CN115819931A - Biodegradable melt-blown non-woven fabric material and preparation method and application thereof - Google Patents
Biodegradable melt-blown non-woven fabric material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a biodegradable melt-blown non-woven fabric material, a preparation method and application thereof, wherein the biodegradable melt-blown non-woven fabric material comprises the following components: biodegradable resin, polylactic acid, a compatilizer, a lubricant, a chain extender and an antioxidant. The preparation process of the material comprises the following steps: the raw materials of the components are uniformly mixed according to a proportion, and are subjected to twin-screw blending granulation to obtain biodegradable slices, and the biodegradable melt-blown non-woven fabric is obtained through melt-blown non-woven process processing. The degradable melt-blown non-woven material provided by the invention has a biodegradable function, excellent filtering performance, air permeability and mechanical property, and hydrophilicity, and is more suitable for being applied to the fields of air filtration, adsorbing materials, mask materials, wiping cloth, various packing materials, medical sanitary materials and the like.
Description
Technical Field
The invention belongs to the field of application of high polymer materials, relates to a biodegradable melt-blown non-woven fabric material, and a preparation method and application thereof, and particularly relates to a processing method for popularization and application of a blended biodegradable material in the field of melt-blown non-woven materials.
Background
The melt-blown non-woven fabric is a non-woven fabric made of polypropylene as a raw material by directly preparing a polymer into a net shape by a melt-blowing method. Because the melt-blown method processing technology utilizes hot air for blowing, and does not have a long drafting channel, the melt-blown method non-woven technology has a short process flow, is known as a one-step polymer direct web formation method with the shortest process flow, and has the advantages of high yield, low cost, high efficiency, no solvent, wide application, more raw material sources and the like. The melt-blown non-woven fabric has the greatest characteristics of very fine fiber, diameter of only a few micrometers, fluffy structure after self bonding, high porosity, small average pore size, and very good application characteristics of filterability, shielding property, heat insulation property, oil absorption property and the like. Therefore, the melt-blown nonwoven fabric is widely used in the fields of medical and industrial masks, heat insulating materials, filter materials, medical and sanitary materials, oil absorbing materials, wiping cloths, battery separators, sound insulating materials, and the like.
At this stage, the following problems mainly exist in the improvement of polypropylene melt-blown nonwoven materials:
firstly, with the rapid development of industry and the increasing huge market of melt-blown non-woven fabrics, the melt-blown non-woven materials bring great convenience to the life of people and also bring threat to the living environment of human beings. The waste of polypropylene melt-blown nonwoven materials generates harmful gases by incineration, and is difficult to degrade if buried, which causes serious environmental pollution problems. This is a rather alarming and demanding problem to solve. In order to solve the problem, chinese patent CN103073868B discloses a biodegradable melt-blown non-woven fabric slice and a preparation method thereof, wherein polypropylene carbonate and polypropylene melt-blown non-woven fabric slice are melt-blended to prepare the biodegradable melt-blown non-woven fabric slice with excellent performance. Although its mechanical and thermal properties are excellent, it does not mention the specific properties of the resulting melt-blown nonwoven fabric, and its degradability is yet to be improved due to the presence of polypropylene.
Secondly, the polypropylene melt-blown non-woven fabric has the problems of insufficient strength, small elongation at break and the like, and the main performance is that the fabric surface feels hard, so that the subsequent processing and use are limited. Chinese patent CN105086394B and Chinese patent CN107227555A both add modified nano inorganic substance into the material to carry out inorganic toughening on the melt-blown non-woven material, thereby improving the mechanical property. However, the surface modification process of the nano inorganic substance is complicated and consumes a large amount of solvent, the nano inorganic substance is easy to agglomerate in the blending process, and the inorganic particles are easy to block a filter screen and a spray head in the melt-blowing process. For example, chinese patent CN105086394B discloses a SiO 2-containing biodegradable composite material for melt-blown nonwoven fabric and a preparation method thereof, wherein SiO2 particles are added to biodegradable resin by nano-composite modification technology, so as to improve the filtration efficiency and mechanical properties of the biodegradable melt-blown nonwoven fabric. However, the problem of incompatibility among several biodegradable resins is not solved, the content of PLA is high, nano SiO2 particles are easy to agglomerate in the blending granulation process, a large amount of alcohol-water solvent is needed, surface chemical modification is needed to be carried out on the nano SiO2 particles, and the like, the process is complex and complex, the yield is low, a large amount of resource waste and energy consumption are caused, and the environment is not friendly.
Thirdly, the biodegradable material has less application research in melt-blowing, and chinese patent CN102295825A discloses a biodegradable composition and a preparation method thereof, the disclosed biodegradable composition consists of biodegradable homopolyester (a), biodegradable copolyester (B) and chain extender (C), the total weight of the biodegradable composition is 100 parts by mass, the biodegradable copolyester (a + B) is 95.0-99.9 parts and the biodegradable copolyester (B) is 0.1-5.0 parts, wherein the ratio of a to B is 1. The method is mainly designed for solving the problems of unstable degradation speed, narrow application of processing physical properties, poor humidity resistance, hydrolysis resistance, oxidation resistance and the like of the biodegradable material, and finally obtains the material with moderate biodegradation speed and good physical processing properties, wherein the main evaluation indexes are mechanical tensile property, mechanical retention rate and biodegradation speed. The material is mainly applied to the fields of blow molding, extrusion molding, injection molding, spinning molding and the like, but the application condition and the application prospect in the field of melt-blown non-woven fabric are not mentioned. The invention obviously does not solve the problem of incompatibility between different biodegradable materials and is not related to the technical problem intended to be solved by the invention and the technical effect obtained.
Fourth, when the melt-blown nonwoven fabric is used as a filter material, the filter performance and the mechanical properties of the melt-blown nonwoven fabric are concerned, and in terms of the prior art, the melt-blown nonwoven fabric needs to obtain higher filter efficiency and better air permeability, various inorganic or organic electrets are inevitably added, and the action of tens of thousands of volts of static electrets is added, so that the cost is high and the energy consumption is huge in the actual production process. For example, chinese patent CN104711764B discloses a high-strength long-acting electret superfine fiber PLA melt-blown nonwoven material and a preparation method thereof, which blends PLA chips and nanoparticle additives, and prepares a degradable melt-blown nonwoven material with good mechanical properties and long-acting electret function through an improved melt-blowing processing process. However, the mechanical properties of the PLA melt-blown non-woven fabric with high gram weight prepared by the method are not very excellent, the comprehensive properties are still to be further improved, and the production cost of the method is very high.
Disclosure of Invention
The invention aims to provide a biodegradable melt-blown non-woven fabric material which is suitable for melt-blown process processing, and the prepared non-woven fabric has a biodegradable function, excellent filtering performance, air permeability and mechanical property and hydrophilicity.
The other purpose of the invention is to provide a preparation method of the biodegradable melt-blown non-woven fabric material.
The invention also aims to provide application of the biodegradable melt-blown non-woven fabric material.
In conclusion, the technical problem to be solved by the technical scheme is to provide a biodegradable melt-blown nonwoven material, which has different filtering performance, air permeability and mechanical property, reduces the production cost and can be widely applied to the field of nonwovens.
The purpose of the invention can be realized by the following technical scheme:
a biodegradable meltblown nonwoven material comprising the following components:
preferably, the method comprises the following steps: the material comprises the following components:
the technical scheme of the invention is as follows: the biodegradable resin is at least one of PBAT, PBST, PBSA and PBS.
Preferably, the method comprises the following steps: the melt index of the biodegradable resin is 100-500g/10min at 210 ℃ and 2.16 kg.
Further: the melt index of the biodegradable resin is 300-500g/10min at 210 ℃ and 2.16 kg.
Most preferably: the biodegradable resin is characterized in that PBAT produced by characterization chemical fibers and/or PBS produced by characterization chemical fibers.
The technical scheme of the invention is as follows: the melt index of the polylactic acid is 80-400g/10min under the conditions of 250 ℃ and 2.16 kg.
And further: the melt index of the polylactic acid is 50-400g/10min under the conditions of 250 ℃ and 2.16 kg; the molecular weight of the polylactic acid is between 10 and 13 ten thousand, and the melting point is between 160 and 170 ℃.
Most preferably: the polylactic acid is PLA-L105 of Suzhou Lvbo degradation materials.
The technical scheme of the invention is as follows: the compatilizer is at least one of maleic anhydride, benzoyl peroxide, tetrabutyl titanate and polybasic acid; the lubricant is at least one selected from zinc stearate, calcium stearate and magnesium stearate; the chain extender is at least one selected from ADR4370S and KL-E4370; the antioxidant is at least one of antioxidant 168 and antioxidant 1010.
In some preferred embodiments: the lubricant is prepared by mixing at least one of zinc stearate, calcium stearate and magnesium stearate with one of chain extenders ADR4370S and KL-E4370 in a ratio of 1:0.5 to 1.5; the antioxidant is antioxidant 168 and antioxidant 1010, and the weight ratio of the antioxidant to the antioxidant is 1:0.5 to 1.5.
In some most preferred embodiments: the lubricant is prepared by mixing at least one of zinc stearate, calcium stearate and magnesium stearate with one of chain extenders ADR4370S and KL-E4370 in a ratio of (1): 1, mixing; the antioxidant is antioxidant 168 and antioxidant 1010, and the weight ratio of the antioxidant to the antioxidant is 1:1 and mixing.
The invention also aims to provide a preparation method of the biodegradable melt-blown non-woven fabric material, which comprises the steps of pretreating and uniformly stirring components including biodegradable resin, polylactic acid (PLA), compatilizer, lubricant, antioxidant and the like to obtain a mixed material, carrying out double-screw granulation and melt-blowing process processing on the mixed material,
a preparation method of the biodegradable melt-blown non-woven fabric material comprises the following steps: the method comprises the following steps:
s1, preparing a mixed material:
s11, stirring and uniformly mixing the dried biodegradable resin, the polylactic acid, the compatilizer, the lubricant, the chain extender and the antioxidant in a high-speed mixer according to a formula ratio to obtain a mixed material;
s2, carrying out double-screw granulation on the mixed material:
melting, extruding, air cooling, bracing and cold cutting the mixed materials to prepare biodegradable resin/PLA blending biodegradable slices;
s3, preparing the melt-blown non-woven fabric by the biodegradable resin/PLA blending biodegradable slice:
s31, drying the prepared biodegradable resin/PLA blending biodegradable slice at 70-90 ℃ for 6-24h;
s32, melt-blowing process processing: adding dried biodegradable resin/PLA blending biodegradable slices into an automatic bin of a melt-blowing device, feeding the slices into a screw extruder, heating and melting the slices, flowing into a prefilter, filtering out impurities in a melt, flowing to a metering pump, extruding the melt to a small hole opening of a spinneret die head by virtue of the pressure of the metering pump, wherein the diameter of a spinneret hole is 0.2-0.5mm, carrying out hot-air high-speed drafting on the melt extruded from the spinneret plate by high-speed hot compressed air on two sides of the small hole, carrying out short-time cooling and crystallization on the obtained melt-blown superfine fiber under the action of side-blown cold air, and gathering the fiber on a web-forming curtain with the distance DCD from the die head of 160-250mm, wherein: the suction wind speed under the net is 1000-3000rpm; meanwhile, the operation speed of the rotary screen is 3-10m/min, and the superfine fiber melt-blown non-woven fabric with good mechanical property is formed by rolling at the speed of 3-10 m/min;
s33, the obtained non-woven fabric does not need to be subjected to electret treatment through an electrode device, energy consumption is greatly saved, and finally, a finished product of the melt-blown non-woven material is obtained through coiling on a lap former and online slitting.
In some specific embodiments, the method comprises the steps of:
s1, preparing a mixed material:
s11, stirring and uniformly mixing the dried biodegradable resin, the polylactic acid, the compatilizer, the lubricant, the chain extender and the antioxidant in a high-speed mixer according to a formula ratio to obtain a mixed material;
s2, carrying out double-screw granulation on the mixed material:
the double-screw granulation process comprises the following steps: adding the obtained mixture into a storage bin, and continuously stirring, wherein the temperature of a granulation screw is 180-230 ℃, the rotating speed of the screw is 200-300r/min, and the rotating speed of a metering pump is 100-300Kg/h; extruding, air cooling, bracing and cold cutting the mixed material to prepare biodegradable resin/PLA blending biodegradable slices;
s3, preparing the melt-blown non-woven fabric by the biodegradable resin/PLA blending biodegradable slice:
s31, drying the prepared biodegradable resin/PLA blending biodegradable slice at 70-90 ℃ for 6-24h;
s32, melt-blowing process processing: adding dried biodegradable resin/PLA blending biodegradable slices into an automatic bin of a melt-blowing device, feeding the slices into a screw extruder, heating and melting the slices, flowing into a prefilter, filtering out impurities in a melt, flowing to a metering pump, extruding the melt to a small hole opening of a spinneret die head by virtue of the pressure of the metering pump, wherein the diameter of a spinneret hole is 0.2-0.5mm, carrying out hot-air high-speed drafting on the melt extruded from the spinneret plate by high-speed hot compressed air on two sides of the small hole, carrying out short-time cooling and crystallization on the obtained melt-blown superfine fiber under the action of side-blown cold air, and gathering the fiber on a web-forming curtain with the distance DCD from the die head of 160-250mm, wherein: the suction wind speed under the net is 1000-3000rpm; meanwhile, the operation speed of the rotary screen is 3-10m/min, and the rotary screen is wound at the speed of 3-10m/min to form the superfine fiber melt-blown non-woven fabric with good mechanical property;
s33, the obtained non-woven fabric does not need to be subjected to electret treatment through an electrode device, energy consumption is greatly saved, and finally, a finished product of the melt-blown non-woven material is obtained through coiling on a lap former and online slitting.
In some specific embodiments: in S32, the parameters are set as follows:
the preparation method of the invention specifically adjusts the following melt-blown process parameters, and obtains a finer and more uniform fiber structure through matching and adjustment of the melt-blown process parameters, thereby improving the filtering performance of the melt-blown non-woven material. According to the properties of different materials, the invention adjusts the technological parameters such as the temperature of the screw rod, the temperature of the die head, the DCD, the air temperature and the air speed at the outlet of the air heater, the speed of the side blowing fan, the suction and suction speed under the net, the speed of the circular net and the like.
The function description of each component in the formula of the invention is as follows:
first, biodegradable resins are chemically stable, generally with deeper traps and stronger ability to capture and store charges due to their structural relationship, and are themselves better electrets. Because the biodegradable resin is slower in crystallization, a charge trap source can be continuously formed in the crystallization process, and the charge trapping stability is better along with the perfection of the crystal grain structure. The biodegradable resin with the melt index of 300-500g/10min has better fluidity, is more beneficial to obtaining thinner fibers under the melt-blowing process, and the formed melt-blown superfine fiber porous structure can form a charge trapping space to obtain the melt-blown non-woven material with high filtration efficiency. The biodegradable resin has good mechanical property, and the melt-blown non-woven material with good mechanical property, soft hand feeling and good hydrophilicity can be obtained.
Secondly, PLA is an amorphous substance, PLA with a melt index of 50-400g/10min is selected to be compounded with biodegradable resin to obtain biodegradable materials with different proportions, crystalline and amorphous mixed fibers are obtained through a melt-blowing process, charges are accumulated on the interface of a crystalline area and an amorphous area, and the charges are reserved in the fibers with three-dimensional aggregation and high porosity, so that the biodegradable melt-blown fabric material with excellent filtering performance is obtained. And the PLA has poor mechanical property, and the melt-blown non-woven material with excellent filtering property and mechanical property and soft hand feeling is obtained through the proportion of the biodegradable resin, the PLA and the additive.
Thirdly, the compatilizer can solve the problem that the biodegradable resin and the PLA are incompatible, and avoids the phenomena of discontinuous and uneven fibers in the melt-blown process, thereby improving the filtration efficiency of the melt-blown non-woven material and improving the mechanical property.
And fourthly, the stearate is used as an auxiliary agent to promote the crystallization of the material, improve the crystallinity and the alpha crystal form proportion of the material, increase the grain size, effectively improve the flow property of the material, and have obvious effect along with the increase of the concentration, thereby improving the filtering efficiency and the electricity storage property of the material. The addition of a proper amount of chain extender ADR4370S or KL-E4370 not only plays a role of a lubricating and nucleating agent, but also can interact with biodegradable resin and PLA, so that the compatibility and mechanical property of a blending system of the biodegradable resin and the PLA are obviously improved.
Fifth, the antioxidant is mainly used for preventing PLA from being decomposed by heat so as not to reduce the physical properties of the material.
The invention is distinguished from the most recent prior art:
firstly, the formula of the degradable melt-blown non-woven material provided by the invention is different from the prior art, the biodegradable function of the melt-blown non-woven material is endowed by blending the biodegradable material and PLA, and the polylactic acid accounts for 10-40% of the mixture. The material with uniform melt and good fluidity is prepared by compounding the compatilizer, the lubricant and the antioxidant, the filtration efficiency and the charge storage capacity of the melt-blown non-woven material are improved, the hand feeling and the mechanical property of the material are improved, the medical protective property of the material is enhanced, and the application field of the material is widened under the condition that an electret is not additionally added. The method has the advantages of simple equipment, short process flow, low energy consumption and no solvent.
Secondly, the preparation method of the degradable melt-blown non-woven material is different from the prior art, and the processing mode that the melt-blown non-woven material can obtain excellent filtering efficiency and lower ventilation resistance without adding an electret additionally or using an electrostatic electret is not seen in the prior art.
Thirdly, the degradable melt-blown non-woven material provided by the invention has a biodegradable function, excellent filtering performance, air permeability and mechanical property, and hydrophilicity, and is more suitable for being applied to the fields of air filtration, adsorbing materials, mask materials, wiping cloth, various packing materials, medical sanitary materials and the like.
The invention has the beneficial effects that:
the degradable melt-blown non-woven material prepared by the invention has the advantages of excellent filtering performance, small ventilation resistance, excellent mechanical property and hydrophilicity under the conditions of not additionally adding an electret and not using an electrostatic electret.
Drawings
FIG. 1 is a scanning electron micrograph of the product of example 2 of the present invention, the fiber mean diameter (. Mu.m)/standard deviation 2.01/0.98.
FIG. 2 is a scanning electron micrograph of a comparative example 1 product of the present invention, the fiber mean diameter (. Mu.m)/standard deviation 2.43/1.42.
FIG. 3 is a scanning electron micrograph of a comparative example 2 product of the present invention, the fiber mean diameter (. Mu.m)/standard deviation 8.6/12.7.
FIG. 4 is a scanning electron micrograph of a comparative example 3 product of the present invention, which shows a fiber average diameter (. Mu.m)/standard deviation of 3.01/23.2.
FIG. 5 is a sectional view of a cut sheet of products of comparative examples 1 to 2 and examples of the present invention.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
the degradable melt-blown nonwoven material of the invention was tested according to the following criteria:
tensile strength: GB/T1040-2006.
Gram weight: FZ/T64078-2019.
Filtration resistance: FZ/T64078-2019, test substance NaCl, particle size 0.3 μm, test flow rate 32L/min.
The filtration efficiency is as follows: FZ/T64078-2019, test substance NaCl, particle size 0.3 μm, test flow rate 32L/min.
Average fiber diameter: the average diameter of 30 fibers was measured by scanning electron microscopy.
Raw materials used in examples and comparative examples:
polypropylene (PP): shandong Doran polymers, inc. Z-1500.
Polylactic acid (PLA): suzhou Lubo degradable materials Co., ltd PLA-L105.
Biodegradable resin: PBAT, PBS, characterization of chemical fiber production.
Electret: tourmaline powder, commercially available.
A compatilizer: maleic anhydride, characterization of chemical fiber production.
Lubricant: magnesium stearate, commercially available; ADR4370S, produced by Pasteur.
Antioxidant: antioxidant 168 and antioxidant 1010, commercially available
Example 1:
the materials and the components are prepared according to the mixture ratio of the table 1, and the following steps are carried out:
s1, preparing a mixed material:
s11, drying the biodegradable resin PBAT at 80 ℃ for 14h, and drying the PLA at 110 ℃ for 14h to obtain a dried biodegradable material;
s12, stirring and uniformly mixing the biodegradable resin, the polylactic acid, the compatilizer, the lubricant, the chain extender and the antioxidant in a high-speed mixer according to a formula ratio to obtain a mixed material;
s2, carrying out double-screw granulation on the mixed material:
the double-screw granulation process comprises the following steps: the obtained mixture is added into a feed bin and is continuously stirred, the temperature of a granulation screw is 195 ℃ in a 1 region, 210 ℃ in a 2 region, 230 ℃ in a 3-9 region, 210 ℃ in a 10 region, the rotating speed of the screw is 250r/min, and the rotating speed of a metering pump is 150Kg/h. The mixed materials are extruded, air-cooled, pulled and cold cut to prepare the biodegradable PBAT/PLA blending biodegradable slice.
S3, preparing the biodegradable PBAT/PLA blending slice to prepare the melt-blown non-woven fabric:
s31, drying the prepared biodegradable PBAT/PLA blending slice at 85 ℃ for 12h.
S32, melt-blowing process processing: adding dried biodegradable PBAT/PLA blended slices into an automatic bin of a melt-blowing device, feeding the slices into a screw extruder, heating and melting, wherein the screw temperature is 180 ℃ in a 1 region, 200 ℃ in a 2 region, 230 ℃ in a 3 region and 245 ℃ in a 4-7 region, then enabling the melt to flow into a prefilter, filtering impurities in the melt, enabling the melt to flow into a metering pump, the flow of the metering pump is 6rpm, enabling the melt to be extruded out to a small hole opening of a spinning die head by the aid of the pressure of the metering pump (the die head temperature is 245 ℃), the diameter of a spinning hole is 0.28mm, carrying out hot air high-speed drafting on the melt extruded from a spinneret plate by high-speed hot compressed air (240 ℃) on two sides of the small hole to obtain melt-blown superfine fibers, carrying out short-time cooling crystallization on the fibers, the speed of a side blowing fan is 2100rpm, the speed of a suction fan below a net is 2700rpm, the fibers are gathered on a net curtain, the receiving distance DCD is 190mm, and the speed of a circular net is 4m/mim, and forming the melt-blown superfine fiber non-woven fabric with good mechanical property.
And S33, coiling the obtained non-woven fabric on a coiling machine, and performing online slitting to obtain a melt-blown non-woven material finished product.
The biodegradable melt-blown nonwoven fabric obtained has the test results of gram weight, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and average fiber diameter, which are shown in table 3.
Example 2:
the materials and components were prepared according to the formulation of table 1, the conditions of the preparation method being the same as example 1 except that in the step S32: the screw temperature was 180 ℃ in the 1 zone, 200 ℃ in the 2 zone, 230 ℃ in the 3 zone, 250 ℃ in the 4-7 zone, the temperature of the hot air drawn was 245 ℃, the speed of the side blowing fan was 1900rpm, the speed of the suction fan under the wire was 2600rpm, and the speed of the cylinder was 6m/mim.
The biodegradable meltblown nonwoven (see fig. 1) obtained had the grammage, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and fiber mean diameter test results shown in table 3.
Example 3:
the materials and components were prepared according to the formulation of table 1, the conditions of the preparation method being the same as example 1 except that in the step S32: the screw temperature was 180 ℃ in the 1 zone, 200 ℃ in the 2 zone, 230 ℃ in the 3 zone, 255 ℃ in the 4-7 zone, the temperature of the hot air for drawing was 250 ℃, the speed of the side blowing fan was 1800rpm, the speed of the suction fan under the wire was 2400rpm, and the speed of the rotary screen was 8m/mim.
The biodegradable melt-blown nonwoven fabric obtained has the test results of gram weight, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and average fiber diameter, which are shown in table 3.
Example 4:
the materials and components were prepared according to the formulation of table 1, the conditions of the preparation method being the same as example 1 except that in the step S32: the side-blowing fan speed was 1800rpm, the under-wire suction fan speed was 2400rpm, and the cylinder speed was 6m/mim.
The biodegradable melt-blown nonwoven fabric obtained has the test results of gram weight, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and average fiber diameter, which are shown in table 3.
Example 5:
the materials and components were prepared according to the formulation of table 1, the conditions of the preparation method being the same as example 1 except that in the step S32: the screw temperature was 180 ℃ in zone 1, 200 ℃ in zone 2, 230 ℃ in zone 3, 250 ℃ in zone 4-7, the temperature of the hot air drawn was 245 ℃, the speed of the side blowing fan was 1800rpm, the speed of the suction fan under the wire was 2500rpm, and the speed of the cylinder was 6m/mim.
The biodegradable melt-blown nonwoven fabric obtained has the test results of gram weight, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and average fiber diameter, which are shown in table 3.
Comparative example 1:
the materials and the components are prepared according to the mixture ratio shown in the table 2, and the following steps are carried out:
s1, preparing a mixed material:
s11, stirring and uniformly mixing polypropylene PP, electret tourmaline powder, magnesium stearate and an antioxidant in a high-speed mixer according to a formula ratio to obtain a mixed material;
s2, preparing the melt-blown non-woven fabric from the mixed material:
s21, processing by a melt-blowing process: the same conditions as in example 2;
s22, the nonwoven fabric obtained in the step is subjected to electret treatment by a string wire-drum type linear electrode device, and the voltage of the electrode is 30kV, so that the melt-blown nonwoven fabric is obtained.
And S23, coiling the obtained non-woven fabric on a coiling machine, and performing online slitting to obtain a melt-blown non-woven material finished product.
The resulting polypropylene meltblown nonwoven (see fig. 2) has the grammage, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and fiber average diameter test results shown in table 3.
Comparative example 2:
the materials and the components are prepared according to the mixture ratio of the table 2, and the following steps are carried out:
s1, drying the biodegradable resin PBAT at 80 ℃ for 14h to obtain a dried biodegradable material;
s2, melt-blown process processing: adding the materials into an automatic storage bin of a melt-blowing device, feeding the materials into a screw extruder, heating and melting, wherein the temperature of a screw is 180 ℃ in a 1 region, 200 ℃ in a 2 region, 230 ℃ in a 3 region and 245 ℃ in a 4-7 region, the melt flows into a prefilter, impurities in the melt are filtered, the melt flows to a metering pump, the flow of the metering pump is 6rpm, the melt is extruded to a small hole of a spinneret die head by the pressure of the metering pump, the diameter of a spinneret hole is 0.28mm, the melt extruded from a spinneret plate is subjected to hot air high-speed drafting by high-speed hot compressed air on two sides of the small hole, the temperature of the drafting hot air is 230 ℃, superfine fibers are obtained, the fibers are subjected to melt-blowing and crystallization in a short time, the speed of a side blowing fan is 2300rpm, the speed of a suction fan under a screen is 2500rpm, the fibers are gathered on a screen forming curtain, the receiving distance DCD is 190mm, and the speed of a rotary screen is 4m/mim, and the melt-blown non-woven fabric is formed.
And S3, coiling the obtained non-woven fabric on a coiling machine, and cutting on line to obtain a finished melt-blown non-woven material.
The biodegradable meltblown nonwoven (see fig. 3) obtained had the grammage, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and fiber mean diameter test results shown in table 3.
In addition: this comparative example would not produce a conventional meltblown nonwoven material if the process parameters were the same as those used in the examples.
Comparative example 3:
the materials and the components are prepared according to the mixture ratio of the table 2, and the following steps are carried out:
s1, drying PLA at 110 ℃ for 14h to obtain a dried biodegradable material;
s2, melt-blown process processing: the same conditions as in example 2;
and S3, coiling the obtained non-woven fabric on a coiling machine, and performing online slitting to obtain a melt-blown non-woven material finished product.
The biodegradable melt-blown nonwoven fabric obtained has the test results of gram weight, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break and average fiber diameter, which are shown in table 3.
Comparative example 4:
the materials and the components are prepared according to the mixture ratio of the table 2, and the following steps are carried out:
s1, preparing a mixed material:
s11, drying the biodegradable resin PBAT at 80 ℃ for 14h, and drying the PLA at 110 ℃ for 14h to obtain a dried biodegradable material;
s12, stirring and uniformly mixing the biodegradable resin PBAT, the PLA and the antioxidant in a high-speed mixer according to a formula ratio to obtain a mixed material;
s2, carrying out double-screw granulation on the mixed material: the same conditions as in example 2;
s3, preparing the biodegradable PBAT/PLA blending slice to prepare the melt-blown non-woven fabric: the same conditions as in example 2;
and S33, coiling the obtained non-woven fabric on a coiling machine, and performing online slitting to obtain a melt-blown non-woven material finished product.
The resulting biodegradable meltblown nonwoven (see fig. 4) had the grammage, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break, and fiber average diameter test results shown in table 3.
Comparative example 5:
the materials and the components are prepared according to the mixture ratio of the table 1, and the following steps are carried out:
s1, preparing a mixed material, and performing the same operation as in example 1;
s2, carrying out double-screw granulation on the mixed material, and carrying out granulation in the same way as in example 1; .
S3, preparing the biodegradable PBAT/PLA blending slice to prepare the melt-blown non-woven fabric:
s31, drying the prepared biodegradable PBAT/PLA blending slice at 85 ℃ for 12h.
S32, melt-blowing process processing: adding dried biodegradable PBAT/PLA blended slices into an automatic bin of a melt-blowing device, feeding the slices into a screw extruder, heating and melting, wherein the temperature of a screw is 1 region 170 ℃,2 region 190 ℃,3 region 220 ℃, and 4-7 region 235 ℃, then the melt flows into a prefilter, filtering impurities in the melt, then flows into a metering pump, the flow of the metering pump is 8rpm, the melt is extruded out to a small hole of a spinning die head (die head temperature 230 ℃) by virtue of the pressure of the metering pump, the diameter of the spinning hole is 0.28mm, high-speed hot compressed air (245 ℃) on two sides of the small hole carries out hot air high-speed drafting on the melt extruded from the spinning plate to obtain melt-blown superfine fibers, cooling and crystallizing the fibers for a short time, the speed of a side blowing fan is 1600rpm, the speed of a suction fan under a net is 2100rpm, the fibers are gathered on a net forming curtain, the receiving distance DCD is 160mm, and the speed of a circular net is 6m/mim, and thus forming the superfine fiber non-woven fabric with good mechanical properties.
And S33, coiling the obtained non-woven fabric on a coiling machine, and performing online slitting to obtain a melt-blown non-woven material finished product.
The resulting biodegradable meltblown nonwoven fabric was tested for grammage, filtration resistance, filtration efficiency, tensile strength, tensile elongation at break, and fiber average diameter, see table 3.
TABLE 1 examples and component proportions and melt blown Process scenarios
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Biodegradable resin | 90(PBAT) | 75(PBAT) | 60(PBAT) | 90(PBS) | 75(PBS) |
| Polylactic acid (PLA) | 10 | 25 | 40 | 10 | 25 |
| Polypropylene PP | 0 | 0 | 0 | 0 | 0 |
| Tourmaline powder | 0 | 0 | 0 | 0 | 0 |
| Compatilizer (maleic anhydride) | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Lubricant (magnesium stearate) | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Chain extender (ADR 4370S) | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Antioxidant 168 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Antioxidant 1010 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Electrostatic electret (kV) | 0 | 0 | 0 | 0 | 0 |
Table 2 comparative example composition ratio of components and melt blown process conditions
| Item | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 |
| Biodegradable resin | 0 | 100(PBAT) | 0 | 75(PBAT) | 90(PBAT) |
| Polylactic acid (PLA) | 0 | 0 | 100 | 25 | 10 |
| Polypropylene PP | 97 | 0 | 0 | 0 | 0 |
| Tourmaline powder | 2 | 0 | 0 | 0 | 0 |
| Maleic anhydride | 0 | 0 | 0 | 0 | 0.2 |
| Magnesium stearate | 1 | 0 | 0 | 0 | 0.1 |
| ADR4370S | 0 | 0 | 0 | 0 | 0.1 |
| Antioxidant 168 | 0.1 | 0 | 0 | 0.1 | 0.1 |
| Antioxidant 1010 | 0.1 | 0 | 0 | 0.1 | 0.1 |
| Electrostatic electret (kV) | 30 | 0 | 0 | 0 | 0 |
Through the test performance results of examples 1-5, comparative example 1 and table 3, it can be seen that compared with the polypropylene melt-blown non-woven fabric prepared by the conventional method, the biodegradable melt-blown non-woven fabric prepared by the formula and the preparation method provided by the invention does not need to be subjected to electret treatment by an electrode device, so that the energy consumption is greatly saved, and the biodegradable melt-blown non-woven fabric has better filtering performance and mechanical property, and simultaneously has a thinner and more uniform fiber structure.
From the test performance results of examples 1 to 3 and comparative examples 2 to 4 and table 3, it can be seen that the advantageous effects shown in the examples of the present invention cannot be obtained by using only one biodegradable raw material (e.g., PBAT resin or PLA resin). In addition, when the compounded lubricant and the compounded dispersant are not added in the raw material formula, the beneficial effects shown in the embodiment of the invention cannot be obtained. The compounded lubricant and the dispersant are added to play roles of promoting crystallization and flow, and simultaneously, the problem of system compatibility is solved, so that the material is more stable. Is beneficial to obtaining the melt-blown non-woven material with excellent filtering performance and mechanical property.
From the test performance results of example 1 and comparative example 5 and table 3, it can be seen that the beneficial effects demonstrated by the examples of the present invention cannot be obtained by fixing the formulation, changing and adjusting the melt-blown process parameters (melt-blown nonwoven preparation method) under the optimal conditions. Therefore, the preparation method of the melt-blown non-woven material provided by the invention is beneficial to obtaining the melt-blown non-woven material with excellent filtering performance and mechanical property.
Meanwhile, as shown in table 3, the biodegradable melt-blown non-woven fabric obtained by blending PBAT and PLA has the advantages that the filtration efficiency is higher than or equal to 97.5%, the ventilation resistance is lower than or equal to 10.2, the biodegradable melt-blown non-woven fabric is superior to melt-blown fabric prepared by polypropylene plus electret and electrostatic electret, the transverse and longitudinal strength of the biodegradable melt-blown non-woven fabric is superior to that of polypropylene melt-blown fabric, and the longitudinal elongation of the embodiment is more than 72.5%. Compared with polypropylene melt-blown fabric, the biodegradable melt-blown non-woven fabric prepared by the invention has the advantages of excellent filtering performance, good elasticity, softer hand feeling and wider application field. Also, it is clear from comparative examples 2 and 3 that the melt blown fabrics made from PBAT and PLA alone are not good in filtration efficiency. PLA melt-blown fabric has larger brittleness (low elongation) and poor mechanical property, and melt-blown non-woven material with excellent filtering property and good mechanical property is obtained by blending PBAT and PLA and combining with the optimization of melt-blown technology.
From fig. 1 to 4, example 2 prepared by the present invention has a finer and more uniform fiber structure than meltblown prepared from polypropylene plus electret, whereas meltblown prepared from PBAT alone has a thicker and non-uniform fiber diameter, whereas meltblown prepared from PLA alone has a thinner but highly non-uniform fiber diameter, which explains the difference in performance indexes of the meltblown nonwoven materials of the above examples and comparative examples.
In addition, by adding the compatilizer and the lubricant into the formula provided by the invention, the blending of PBAT and PLA is more uniform, and the compatibility is better, as shown in FIG. 5. It can be seen from the table that the compatibility of PBAT and PLA in example 2 is significantly improved by the optimization of the material formulation, and when observing the section of the slice, the blended slice optimized by the formulation does not have holes, and the cut section is smooth and flat, which provides favorable conditions for the subsequent melt-blown process processing and makes it possible to obtain melt-blown nonwoven products with excellent properties.
Claims (11)
1. A biodegradable melt-blown nonwoven material characterized by: the material comprises the following components:
2. a biodegradable meltblown nonwoven material according to claim 1, characterized in that:
3. a biodegradable meltblown nonwoven material according to claim 1, characterized in that: the biodegradable resin is at least one of PBAT, PBST, PBSA and PBS.
4. A biodegradable meltblown nonwoven material according to claim 1 or 2, characterised in that: the melt index of the biodegradable resin is 100-500g/10min at 210 ℃ and under the condition of 2.16 kg; preferably: the melt index of the biodegradable resin is 300-500g/10min at 210 ℃ and 2.16 kg.
5. A biodegradable meltblown nonwoven material according to claim 1, characterized in that: the melt index of the polylactic acid is 80-400g/10min under the conditions of 250 ℃ and 2.16 kg.
6. A biodegradable meltblown nonwoven material according to claim 5, characterized in that: the melt index of the polylactic acid is 50-400g/10min under the conditions of 250 ℃ and 2.16 kg; the molecular weight of the polylactic acid is between 10 and 13 ten thousand, and the melting point is between 160 and 170 ℃.
7. A biodegradable meltblown nonwoven material according to claim 1, characterized in that: the compatilizer is at least one of maleic anhydride, benzoyl peroxide, tetrabutyl titanate and polybasic acid; the lubricant is at least one selected from zinc stearate, calcium stearate and magnesium stearate; the chain extender is at least one selected from ADR4370S and KL-E4370; the antioxidant is at least one of antioxidant 168 and antioxidant 1010.
8. The biodegradable meltblown nonwoven material of claim 7, wherein: the lubricant is prepared by mixing at least one of zinc stearate, calcium stearate and magnesium stearate with one of chain extenders ADR4370S and KL-E4370 in a ratio of 1:0.5 to 1.5; the antioxidant is antioxidant 168 and antioxidant 1010, and the weight ratio of the antioxidant to the antioxidant is 1:0.5 to 1.5.
9. A method of making the biodegradable melt-blown nonwoven material of claim 1, wherein: the method comprises the following steps:
s1, preparing a mixed material:
s11, stirring and uniformly mixing the dried biodegradable resin, the polylactic acid, the compatilizer, the lubricant, the chain extender and the antioxidant in a high-speed mixer according to a formula ratio to obtain a mixed material;
s2, carrying out double-screw granulation on the mixed material:
melting, extruding, air cooling, bracing and cold cutting the mixed materials to prepare biodegradable resin/PLA blending biodegradable slices;
s3, preparing the melt-blown non-woven fabric by the biodegradable resin/PLA blending biodegradable slice:
s31, drying the prepared biodegradable resin/PLA blending biodegradable slice at 70-90 ℃ for 6-24h;
s32, melt-blowing process processing: adding dried biodegradable resin/PLA blending biodegradable slices into an automatic bin of a melt-blowing device, feeding the slices into a screw extruder, heating and melting the slices, flowing into a prefilter, filtering out impurities in a melt, flowing to a metering pump, extruding the melt to a small hole opening of a spinneret die head by virtue of the pressure of the metering pump, wherein the diameter of a spinneret hole is 0.2-0.5mm, carrying out hot-air high-speed drafting on the melt extruded from the spinneret plate by high-speed hot compressed air on two sides of the small hole, carrying out short-time cooling and crystallization on the obtained melt-blown superfine fiber under the action of side-blown cold air, and gathering the fiber on a web-forming curtain with the distance DCD from the die head of 160-250mm, wherein: the suction wind speed under the net is 1000-3000rpm; meanwhile, the operation speed of the rotary screen is 3-10m/min, and the rotary screen is wound at the speed of 3-10m/min to form the superfine fiber melt-blown non-woven fabric with good mechanical property;
s33, the obtained non-woven fabric does not need to be subjected to electret treatment by an electrode device, so that energy consumption is greatly saved, and finally, a finished product of the melt-blown non-woven material is obtained by coiling on a coiling machine and online cutting.
10. A method of making a biodegradable meltblown nonwoven material according to claim 9, characterized in that: the method comprises the following steps:
s1, preparing a mixed material:
s11, stirring and uniformly mixing the dried biodegradable resin, the polylactic acid, the compatilizer, the lubricant, the chain extender and the antioxidant in a high-speed mixer according to a formula ratio to obtain a mixed material;
s2, carrying out double-screw granulation on the mixed material:
the double-screw granulation process comprises the following steps: adding the obtained mixture into a storage bin, and continuously stirring, wherein the temperature of a granulation screw is 180-230 ℃, the rotating speed of the screw is 200-300r/min, and the rotating speed of a metering pump is 100-300Kg/h; extruding, air cooling, bracing and cold cutting the mixed material to prepare biodegradable resin/PLA blending biodegradable slices;
s3, preparing the melt-blown non-woven fabric by the biodegradable resin/PLA blending biodegradable slice:
s31, drying the prepared biodegradable resin/PLA blending biodegradable slice at 70-90 ℃ for 6-24h;
s32, melt-blowing process processing: adding dried biodegradable resin/PLA blending biodegradable slices into an automatic bunker of a melt-blowing device, feeding the slices into a screw extruder, heating and melting the slices, flowing into a prefilter, filtering impurities in a melt, flowing to a metering pump, extruding the melt to a small hole opening of a spinneret die head by virtue of the pressure of the metering pump, wherein the diameter of a spinneret hole is 0.2-0.5mm, carrying out hot-air high-speed drafting on the melt extruded from the spinneret plate by high-speed hot compressed air on two sides of the small hole, and carrying out short-time cooling crystallization on obtained melt-blown superfine fibers under the action of side-blown cold air, wherein the fibers are gathered on a web forming curtain with the distance DCD (direct chemical vapor deposition) from the die head of 160-250mm, wherein: the suction wind speed under the net is 1000-3000rpm; meanwhile, the operation speed of the rotary screen is 3-10m/min, and the superfine fiber melt-blown non-woven fabric with good mechanical property is formed by rolling at the speed of 3-10 m/min;
s33, the obtained non-woven fabric does not need to be subjected to electret treatment through an electrode device, energy consumption is greatly saved, and finally, a finished product of the melt-blown non-woven material is obtained through coiling on a lap former and online slitting.
11. The method for producing as claimed in claim 10, characterized in that: in S32, the parameters are set as follows:
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