twin-screw granulator respectively, blend and melt in the twin-screw extruder at a temperature of 180°C, extrude, cool in a water bath, dry, and cut into granules to obtain PBAT Energizing Masterbatch. Among them, the mass ratio of the energy-enhancing additive to the PBAT energy-enhancing masterbatch is 29%; the energy-enhancing additive is a mixture of calcium stearate, magnesium stearate, and silicon nitride, and the calcium stearate in the energy-enhancing additive , magnesium stearate, silicon nitride ratio is 5:3:2.
将抗菌颗粒与二氧化碳基聚氨酯颗粒分别加入双螺杆造粒机的两个料斗,在200℃的温度下于双螺杆挤出机中共混熔融后挤出,经水浴冷却、干燥后切割成粒,得到改性二氧化碳基聚氨酯母粒。其中,抗菌颗粒占改性二氧化碳基聚氨酯母粒的质量比为18%,且抗菌颗粒为纳米氧化锌。The antibacterial granules and carbon dioxide-based polyurethane granules were added to the two hoppers of the twin-screw granulator respectively, blended and melted in the twin-screw extruder at a temperature of 200°C, extruded, cooled in a water bath, dried, and cut into granules to obtain Modified carbon dioxide-based polyurethane masterbatch. Wherein, the mass ratio of the antibacterial particles to the modified carbon dioxide-based polyurethane masterbatch is 18%, and the antibacterial particles are nanometer zinc oxide.
将改性二氧化碳基聚氨酯母粒与常规二氧化碳基聚氨酯颗粒混合作为皮层原料,改性二氧化碳基聚氨酯母粒占皮层原料的质量比为7%;将PBAT增能母粒与常规PBAT混合作为芯层原料,PBAT增能母粒占芯层原料的质量比为8%。The modified carbon dioxide-based polyurethane masterbatch is mixed with conventional carbon dioxide-based polyurethane particles as the raw material of the skin layer, and the mass ratio of the modified carbon dioxide-based polyurethane masterbatch to the raw material of the skin layer is 7%; the PBAT energized masterbatch is mixed with conventional PBAT as the core layer raw material , the mass ratio of PBAT energized masterbatch to the core material is 8%.
制备兼具增能/抗菌功能的可降解纺黏过滤材料的具体设备工艺流程图4所示;皮芯型双组分纺黏设备的纺丝组件的剖面图如图5所示;由图4和图5可以看出:将皮层原料与芯层原料分别加入皮芯型双组分纺黏设备的两个料斗中,分别经各自的螺杆挤出机加热熔融、过滤器过滤杂质、计量泵计量后,到达纺丝组件形成皮芯复合结构的熔体细流,经侧吹风冷却,调节牵伸时气流的初始速度、分丝,制备得到皮芯结构的纤维,皮芯结构的纤维到达成网帘,分别制备出上、中、下三层纤维网。当牵伸时气流的初始速度为70m/s时制备得到纤维直径为19μm、克重为35g/m2的上层纤维网;当牵伸时气流的初始速度为90m/s时制备得到纤维直径为15μm、克重为40g/m2的中层纤维网;当牵伸时气流的初始速度为110m/s时制备得到纤维直径为11μm、克重为60g/m2的下层纤维网,将制成的纤维直径不一的上、中、下三层纤维网(三层纤维网的结构示意图如图2所示)自上而下依次排列,使用温度为175℃的热轧辊进行热黏合加固,固结成布、卷绕成型,最后将其在14kV/cm的静电场中电晕驻极70秒,即得到兼具增能/抗菌功能的可降解纺黏过滤材料。The specific equipment process flow chart for preparing degradable spunbond filter materials with energy-enhancing/antibacterial functions is shown in Figure 4; the cross-sectional view of the spinning assembly of the skin-core two-component spunbond equipment is shown in Figure 5; It can be seen from Figure 5 that the raw materials for the skin layer and the core layer are added to the two hoppers of the skin-core type two-component spunbond equipment, heated and melted by the respective screw extruders, filtered by the filter, and metered by the metering pump. Finally, the thin stream of melt that reaches the spinning assembly to form a skin-core composite structure is cooled by side blowing, and the initial speed and splitting of the airflow during drafting are adjusted to prepare fibers with a skin-core structure. The fibers of the skin-core structure reach the net For the curtain, the upper, middle and lower layers of fiber webs were prepared respectively. When the initial velocity of the air-flow was 70m/s when drawing, the fiber diameter was 19 μm and the grammage was 35g/m The upper fiber web was prepared; when the initial velocity of the air-flow was 90m/s, the fiber diameter was prepared as 15 μm, grammage is the middle fiber web of 40g/m 2 ; When the initial speed of airflow is 110m/s when drafting, the lower layer fiber web with fiber diameter of 11 μm and grammage of 60g/m 2 is prepared, and the prepared The upper, middle and lower three-layer fiber webs with different fiber diameters (the structural diagram of the three-layer fiber web is shown in Figure 2) are arranged sequentially from top to bottom, and are thermally bonded and reinforced by using a hot roll at a temperature of 175 °C. Fabrication, winding and molding, and finally corona electret in an electrostatic field of 14kV/cm for 70 seconds, a degradable spunbond filter material with both energy-enhancing and antibacterial functions can be obtained.
采用TSI8130滤料综合性能测试台测试所得兼具增能/抗菌功能的可降解纺黏过滤材料的过滤效率和过滤阻力:在流速为32L/min,氯化钠气溶胶质量中值直径为0.26m时,其过滤阻力为50Pa,过滤效率为93%。The filtration efficiency and filtration resistance of the degradable spunbond filter material with energy-enhancing/antibacterial functions tested by TSI8130 filter material comprehensive performance test bench: at a flow rate of 32L/min, the mass median diameter of sodium chloride aerosol is 0.26m When the filter resistance is 50Pa, the filter efficiency is 93%.
对比例1Comparative example 1
本对比例与实施例1类似,区别仅在于,所述滤料纤维的芯层组分中不添加增能助剂,即硬脂酸钙、硬脂酸镁、氮化硅的混合物。This comparative example is similar to Example 1, the only difference is that no energy-enhancing additive, that is, a mixture of calcium stearate, magnesium stearate, and silicon nitride, is added to the core layer component of the filter material fiber.
对比例2Comparative example 2
本对比例与实施例1类似,区别仅在于,所述滤料纤维的皮层组分中不添加抗菌颗粒,即纳米氧化锌。This comparative example is similar to Example 1, the only difference is that no antibacterial particles, ie nano zinc oxide, are added to the skin layer component of the filter material fiber.
对比例3Comparative example 3
本对比例与实施例1类似,区别仅在于,所述上、中、下三层纤维网进行热黏合加固后,直接固结成布、卷绕成型,不进行电晕驻极处理。This comparative example is similar to Example 1, the only difference being that the upper, middle and lower layers of fiber webs are thermally bonded and reinforced, and then directly consolidated into cloth and wound into shape without corona electret treatment.
性能测试Performance Testing
将实施例1-3及对比例1-3所制备的兼具增能/抗菌功能的可降解纺黏过滤材料进行过滤性能、抗菌性能、强力性能和透气性能测试,测试依据的标准如下:The degradable spunbonded filter material with both energy-enhancing/antibacterial functions prepared in Examples 1-3 and Comparative Examples 1-3 was tested for filtration performance, antibacterial performance, strength performance and air permeability. The standards for the test basis are as follows:
(1)采用TSI8130滤料自动测试仪测试所得双组分纺黏滤料的过滤性能:在流速为32L/min,氯化钠气溶胶质量中值直径为0.26m时,测试过滤阻力和过滤效率。(1) Use TSI8130 filter material automatic tester to test the filtration performance of the obtained two-component spunbond filter material: when the flow rate is 32L/min and the median diameter of the sodium chloride aerosol mass is 0.26m, the filtration resistance and filtration efficiency are tested .
(2)抗菌性能测试指标:T/YNIA 001-2021《抗菌抗病毒非织造材料》(2) Antibacterial performance test index: T/YNIA 001-2021 "Antibacterial and antiviral nonwoven materials"
(3)降解性能测试指标:GB T22047-2008《土壤中塑料材料最终需氧生物分解能力的测定通过测定密闭呼吸机中需氧量或测定释放的二氧化碳的方法》。(3) Degradation performance test index: GB T22047-2008 "Determination of the final aerobic biodegradability of plastic materials in soil by measuring the oxygen demand in a closed ventilator or measuring the released carbon dioxide".
表1实施例1-3,对比例1-3制备的兼具增能/抗菌功能的可降解纺黏过滤材料的性能测试结果Table 1 Example 1-3, the performance test results of the degradable spunbonded filter material with energy-enhancing/antibacterial function prepared in Comparative Example 1-3
由表1的结果显示,实施例1-4制备的一种兼具增能/抗菌功能的可降解纺黏过滤材料中增能助剂、抗菌颗粒、改性二氧化碳基聚氨酯母粒及PBAT增能母粒的含量逐渐增加,三层纤维网纤维直径、纤维网克重逐渐增大,电晕驻极的驻极电压逐渐增大,驻极时间逐渐增长,故而该滤料的过滤效率、抑菌率逐渐提高。The results in Table 1 show that in a degradable spunbonded filter material with energy enhancement/antibacterial function prepared in Examples 1-4, energy enhancement additives, antibacterial particles, modified carbon dioxide-based polyurethane masterbatches and PBAT energy enhancement The content of the masterbatch gradually increases, the fiber diameter of the three-layer fiber net and the weight of the fiber net gradually increase, the electret voltage of the corona electret gradually increases, and the electret time gradually increases, so the filtration efficiency of the filter material, antibacterial rate gradually increased.
对比例1制备的一种兼具增能/抗菌功能的可降解纺黏过滤材料中没有加入增能助剂,故而该滤料的过滤效率偏低,但抑菌率基本不变。A degradable spunbond filter material with energy-enhancing/antibacterial functions prepared in Comparative Example 1 did not add energy-enhancing additives, so the filtration efficiency of the filter material was low, but the bacteriostatic rate remained basically unchanged.
对比例2制备的一种兼具增能/抗菌功能的可降解纺黏过滤材料中没有加入抗菌颗粒,故而该滤料的过滤效率基本不变,但抑菌率偏低。A degradable spunbonded filter material with energy-enhancing/antibacterial functions prepared in Comparative Example 2 did not add antibacterial particles, so the filtration efficiency of the filter material remained basically unchanged, but the antibacterial rate was low.
对比例3制备的一种兼具增能/抗菌功能的可降解纺黏过滤材料没有进行电晕驻极处理,故而该滤料的过滤效率偏低,且抑菌率较低。A degradable spunbonded filter material with both energy-enhancing and antibacterial functions prepared in Comparative Example 3 was not subjected to corona electret treatment, so the filter material had low filtration efficiency and low bacteriostatic rate.
综上,本发明是通过增能助剂、三层纤维网的设置以及电晕驻极工艺等参数共同提高材料过滤效率的。To sum up, the present invention improves the material filtration efficiency through parameters such as the energizing agent, the setting of the three-layer fiber net, and the corona electret process.
显然,上述实施例仅仅是为清楚地说明所作的举例,并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。Apparently, the above-mentioned embodiments are only examples for clear description, and are not intended to limit the implementation. For those of ordinary skill in the art, on the basis of the above description, other changes or changes in various forms can also be made. It is not necessary and impossible to exhaustively list all the implementation manners here. However, the obvious changes or changes derived therefrom are still within the scope of protection of the present invention.
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