WO2022000939A1 - 低阻力口罩用熔喷无纺布用驻极母粒及其制备方法 - Google Patents

低阻力口罩用熔喷无纺布用驻极母粒及其制备方法 Download PDF

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WO2022000939A1
WO2022000939A1 PCT/CN2020/129278 CN2020129278W WO2022000939A1 WO 2022000939 A1 WO2022000939 A1 WO 2022000939A1 CN 2020129278 W CN2020129278 W CN 2020129278W WO 2022000939 A1 WO2022000939 A1 WO 2022000939A1
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melt
electret
low
polypropylene
resistance
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French (fr)
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李力
王斌
王道娟
杨友强
杨曦
程文建
刘乐文
杨霄云
陈平绪
叶南飚
黄险波
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金发科技股份有限公司
广东金发科技有限公司
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Publication of WO2022000939A1 publication Critical patent/WO2022000939A1/zh

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10Homopolymers or copolymers of propene
    • C08J2423/12Polypropene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04Polysiloxanes
    • C08J2483/07Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04Ingredients characterised by their shape and organic or inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/38Boron-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098Metal salts of carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/20Carboxylic acid amides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • C08K7/26Silicon- containing compounds

Definitions

  • the invention relates to the field of melt-blown non-woven fabrics, in particular to electret masterbatches for melt-blown non-woven fabrics for low-resistance masks and a preparation method thereof.
  • Melt-blown non-woven fabric for masks is a material for preparing filter masks. Although the filtration efficiency can be improved by electret treatment, only electret treatment of the non-woven fabric itself can improve the filtration efficiency to a limited extent. In order to achieve the ideal filtering effect, electret materials or electret masterbatches are generally added to the formula of meltblown non-woven fabrics for masks. However, the addition of electret masterbatch leads to a great increase in the resistance of the mask. Therefore, to make a filter mask, it is necessary to balance the contradiction between the filtering effect and the resistance.
  • melt-blown non-woven fabric that can have both excellent filtering effect and low breathing resistance as soon as possible.
  • the object of the present invention is to overcome the deficiencies in the prior art, provide a kind of electret master batch for the melt-blown nonwoven fabric for masks with low resistance, when the master batch is used for the production of the melt-blown non-woven fabric for masks, it can produce the Meltblown non-woven fabrics for masks have high filtration efficiency and low breathing resistance.
  • Another object of the present invention is to provide a method for preparing the electret masterbatch for the melt-blown nonwoven fabric for the low-resistance mask.
  • Another object of the present invention is to provide a melt-blown non-woven fabric containing the electret masterbatch for the melt-blown non-woven fabric for low-resistance masks.
  • a kind of electret masterbatch for melt-blown non-woven fabrics for low-resistance masks is made of the following components calculated by weight percentage:
  • the softener is erucamide
  • the polypropylene resin is homopolymer polypropylene and/or copolymer polypropylene, and its melt index MFI is not less than 1000g/10min at 230°C/2.16kg.
  • adding a softener to the melt-blown nonwoven fabric for masks can reduce the friction between the air and the fibers.
  • the presence of softener may have a negative impact on the electret treatment, especially the effect of electret powder, so it needs to be screened.
  • adding a nucleating agent to the melt-blown non-woven fabric for masks at the same time can reduce the self-adhesion of polypropylene fibers during the melt-blown process, thereby reducing the density of the fiber web, and the softener and nucleating agent are reasonably compatible. , which can significantly reduce the resistance of the melt-blown non-woven fabric.
  • the combination of a specific softener and electret powder can maintain a good filtering effect, so the melt-blown non-woven fabric for masks can have excellent filtering performance. and low resistance.
  • the melt index MFI of the polypropylene resin is preferably 1000-1500 g/10min at 230°C/2.16kg.
  • the melt index of polypropylene resin is greater than or equal to 1000g/10min, it can already meet the filtering capacity of ordinary medical masks (YY/T 0969-2013 "Disposable Medical Masks").
  • the melt index MFI of the polypropylene resin is 1500g/10min, the filtering effect required by KN95 can be achieved.
  • the electret powder is an important component of the melt-blown nonwoven fabric for masks, and its addition can make the filtering effect of the melt-blown non-woven fabric for masks reach an ideal level.
  • the conventional electret powder of cloth for example, is one or more of nano tourmaline powder, nano silicon dioxide, nano polysilsesquioxane powder (nano POSS powder). Most preferably, the electret powder is most preferably nano tourmaline powder, and its electret effect is better than other conventional electret powders.
  • the dispersing agent is polyethylene wax, fatty acid salt, maleic anhydride grafted polypropylene, maleic anhydride grafted polyethylene, maleic anhydride grafted POE, glycidyl methacrylate grafted polypropylene, Any one or more of glycidyl methacrylate graft POE and glycidyl methacrylate graft EPDM.
  • Common fatty acid salt dispersants are, for example, calcium stearate, zinc stearate, magnesium stearate, lithium stearate, and the like.
  • the function of the nucleating agent is to increase the crystallization temperature of polypropylene fibers, so that the self-adhesion of polypropylene during the melt blowing process is reduced.
  • the nucleating agent is a carboxylate-based nucleating agent, a phosphate-based nucleating agent or a sorbitol-based nucleating agent.
  • Commonly used nucleating agents can be: aluminum p-tert-butylbenzoate, bis[2,2'-methylene-bis(4,6-di-tert-butylphenyl)phosphate]hydroxyaluminum, dibenzylidene sorbitol Wait.
  • processing aids are usually added to the masterbatch.
  • the processing aid is one or more of antioxidants and antiaging agents.
  • antioxidants are, for example, antioxidant 1010 (tetrakis[beta-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid]pentaerythritol ester), antioxidant 168 (tris(2,4- Di-tert-butylphenyl) phosphite) and the like.
  • the preparation method of the electret masterbatch for the melt-blown non-woven fabric for the low-resistance mask is to premix the components through a mixer, and then use a twin-screw extruder to perform melt-blending extrusion and granulation to obtain,
  • the process temperature is 130 ⁇ 220°C.
  • the screw length-diameter ratio of the twin-screw extruder is greater than or equal to 40:1.
  • the larger screw aspect ratio is conducive to the uniform dispersion of the components in the masterbatch, so that it can achieve better results after mixing with the ultra-high melt index polypropylene resin.
  • the screw length-diameter ratio of the twin-screw extruder is 40:1 to 48:1.
  • a melt-blown nonwoven fabric for a low-resistance mask comprising electret masterbatch for the melt-blown non-woven fabric for the low-resistance mask and polypropylene for the melt-blown non-woven fabric, and a melt-blown non-woven fabric for the low-resistance mask
  • the weight ratio of electret masterbatch to polypropylene for melt-blown nonwoven is 1:(19-49).
  • the melt index MFI of the polypropylene for melt-blown nonwovens is usually greater than or equal to 1000g/10min at 230°C/2.16kg.
  • the present invention has the following beneficial effects:
  • the electret masterbatch for melt-blown non-woven fabrics for low-resistance masks provided by the present invention, by adding ingredients such as softeners and nucleating agents, the electret masterbatches for melt-blown non-woven fabrics for low-resistance masks and ultra-high
  • melt-finger polypropylene is mixed for the production of melt-blown non-woven fabrics
  • the obtained melt-blown non-woven fabric for masks can have high filtration efficiency and low breathing resistance, so it is especially suitable as a mask material.
  • the formulation also does not make major adjustments to the formulation of the existing electret masterbatch, and is easy to implement.
  • melt index MFI 1500g/10min at 230°C/2.16kg
  • Polypropylene for melt-blown non-woven fabrics was purchased from Kingfa Technology Company, and its melt index MFI was 1500g/10min at 230°C/2.16kg;
  • melt index MFI 1000g/10min at 230°C/2.16kg
  • Nano tourmaline powder purchased from Tianjin Hongyan Tianshan Stone Industry Nanotechnology Co., Ltd.;
  • Nano POSS powder purchased from Aladdin, model octavinyl-POSS;
  • Nano-silica purchased from Guangzhou Jibiseng Technology Industrial Co., Ltd.;
  • Zinc stearate was purchased from Jiangxi Hongyuan
  • Maleic anhydride grafted POE was purchased from DuPont, USA;
  • Erucamide was purchased from Croda Oleochemicals, UK;
  • Antioxidant 1010 and Antioxidant 168 were both purchased from BASF.
  • the material is put into a high-speed mixer for mixing, and is melted, blended and extruded by a twin-screw extruder with a length-to-diameter ratio of 40:1, and the temperature of the melting section is 150 to 210 ° C to obtain a melt-blown nonwoven fabric for masks.
  • the melt-blown non-woven fabric material for the mask was tested by TSI8130 automatic filter material tester, using the GB19083-2010 "Technical Requirements for Medical Protective Masks" standard, the medium was NaCl particles with a median particle size of 0.075 ⁇ 0.02 ⁇ m, and the test flow rate was 85L/ min, carry out filtration efficiency and inhalation resistance test. The results are shown in Table 2.
  • the filtration efficiency is required to be above 95%, and the inhalation resistance is required to be below 343.2Pa.
  • the inhalation resistance is required to be below 343.2Pa.
  • generally higher than 200Pa will cause difficulty in breathing.
  • Comparative Example 1 it can be seen from Comparative Example 1 that when the nucleating agent and softening agent are not added, the inhalation resistance of the product is still high. It can be seen from Comparative Example 2 that when only the nucleating agent is added, the resistance of the product decreases slightly, and its filtration efficiency also increases slightly, but it is not significant. It can be seen from Comparative Example 3 that the addition of silicone as a softener to the system will have a negative impact on the electret effect, resulting in a decrease in filtration efficiency, which cannot meet the requirements of GB 19083-2010 "Technical Requirements for Medical Protective Masks" for medical protective masks. Standard filter performance.
  • the material is put into a high-speed mixer for mixing, and is melted, blended and extruded by a twin-screw extruder with a length-to-diameter ratio of 48:1, and the temperature of the melting section is 150-210 ° C to obtain a melt-blown nonwoven fabric for masks.
  • comparative example 5 prepares the mask with the melt-blown non-woven fabric electret master batch and melt-blown non-woven fabric with polypropylene (melt index 1500g/10min) mixes, and wherein said mask is melt-blown with
  • the weight ratio of electret masterbatch for non-woven fabric to polypropylene for melt-blown non-woven fabric is 1:49.
  • the obtained mixture is melted by a single screw, metered by a metering pump, and sprayed through a spinneret to form fibers.
  • the fibers are drawn by hot air at 230-270°C to form test samples.
  • the test sample was then subjected to a 30kV voltage electret treatment and then wound up to obtain a sample melt-blown non-woven fabric material.
  • the melt-blown non-woven fabric material for the mask was tested by TSI8130 automatic filter material tester, using the GB19083-2010 "Technical Requirements for Medical Protective Masks" standard, the medium was NaCl particles with a median particle size of 0.075 ⁇ 0.02 ⁇ m, and the test flow rate was 85L/ min, carry out the filtration efficiency test; at the same time carry out the inspiratory resistance test.
  • Table 4 The results are shown in Table 4.
  • Example 3 97.9 113
  • Example 4 91.2 115
  • Example 5 95.2
  • Example 6 90.6 110
  • Example 7 90.1 112
  • Example 8 91.0 108 Comparative Example 5 82.1 115

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Respiratory Apparatuses And Protective Means (AREA)
  • Filtering Materials (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

本发明公开一种低阻力口罩用熔喷无纺布用驻极母粒及其制备方法。所述低阻力口罩用熔喷无纺布用驻极母粒由如下按重量百分数计算的组分制成:聚丙烯树脂65~85%;驻极粉1~3%;分散剂5~15%;成核剂3~10%;柔软剂3~10%;加工助剂0.05~0.5%;所述柔软剂为芥酸酰胺;所述聚丙烯树脂为均聚聚丙烯和/或共聚聚丙烯,其熔融指数MFI在230℃/2.16kg下,不低于1000g/10min。所述驻极母粒,通过加入柔软剂、成核剂等成分,使得驻极母粒与超高熔指聚丙烯混合用于口罩用熔喷无纺布生产时,得到的口罩用熔喷无纺布可以在具有较高过滤效率的同时,兼具低的呼吸阻力,因此特别适合作为口罩材料。该配方也并未对已有的驻极母粒的配方进行大的调整,容易实施。

Description

低阻力口罩用熔喷无纺布用驻极母粒及其制备方法 技术领域
本发明涉及熔喷无纺布领域,特别涉及低阻力口罩用熔喷无纺布用驻极母粒及其制备方法。
背景技术
口罩用熔喷无纺布是一种制备过滤口罩的材料,尽管可以通过驻极处理提高其过滤效率,但是仅仅对无纺布自身进行驻极处理过滤效率的提升程度有限。为了达到理想的过滤效果,一般在口罩用熔喷无纺布的配方中,加入驻极材料或驻极母粒。然而,驻极母粒的加入导致口罩的阻力大大上升。因此,制作过滤口罩,需要平衡过滤效果和阻力这对矛盾。
现有技术中,有通过调整工艺和配方两种思路来实现,但由于过滤性能及呼吸阻力的因素很多,如纤维线密度、纤网的结构、厚度和密度等,导致调整工艺的工作变得非常复杂和困难;配方调整似乎是一条更可行的思路,如CN103046231A公开,在熔纺非织造材料的配方中,通过羧酸金属盐、磷酸金属盐、透明成核剂等添加剂来控制纤网中纤维的细度分布,从而改善其蓬松性能,不过未反映对呼吸阻力的影响。
在口罩材料需求量较大的当下,尽快开发出一种能兼具优异的过滤效果和低呼吸阻力的熔喷无纺布具有重大意义。
发明内容
本发明的目的在于克服现有技术的不足,提供一种低阻力口罩用熔喷无纺布用驻极母粒,该母粒用于口罩用熔喷无纺布生产时,能使生产得到的口罩用熔喷无纺布在具有较高过滤效率的同时,兼具低的呼吸阻力。
本发明的另一目的在于提供所述低阻力口罩用熔喷无纺布用驻极母粒的制备方法。
本发明的另一目的在于提供一种含有所述低阻力口罩用熔喷无纺布用驻极母粒的熔喷无纺布。
本发明的上述目的通过如下技术方案予以实现:
一种低阻力口罩用熔喷无纺布用驻极母粒,由如下按重量百分数计算的组分制成:
聚丙烯树脂 65~85%;
驻极粉 1~3%;
分散剂 5~15%;
成核剂 3~10%;
柔软剂 3~10%;
加工助剂 0.05~0.5%;
所述柔软剂为芥酸酰胺;
所述聚丙烯树脂为均聚聚丙烯和/或共聚聚丙烯,其熔融指数MFI在230℃/2.16kg下,不低于1000g/10min。
发明人经过大量实验尝试总结发现,在口罩用熔喷无纺布中加入柔软剂时,能降低空气与纤维之间的摩擦力。但柔软剂的存在,对驻极处理,尤其是驻极粉的效果有可能存在负面影响,因此需要对其进行筛选。另外,在口罩用熔喷无纺布中同时加入成核剂,可以通过减少聚丙烯纤维在熔喷过程中的自粘程度,从而使纤维网的密实程度降低,柔软剂和成核剂合理配伍,能使得熔喷无纺布的阻力显著降低,同时,特定的柔软剂与驻极粉的搭配,能维持很好的过滤效果,因此使得口罩用熔喷无纺布能兼具优秀的过滤性能和低阻力。
本发明中,所述聚丙烯树脂的熔融指数MFI优选在230℃/2.16kg下,为1000~1500g/10min。根据聚丙烯树脂的熔融指数不同,也会影响最终口罩用熔喷无纺布的过滤效率。因此,当聚丙烯树脂的熔融指数大于等于1000g/10min时,已经能满足普通医护口罩(YY/T 0969-2013《一次性使用医用口罩》)的过滤能力。而当所述聚丙烯树脂的熔融指数MFI在1500g/10min时,能够达到KN95要求的过滤效果。
驻极粉是口罩用熔喷无纺布的重要成分,其加入能使口罩用熔喷无纺布的过滤效果达到理想的程度,本发明所述驻极粉可以是制备口罩用熔喷无纺布的常规驻极粉,例如是纳米电气石粉、纳米二氧化硅、纳米聚倍半硅氧烷粉(纳米POSS粉)中一种或几种。最优选地,所述驻极粉最优选为纳米电气石粉,其驻极效果相对于其他常规驻极粉更好。
为了使驻极粉更好地分散,通常会加入分散剂。优选地,所述分散剂为聚乙烯蜡、脂肪酸盐、马来酸酐接枝聚丙烯、马来酸酐接枝聚乙烯、马来酸酐接枝POE、甲基丙烯酸缩水甘油酯接枝聚丙烯、甲基丙烯酸缩水甘油酯接枝POE、甲基丙烯酸缩水甘油酯接枝EPDM中任意一种或几种。常见的脂肪酸盐分散剂例如是硬脂酸钙、硬脂酸锌、硬脂酸镁、硬脂酸锂等。
成核剂的作用是提高聚丙烯纤维的结晶温度,使得熔喷过程中聚丙烯的自粘情况减少。优选地,所述成核剂为羧酸盐类成核剂、磷酸盐类成核剂或山梨醇类成核剂。常用的成核剂可以是:对叔丁基苯甲酸铝、双[2,2’-亚甲基-双(4,6-二叔丁基苯基)磷酸]羟基铝、二苄叉山梨醇等。
为了便于加工方便,还通常在母粒中还会加入加工助剂。优选地,所述加工助剂为抗氧剂、抗老化剂中的一种或几种。常用的抗氧剂例如是抗氧剂1010(四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯)、抗氧剂168(三(2,4-二叔丁基苯基)亚磷酸酯)等。
所述低阻力口罩用熔喷无纺布用驻极母粒的制备方法为将所述组分通过混合机进行预混合,然后用双螺杆挤出机进行熔融共混挤出并造粒得到,工艺温度在130~220℃。
优选地,所述双螺杆挤出机的螺杆长径比大于等于40:1。更大的螺杆长径比有利于组分在母粒中均匀分散,使其与超高熔指聚丙烯树脂混合后能达到更好的效果。更优选地,所述双螺杆挤出机的螺杆长径比为40:1~48:1。
一种低阻力口罩用熔喷无纺布,包含所述低阻力口罩用熔喷无纺布用驻极母粒及熔喷无纺布用聚丙烯,所述低阻力口罩用熔喷无纺布用驻极母粒与熔喷无纺布用聚丙烯的重量比为1:(19~49)。
所述熔喷无纺布用聚丙烯的熔融指数MFI通常在230℃/2.16kg下,大于等于1000g/10min。
与现有技术相比,本发明具有如下有益效果:
本发明提供的低阻力口罩用熔喷无纺布用驻极母粒,通过加入柔软剂、成核剂等成分,使得所述低阻力口罩用熔喷无纺布用驻极母粒与超高熔指聚丙烯混合用于熔喷无纺布生产时,得到的口罩用熔喷无纺布可以在具有较高过滤效率的同时,兼具低的呼吸阻力,因此特别适合作为口罩材料。该配方也并未对已有的驻 极母粒的配方进行大的调整,容易实施。
具体实施方式
如无特殊说明,本发明所用原料、试剂及溶剂,均为商业购买未经任何处理。下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式并不受下述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。另外,关于本说明书中“份”、“%”,除非特别说明,分别表示“质量份”、“质量%”。
均聚聚丙烯,购自金发科技公司,其熔融指数MFI在230℃/2.16kg下,为1500g/10min,
熔喷无纺布用聚丙烯,购自金发科技公司,其熔融指数MFI在230℃/2.16kg下,为1500g/10min;
均聚聚丙烯,购自金发科技公司,其熔融指数MFI在230℃/2.16kg下,为1000g/10min,
纳米电气石粉,购自天津鸿雁天山石业纳米技术有限公司;
纳米POSS粉,购自阿拉丁,型号为八乙烯基-POSS;
纳米二氧化硅,购自广州吉必胜科技实业有限公司;
硬脂酸锌购自江西宏远;
马来酸酐接枝POE购自美国杜邦;
对叔丁基苯甲酸铝购自金锦乐化学;
芥酸酰胺购自英国禾大油脂化学品公司;
硅酮购自陶熙道康宁;
抗氧剂1010及抗氧剂168均购自BASF。
实施例1~2及对比例1~4
按照表1配方将材料投到高速混合机混合,并通过长径比为40:1的双螺杆挤出机熔融共混挤出,熔融段温度150~210℃,得到口罩用熔喷无纺布用驻极母粒。
表1
Figure PCTCN2020129278-appb-000001
测试例1:过滤效率及阻力测试
将上述实施例1~2及对比例1~4制备的口罩用熔喷无纺布用驻极母粒与熔喷无纺布用聚丙烯(熔指1500g/10min)混合,其中所述口罩用熔喷无纺布用驻极母粒与熔喷无纺布用聚丙烯的重量比为1:49。将所得的混合物经过单螺杆熔融,经计量泵计量后通过喷丝板喷出形成纤维。所述纤维经过230~270℃的热风牵引,形成测试样品。测试样品再经过30kV电压驻极处理后再收卷,得到样品熔喷无纺布材料。
该口罩用熔喷无纺布材料使用TSI8130自动滤料测试仪测试,使用GB19083-2010《医用防护口罩技术要求》标准,介质采用数量中值粒径0.075±0.02μm的NaCl颗粒,测试流量85L/min,进行过滤效率及吸气阻力测试。结果如表2所示。
作为医用防护口罩的标准,过滤效率要求在95%以上,吸气阻力要求在343.2Pa以下,对于实际应用来说,一般高于200Pa以上会导致呼吸有困难,个人使用时为了最求舒适感,阻力越低舒适感越好,因此需要开发在保持高过滤效率的同时低阻力的无纺布材料。
从对比例1可以看出,当不加入成核剂和柔软剂时,产品的吸气阻力仍较高。 从对比例2可以看出,当仅加入成核剂时,产品的阻力略有下降,且其滤效也略微上升,但并不显著。从对比例3可以看出,硅酮作为柔软剂添加至本体系中,会对驻极效果带来负面影响,导致过滤效率下降,无法满足医用防护口罩GB 19083-2010《医用防护口罩技术要求》标准的过滤性能。有报道称碳原子数为6~20的脂肪酸或其盐(硬脂酸锌)等物质可以作为驻极剂,但对比例4可以看出,本体系中,如果不加入电气石粉等传统驻极剂,过滤效果也是无法达到要求的。
表2
样品 过滤效率% 吸气阻力Pa
实施例1 97.9 115
实施例2 96.0 112
对比例1 96.3 150
对比例2 96.8 142
对比例3 90.2 120
对比例4 79.4 106
实施例3~8和对比例5
按照表3配方将材料投到高速混合机混合,并通过长径比为48:1的双螺杆挤出机熔融共混挤出,熔融段温度150~210℃,得到口罩用熔喷无纺布用驻极母粒。
表3
Figure PCTCN2020129278-appb-000002
Figure PCTCN2020129278-appb-000003
测试例2:过滤效率及阻力测试
将上述实施例3~8、对比例5制备的口罩用熔喷无纺布用驻极母粒与熔喷无纺布用聚丙烯(熔指1500g/10min)混合,其中所述口罩用熔喷无纺布用驻极母粒与熔喷无纺布用聚丙烯的重量比为1:49。将所得的混合物经过单螺杆熔融,经计量泵计量后通过喷丝板喷出形成纤维。所述纤维经过230~270℃的热风牵引,形成测试样品。测试样品再经过30kV电压驻极处理后再收卷,得到样品熔喷无纺布材料。
该口罩用熔喷无纺布材料使用TSI8130自动滤料测试仪测试,使用GB19083-2010《医用防护口罩技术要求》标准,介质采用数量中值粒径0.075±0.02μm的NaCl颗粒,测试流量85L/min,进行过滤效率测试;同时进行吸气阻力测试。结果如表4所示。
表4
样品 过滤效率% 吸气阻力Pa
实施例3 97.9 113
实施例4 91.2 115
实施例5 95.2 114
实施例6 90.6 110
实施例7 90.1 112
实施例8 91.0 108
对比例5 82.1 115
从实施例4、6~8可以看出,当母粒的聚丙烯采用熔指为1000g/10min的均聚聚丙烯时,无纺布的过滤效率也受到明显的影响,不再满足KN95的过滤要求,但仍能满足普通口罩(90%)的过滤要求。从对比例5与实施例4比较可以看出, 以硅酮作为柔软剂添加至本体系中,会对驻极效果带来负面影响,导致过滤效率下降,无法满足标准下的过滤性能要求。

Claims (10)

  1. 一种低阻力口罩用熔喷无纺布用驻极母粒,其特征在于,由如下按重量百分数计算的组分制成:
    聚丙烯树脂65~85%;
    驻极粉1~3%;
    分散剂5~15%;
    成核剂3~10%;
    柔软剂3~10%;
    加工助剂0.05~0.5%;
    所述柔软剂为芥酸酰胺;
    所述聚丙烯树脂为均聚聚丙烯和/或共聚聚丙烯,其熔融指数MFI在230℃/2.16kg下,不低于1000g/10min。
  2. 根据权利要求1所述低阻力口罩用熔喷无纺布用驻极母粒,其特征在于,所述聚丙烯树脂的熔融指数MFI在230℃/2.16kg下,为1000~1500g/10min。
  3. 根据权利要求1所述低阻力口罩用熔喷无纺布用驻极母粒,其特征在于,所述驻极粉为纳米电气石粉、纳米二氧化硅、纳米聚倍半硅氧烷粉中一种或几种。
  4. 根据权利要求1所述低阻力口罩用熔喷无纺布用驻极母粒,其特征在于,所述驻极粉为纳米电气石粉。
  5. 根据权利要求1所述低阻力口罩用熔喷无纺布用驻极母粒,其特征在于,所述分散剂为聚乙烯蜡、脂肪酸盐、马来酸酐接枝聚丙烯、马来酸酐接枝聚乙烯、马来酸酐接枝POE、甲基丙烯酸缩水甘油酯接枝聚丙烯、甲基丙烯酸缩水甘油酯接枝POE、甲基丙烯酸缩水甘油酯接枝EPDM中任意一种或几种。
  6. 根据权利要求1所述低阻力口罩用熔喷无纺布用驻极母粒,其特征在于,所述成核剂为羧酸盐类成核剂、磷酸盐类成核剂或山梨醇类成核剂。
  7. 根据权利要求1所述低阻力口罩用熔喷无纺布用驻极母粒,其特征在于,所述加工助剂为抗氧剂、抗老化剂中的一种或几种。
  8. 权利要求1至7任一项所述低阻力口罩用熔喷无纺布用驻极母粒的制备方法,其特征在于,将所述组分通过混合机进行预混合,然后用双螺杆挤出机进行熔融共混挤出并造粒得到,工艺温度在130~220℃。
  9. 根据权利要求8所述制备方法,其特征在于,所述双螺杆挤出机的螺杆长径 比大于等于40:1。
  10. 一种低阻力口罩用熔喷无纺布,其特征在于,包含权利要求1至7任一项所述低阻力口罩用熔喷无纺布用驻极母粒及熔喷无纺布用聚丙烯,低阻力口罩用熔喷无纺布用驻极母粒与熔喷无纺布用聚丙烯的重量比为1:(19~49)。
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