CN112267212A - Biodegradable polypropylene composite material, melt-blown non-woven fabric and application thereof - Google Patents
Biodegradable polypropylene composite material, melt-blown non-woven fabric and application thereof Download PDFInfo
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- CN112267212A CN112267212A CN202011105960.6A CN202011105960A CN112267212A CN 112267212 A CN112267212 A CN 112267212A CN 202011105960 A CN202011105960 A CN 202011105960A CN 112267212 A CN112267212 A CN 112267212A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING 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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-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
- D04H1/54—Non-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
- D04H1/56—Non-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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING 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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-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
- D04H1/54—Non-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
- D04H1/542—Adhesive fibres
- D04H1/544—Olefin series
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Abstract
The invention discloses an anaerobic biodegradable polypropylene composite material, polypropylene-based melt-blown non-woven fabric, and a preparation method and application thereof. The polypropylene composite material capable of being anaerobically and biologically degraded comprises polypropylene resin, a processing aid and a biodegradation accelerator, wherein the content of the biodegradation accelerator is 1% -5% of that of the polypropylene resin, and the biodegradation accelerator comprises the degradation accelerator and bacterial signal conduction molecules. The polypropylene-based melt-blown nonwoven fabric is prepared from the polypropylene composite material according to the melt-blown nonwoven fabric process. The polypropylene composite material capable of being anaerobically and biologically degraded has high biodegradation rate in an anaerobic environment, is suitable for melt-blown non-woven fabrics, and can endow the melt-blown non-woven fabrics with good barrier property.
Description
Technical Field
The invention belongs to the technical field of melt-blown non-woven fabrics and materials thereof, and particularly relates to an anaerobic biodegradable polypropylene composite material, a polypropylene-based melt-blown non-woven fabric, and a preparation method and application thereof.
Background
Meltblown nonwovens are sheets, webs or batts made of polypropylene as the primary material, with fibers that are oriented or randomly oriented and bonded to one another by friction, cohesion or bonding, or a combination of these methods. The fiber diameter can reach 1-5 microns, the gaps are large, the structure is fluffy, the anti-wrinkle capacity is good, the fiber melt-blown fabric has a unique capillary structure, the number of fibers in unit area is increased by utilizing the specific surface area of superfine fibers, so that the melt-blown fabric has good filtering property, shielding property, heat insulating property and oil absorbing property, and the fiber melt-blown fabric can be used in the fields of air, liquid filtering materials, isolating materials, absorbing materials, mask materials, heat-insulating materials, oil absorbing materials, wiping cloth and the like.
The polypropylene-based melt-blown non-woven fabric cannot be degraded, has high melt index, and has no means for effectively recycling the polypropylene-based melt-blown non-woven fabric, so that the waste polypropylene-based melt-blown non-woven fabric causes serious pollution after being improperly treated after the use period, and does not meet the requirement of sustainable development.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide an anaerobically biodegradable polypropylene composite material, polypropylene-based melt-blown nonwoven fabric and a preparation method thereof, so as to solve the technical problems of low degradation rate of melt-blown nonwoven fabric materials, particularly low anaerobic biodegradation rate or difficult degradation.
In order to achieve the above object, according to one aspect of the present invention, there is provided an anaerobically biodegradable polypropylene composite. The polypropylene composite material capable of being anaerobically and biologically degraded comprises polypropylene resin, a processing aid and a biodegradation accelerator, wherein the content of the biodegradation accelerator is 1% -5% of that of the polypropylene resin, and the biodegradation accelerator comprises the degradation accelerator and bacterial signal conduction molecules.
Preferably, the biodegradation accelerator comprises a core and a shell coating the core; wherein the material of the core comprises the degradation promoting agent and a bacterial signaling molecule, and the degradation promoting agent forms a mixture with the bacterial signaling molecule; the material of the shell layer comprises a high molecular material for providing nutrients.
And/or, preferably, the melt index of the polypropylene resin is 1200-1800 g/10 min.
In another aspect of the present invention, a polypropylene-based meltblown nonwoven is provided. The polypropylene-based melt-blown non-woven fabric is made of the polypropylene composite material capable of being anaerobically and biologically degraded.
In yet another aspect of the present invention, a method for preparing a polypropylene-based meltblown nonwoven fabric is provided. The preparation method of the polypropylene-based melt-blown non-woven fabric comprises the following steps:
carrying out melting treatment on the polypropylene composite material to obtain a melt;
and sequentially carrying out filtering spinning treatment, cooling traction treatment, net forming pre-pressing treatment and hot rolling consolidation treatment on the melt.
In yet another aspect of the present invention, a meltblown nonwoven article is provided. The melt-blown non-woven fabric product is prepared from the polypropylene-based melt-blown non-woven fabric or the polypropylene-based melt-blown non-woven fabric prepared by the preparation method.
Compared with the prior art, the invention has the following technical effects:
the degradation promoter contained in the polypropylene composite material capable of being anaerobically biodegraded can accelerate the degradation speed of a polypropylene resin molecular chain, the bacteria signal conduction molecules can induce bacteria to send out a signal of gene expression change so as to promote anaerobic bacteria groups to aggregate to form a biomembrane, so that the gnawing effect on the polypropylene resin is accelerated, the accelerated degradation of the polypropylene resin in an anaerobic environment is realized, and the polypropylene composite material capable of being anaerobically biodegraded is also suitable for melt-blown non-woven fabrics and can endow the melt-blown non-woven fabrics with good barrier property.
Preferably, the biodegradation accelerator contained in the anaerobically biodegradable polypropylene composite material is in a core-shell structure, so that the high polymer material contained in the shell layer can provide sufficient nutrients for the propagation of bacteria and enable the bacteria to gather, thereby accelerating the degradation of the polypropylene resin by a core body in an anaerobic environment; in the anaerobic degradation process, the gaps left after the high polymer materials are consumed can provide space for the propagation of bacteria.
The polypropylene-based melt-blown non-woven fabric is made of the polypropylene composite material which can be biologically degraded anaerobically, so that the polypropylene-based melt-blown non-woven fabric has good barrier property and good biodegradability, particularly anaerobic biodegradation property, and the harm of the waste polypropylene-based melt-blown non-woven fabric to the environment is reduced.
The polypropylene-based melt-blown non-woven fabric is directly prepared from the polypropylene composite material capable of being anaerobically and biologically degraded by adopting a melt-blowing method, so that the prepared polypropylene-based melt-blown non-woven fabric has good barrier property, smooth filtration and spinning treatment and uniform texture, the quality of the prepared polypropylene-based melt-blown non-woven fabric is effectively ensured, and the efficiency is high.
The melt-blown non-woven fabric product is prepared from the polypropylene-based melt-blown non-woven fabric, so that the melt-blown non-woven fabric product has good barrier property, meets the requirements of the industry, can be effectively degraded after being discarded, can be rapidly degraded particularly in an anaerobic environment, and is environment-friendly.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic structural diagram of a biodegradation accelerator according to an embodiment of the present invention;
FIG. 2 is a schematic process flow diagram of a preparation method of the biodegradation accelerator according to the embodiment of the invention;
FIG. 3 is a schematic process flow diagram of a method for preparing a polypropylene-based meltblown nonwoven fabric according to an embodiment of the invention;
FIG. 4 is an SEM photograph of a commercially available polypropylene-based meltblown nonwoven fabric without added biodegradation accelerator and polypropylene-based meltblown nonwoven fabrics provided in examples 21-23 of the present invention; wherein, FIG. 4(a) is an SEM photograph of a commercially available polypropylene-based meltblown nonwoven fabric; fig. 4(b) to 4(d) are SEM photographs of the polypropylene-based meltblown nonwoven fabric provided in the order of example 21 to example 23;
fig. 5 is a photograph of a polypropylene-based meltblown nonwoven fabric provided in example 22 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the present application, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (a), b, and c", may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, and c may be single or plural, respectively.
It should be understood that, in various embodiments of the present application, the sequence numbers of the above-mentioned processes do not mean the execution sequence, and some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weight of the related components mentioned in the description of the embodiments of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present application as long as it is scaled up or down according to the description of the embodiments of the present application. Specifically, the mass in the description of the embodiments of the present application may be in units of mass known in the chemical industry, such as μ g, mg, g, and kg.
In one aspect, embodiments of the present invention provide an anaerobically biodegradable polypropylene composite (hereinafter, referred to simply as polypropylene composite). The polypropylene composite material comprises polypropylene resin, a processing aid and a biodegradation accelerator.
The biodegradation accelerant contained in the polypropylene composite material comprises 1% -5% of the biodegradation accelerant and bacterial signal conduction molecules, so that the biodegradation accelerant contained in the biodegradation accelerant can accelerate the degradation speed of a molecular chain of the polypropylene composite material, and the bacterial signal conduction molecules can induce bacteria to send out signals of gene expression change so as to promote anaerobic flora aggregates to form a biomembrane, so that the gnawing effect on the polypropylene composite material is accelerated, and the accelerated degradation of the polypropylene composite material in an anaerobic environment is realized.
In one embodiment, the biodegradation accelerator contained in the polypropylene composite material is a core-shell structure as shown in figure 1, and specifically comprises a core body 2 and a shell layer 1 for coating the core body 2; the material of the shell layer 1 comprises a high polymer material for providing nutrients, and the molecules of the high polymer material are crosslinked; the material of the nucleus 2 comprises a degradation promoting agent and a bacterial signalling molecule, and the degradation promoting agent forms a mixture with said bacterial signalling molecule. Thus, the biodegradation accelerator is arranged into a core-shell structure as shown in figure 1, and the high molecular material in the shell layer 1 can effectively form a film layer to coat the core body 2; on the other hand, the high molecular material can provide sufficient nutrients for the propagation of bacteria, particularly anaerobic bacteria, and enable the bacteria, particularly the anaerobic bacteria, to gather; and the high molecular material molecules are crosslinked, so that the stability of the shell layer 1 can be ensured, and the core body 2 can be stably coated, thereby improving the stability of the core-shell structure of the composite biodegradation accelerator. In one embodiment, the polymer material in the shell 1 is a natural polymer material. In a specific embodiment, the natural polymer material comprises at least one of starch, gelatin, chitosan and sodium alginate, preferably chitosan, wherein the deacetylation degree of the chitosan is more than or equal to 85%, and the freezing value of the gelatin is more than or equal to 120. The optimized high polymer material can not only provide nutrients for bacteria, particularly anaerobic bacteria, but also form a coating shell layer 1, is natural and harmless, is easy to biodegrade, does not have secondary pollution, is environment-friendly and has low cost.
In another embodiment, the shell 1 has a thickness of 200nm to 2 μm, preferably 200nm to 1 μm. By adjusting and optimizing the thickness of the shell layer 1, on the one hand, sufficient nutrients for the propagation of bacteria, particularly anaerobic bacteria, are provided, and on the other hand, a coating shell layer can be effectively formed to effectively coat the nucleus body 2.
The material of the nucleus 2 comprises the degradation accelerant and the bacterial signal conduction molecules, so that the degradation accelerant contained in the nucleus 2 can accelerate the degradation speed of the molecular chain of the polypropylene composite material, and the contained bacterial signal conduction molecules can induce bacteria to send out signals of gene expression change so as to promote anaerobic flora to gather to form a biomembrane, thereby accelerating the feeding effect on the polypropylene composite material and accelerating the accelerated degradation of the polypropylene composite material in an anaerobic environment.
In each of the above embodiments, as an embodiment of the present invention, the weight ratio of the degradation promoter contained in the biodegradation accelerator to the bacterial signaling molecule is 1: (1-4). In one embodiment, the degradation promoting agent comprises a metal stearate, and in a specific embodiment, the metal stearate comprises at least one of iron stearate salt, copper stearate salt, cobalt stearate salt, and nickel stearate salt, preferably nickel stearate salt. In another embodiment, the bacterial signaling molecule comprises at least one of 3, 5-dimethyl-pentenyl-dihydro-2 (3H) furan, N-acyl homoserine lactone, furanyl boronic acid diester, preferably N-acyl homoserine lactone. The proportion and the variety of the degradation accelerant and the bacterial signal conduction molecules are adjusted and optimized to improve the above functions of the nucleus body 2, specifically, the degradation accelerant is optimized and improved to accelerate the degradation speed of a polypropylene composite material molecular chain, the bacterial signal conduction molecules are optimized and improved to induce bacteria to send out a signal of gene expression change, so that anaerobic bacteria groups are improved to gather to form a biological membrane, the gnawing effect of the polypropylene composite material is accelerated, and the accelerated degradation effect of the polypropylene composite material in an anaerobic environment is accelerated.
In another embodiment, the core body 2 has a particle size of 600nm to 4 μm, preferably 600nm to 2 μm, more preferably 400nm to 2 μm. Through the regulation and optimization of the particle size of the nucleus body 2, the functions of the degradation promoter and the bacterial signal conduction molecules are fully exerted, the degradation speed of the nucleus body 2 to the molecular chain of the polypropylene composite material is improved, and the bacteria are induced to send out a signal of gene expression change, so that the accelerated degradation effect of the polypropylene composite material in an anaerobic environment is improved.
In addition, the particle size of the core-shell structure of the biodegradation accelerator in each of the above embodiments can be adjusted by controlling and adjusting the thickness of the shell layer 1 and the particle size of the core body 2, and in one embodiment, the particle size of the biodegradation accelerator is 800nm to 6 μm, preferably 600nm to 3 μm.
Therefore, the above preferred biodegradation accelerator is preferably a composite structure with a core shell, can provide nutrients required for propagation of bacteria, particularly anaerobic bacteria, under the synergistic action of the shell layer 1 and the core body 2, and can induce the bacteria, particularly anaerobic bacteria, to aggregate to form a biofilm, so that the feeding effect on the polypropylene composite material is realized, and the accelerated degradation of the polypropylene composite material in an anaerobic environment is accelerated. And the synergistic interaction between the core body 2 and the shell layer 1 can be improved by adjusting and optimizing the components, the weight ratio and the like of the core body 2 and the shell layer 1, so that the accelerated degradation effect of the polypropylene composite material in an anaerobic environment is improved. Specifically, in the anaerobic degradation, the natural polymer material preferably used in the shell layer 1 and the bacterial signal transduction molecule contained in the core body 2 play a synergistic role in regulating the bacterial reproduction, and the shell layer 1 can provide a space for the enlarged reproduction of bacteria after being decomposed.
In one embodiment, the biodegradation accelerator described hereinabove may be used in accordance with a process flow comprising the steps of:
step S01: dispersing a degradation promoter and a bacterial signaling molecule in an aqueous solution containing a polymeric material for providing nutrients to form an aqueous phase;
step S02: preparing an oil phase;
step S03: emulsifying the water phase and the oil phase to obtain water-in-oil reverse microemulsion;
step S04: and adding a cross-linking agent into the water-in-oil reverse microemulsion for cross-linking reaction, and then carrying out solid-liquid separation treatment.
Wherein the polymer material contained in the aqueous phase in step S01 is a material contained in the core body 2 forming the biodegradation accelerator, the degradation accelerator and the bacterial signaling molecule constituting the biodegradation accelerator, which material is formed in the shell layer 1 of the biodegradation accelerator shown in fig. 1. Thus, the polymeric material, the degradation promoter and the bacterial signalling molecule are added in proportions such that the shell 1 and core 2 are capable of forming the biodegradation promoter as shown in figure 1 when formulating the aqueous phase. As in one embodiment, the polymeric material, the degradation promoter, and the bacterial signaling molecule are present in a weight ratio of 0.6-0.8: 1: (1-4), preferably 0.6-0.8: 1: (1-2). In another embodiment, the weight concentration of the aqueous solution of the polymer material is preferably 1% to 5%. By controlling and optimizing the components of the water phase and the concentration of each component, the stable water-in-oil reverse microemulsion formed in the emulsification treatment process of the water phase is improved, and the stability of the water-in-oil reverse microemulsion particles is improved.
In addition, the degradation promoter, the bacterial signal transduction molecule and the polymer material in step S01 are respectively the degradation promoter, the bacterial signal transduction molecule and the polymer material contained in the above biodegradation promoter, and for the sake of saving space, the degradation promoter, the bacterial signal transduction molecule and the polymer material in the aqueous phase are not described in detail herein.
The oil phase in step S02 can be formulated as a conventional oil phase, and in a preferred embodiment, the oil phase is formulated as follows:
and mixing the continuous phase and the surfactant to form the oil phase, wherein the weight ratio of the continuous phase to the surfactant is 1-1.5: 1.
In particular embodiments, the continuous phase includes at least one of liquid paraffin, kerosene, white oil, or isomeric hexadecanes. In another embodiment, the surfactant contained in the oil phase comprises at least one of span and tween. The stability of the emulsion is improved by selecting the types of the oil phase components.
The emulsification treatment in step S03 is to mix the aqueous phase and the oil phase and may be a conventional emulsification treatment so that aqueous phase particles are formed in the oil phase. In addition, the aqueous phase and the oil phase may be mixed in proportions that form a water-in-oil reverse microemulsion, such as in one embodiment, the aqueous phase and the oil phase are present in a weight ratio of 1: (2-5) to form a water-in-oil reverse microemulsion in which the aqueous phase particles are uniform and stable.
In step S04, after the cross-linking agent is added to the water-in-oil inverse microemulsion, the cross-linking agent will promote the cross-linking reaction of the polymer material in the aqueous phase microparticles, and form a polymer film layer on the surface of the aqueous phase microparticles, that is, the shell layer 1 of the above biodegradation accelerator shown in fig. 1, and coat the degradation accelerator and the bacterial signaling molecules contained in the aqueous phase microparticles in the shell layer 1, so that the degradation accelerator and the bacterial signaling molecules form the core body 2 of the above biodegradation accelerator shown in fig. 1.
In addition, in the crosslinking reaction, the crosslinking agent should be added in a sufficient amount to allow the sufficient crosslinking reaction of the high molecules in the aqueous phase fine particles. In one embodiment, the cross-linking agent is added into the water-in-oil reverse microemulsion according to a weight ratio of the cross-linking agent to the polymer material of 1% to 5% to perform the cross-linking reaction, that is, the cross-linking agent is added into the water-in-oil reverse microemulsion according to a weight ratio of the cross-linking agent to the polymer material of 1: (20-100) is added into the water-in-oil reverse microemulsion to carry out the crosslinking reaction. In a particular embodiment, the cross-linking agent comprises at least one of glutaraldehyde, genipin, epichlorohydrin. The addition amount and the type of the cross-linking agent are optimized, so that the efficiency of the cross-linking reaction is improved, and the biodegradation accelerant with stable core-shell structure is formed.
In one embodiment, in step S04, the temperature of the water-in-oil reverse microemulsion is preferably 25 to 60 ℃ during the crosslinking reaction. In order to disperse the crosslinking agent uniformly and to sufficiently act on each aqueous phase fine particle in the water-in-oil reverse microemulsion, it is preferable to carry out a treatment such as stirring during the crosslinking reaction.
In addition, after the step of the crosslinking reaction in step S04, the method further includes a step of performing solid-liquid separation on the mixed solution to collect and wash the solid matter, to remove the solvent in the mixed solution after the crosslinking reaction, and to remove the surfactant and other organic impurities adhered to the surface, and to vacuum-dry the mixed solution.
The biodegradation accelerator in the embodiments is prepared by a microemulsion method, so that the prepared biodegradation accelerator has relatively uniform grain size and complete core-shell structure. The prepared biodegradation accelerator has the advantages of providing nutrients required for propagation of bacteria, particularly anaerobic bacteria, inducing the bacteria, particularly the anaerobic bacteria to aggregate to form a biological membrane, and realizing the feeding effect on the polypropylene composite material, thereby accelerating the degradation of the polypropylene composite material in an anaerobic environment. In addition, the preparation method of the biodegradation accelerator has easily controlled conditions, so that the prepared biodegradation accelerator has stable performance and high efficiency.
The polypropylene resin contained in the polypropylene composite material can be polypropylene resin commonly used for preparing melt-blown non-woven fabrics, and is preferably selected from polypropylene resin with the melt index of 1200-1800 g/10min by combining the biodegradation accelerant. The polypropylene resin with the optimized melt index range can improve the applicability of the polypropylene composite material in the preparation of melt-blown non-woven fabrics, improve the quality of the melt-blown non-woven fabrics and fully play the role of the biodegradation accelerant.
The type and amount of the processing aid contained in the polypropylene composite material can be flexibly selected and controlled according to the processing requirements or application environment of the polypropylene composite material, for example, in one embodiment, the processing aid comprises at least one of a dispersant, a lubricant, a nucleating agent and an antioxidant. In another embodiment, the processing aid comprises 0.5-2% by weight of the polypropylene composite.
In addition, the polypropylene composite material in each of the above embodiments may be subjected to a mixing process of the components and the content ratio contained in the polypropylene composite material, such as a melt extrusion granulation process.
Therefore, the synergistic effect of the degradation promoter and the bacterial signal conducting molecule contained in the polypropylene composite material in each of the above embodiments, preferably the effect of the biodegradation promoter with the core-shell structure described above, can realize the accelerated degradation of the polypropylene resin, particularly the accelerated degradation in an anaerobic environment, without increasing the cost, and compared with biodegradable melt-blown nonwoven fabrics such as PLA, PBAT, PBS, and the like, the polypropylene composite material has the advantages of low cost, sufficient raw material sources, low degradation requirement, and degradability in an anaerobic landfill. And endows the polypropylene composite material with good barrier property, and is also suitable for melt-blown non-woven fabrics.
On the other hand, based on the above polypropylene composite material having good biodegradation, especially accelerated degradation in an anaerobic environment, and being suitable for melt-blown nonwoven fabrics, the embodiment of the invention also provides a polypropylene-based melt-blown nonwoven fabric. The polypropylene-based melt-blown non-woven fabric is made of the polypropylene composite material, namely the polypropylene-based melt-blown non-woven fabric is prepared from the polypropylene composite material according to the preparation process of the melt-blown non-woven fabric. Therefore, the polypropylene-based melt-blown non-woven fabric not only has good barrier property, but also has good biodegradation property, particularly anaerobic biodegradation property, thereby reducing the harm of the waste polypropylene-based melt-blown non-woven fabric to the environment.
Correspondingly, the embodiment of the invention provides a preparation method of the polypropylene-based melt-blown non-woven fabric. The process flow of the preparation method of the polypropylene-based melt-blown non-woven fabric is shown in figure 3, and comprises the following steps:
step S05: carrying out melting treatment on the polypropylene composite material to obtain a melt;
step S06: and sequentially carrying out filtering spinning treatment, cooling traction treatment, net forming pre-pressing treatment and hot rolling consolidation treatment on the melt.
The polypropylene composite material in step S05 is the above polypropylene composite material, and therefore, for the sake of saving space, the components and the contents of the components contained in the polypropylene composite material are not described again.
The filtration spinning treatment, the cooling traction treatment, the web-forming pre-pressing treatment and the hot rolling consolidation treatment of the step S06 can be carried out according to the preparation process conditions of the polypropylene melt-blown non-woven fabric. In combination with the components and the contents of the components contained in the polypropylene composite material, in an embodiment, the filtration precision in the filtration spinning treatment process in the step S06 is 18-22 μm, the diameter of the filter screen is 90-110mm, the pressure before filtration is 2.4-2.6MPa, the pressure after filtration is 5.9-6.1MPa, the rotation speed of the metering pump is 15-20 rpm, the temperature of the metering section is 200-.
The air quantity of a suction air channel in the cooling and traction treatment process is preferably 800-900 m3The air pressure is preferably 5-6 kPa.
The rotating speed of the conveying belt for the web-forming prepressing treatment is preferably 10-20 m/min, and the pressure is preferably 0.6-0.8 MPa.
The rolling pressure of the hot rolling consolidation treatment is preferably 5.5-8 MPa, and the temperature of the upper roller and/or the lower roller is preferably 80-85 ℃.
Through the optimization of each processing process condition in the step S06, the prepared melt-blown non-woven fabric is uniform in texture, the quality of the prepared polypropylene-based melt-blown non-woven fabric is effectively guaranteed, and the barrier property is good. In addition, the preparation method of the polypropylene-based melt-blown non-woven fabric has the advantages of short flow, low cost, stable melt quality and excellent processing performance, the mechanical properties and other indexes of the prepared non-woven fabric can meet the use requirements, the final product is decomposed by microorganisms or enzymes in the nature after being discarded, and the final product is methane, carbon dioxide and water, and is a completely biodegradable high polymer material.
In yet another aspect, embodiments of the present invention also provide a meltblown nonwoven article based on the above polypropylene composite and polypropylene-based meltblown nonwoven. In particular embodiments, the meltblown nonwoven article may be a filtration article, a barrier article, an absorbent article, a respirator, a thermal article, an oil absorbent article, a wipe, and the like. Therefore, the melt-blown non-woven fabric product is made of the polypropylene-based melt-blown non-woven fabric, so that the melt-blown non-woven fabric product has good barrier property, meets the requirements of the industry, can be effectively degraded after being discarded, can be rapidly degraded particularly in an anaerobic environment, and is environment-friendly.
The present invention will now be described in further detail by taking polypropylene composites and polypropylene-based meltblown nonwovens and methods for making them as examples.
1. Examples of Polypropylene composite materials
Example 11
The embodiment of the invention provides a polypropylene composite material, which comprises polypropylene resin, 1 percent of antioxidant 1010 and 1 percent of biodegradation accelerator by weight percentage; wherein the melt index of the polypropylene composite material is 1500g/10 min; the processing aid is antioxidant 1010; the biodegradation accelerator is in a core-shell structure as shown in figure 1, wherein a core body comprises a mixture of nickel stearate and N-acyl homoserine lactone in a mass ratio of 1: 1; the shell layer comprises chitosan with deacetylation degree of 95%. The grain size of the core body of the biodegradation accelerator is 600nm +/-200 nm, and the grain size of the biodegradation accelerator is 1 mu m +/-200 nm.
The polypropylene composite material provided by the embodiment of the invention is prepared by stirring the components and the content ratio for 15min at the rotating speed of 2500r/min, taking out, drying for 2h at about 100 ℃, and then extruding and granulating by a double-screw extruder, wherein the processing temperature is 190-210 ℃.
The preparation method of the biodegradation accelerator comprises the following steps:
s1: weighing 3g of chitosan powder with deacetylation degree of 95% into 250ml of 2% acetic acid aqueous solution, stirring until no bubbles are generated, adding 4g of nickel stearate and 4g N-acylhomoserine lactone, and uniformly dispersing to obtain a water phase;
s2: adding 150g span and 150g Tween 80 into 300g paraffin, and stirring to obtain a uniform system as an oil phase;
s3: adding the water phase into the oil phase, and stirring uniformly to obtain a semitransparent white oil water-in-water type reverse microemulsion;
s4: adding 0.15g of glutaraldehyde as a cross-linking agent into the system, carrying out constant-temperature water bath at 40 ℃, mechanically stirring, washing particles with isopropanol after reaction, removing a surfactant and an organic matter, and drying in a vacuum drying oven at 60 ℃.
Example 12
The embodiment of the invention provides a polypropylene composite material, which comprises polypropylene resin, an antioxidant 1010 and a biodegradation accelerant, wherein the antioxidant 1010 accounts for 0.5 percent of the weight of the polypropylene resin, and the biodegradation accelerant accounts for 1.5 percent of the weight of the polypropylene resin; wherein the melt index of the polypropylene composite material is 1800g/10 min; the processing aid is antioxidant 1010; the biodegradation accelerator is in core-shell structure as shown in figure 1, and the core body comprises a mixture of cobalt stearate and 3, 5-dimethyl-pentenyl-dihydro-2 (3H) furan in a mass ratio of 1: 1.5; the shell layer comprises chitosan with deacetylation degree of 95%. The particle size of the core body of the biodegradation accelerator is 800nm +/-100 nm, and the particle size of the biodegradation accelerator is 1.5 mu m +/-100 nm.
The polypropylene composite material provided by the embodiment of the invention is prepared by stirring the components and the content ratio for 15min at the rotating speed of 2500r/min, taking out, drying for 2h at about 100 ℃, and then extruding and granulating by a double-screw extruder at the processing temperature of 200-210 ℃.
The preparation method of the biodegradation accelerator comprises the following steps:
s1: weighing 3g of chitosan powder with the deacetylation degree of 95 percent, adding the chitosan powder into 250ml of 2 percent acetic acid aqueous solution, stirring until no bubbles are generated, adding 3g of nickel stearate and 4.5g of 3, 5-dimethyl-pentenyl-dihydro-2 (3H) furan, and uniformly dispersing to obtain a water phase;
s2: adding 150g span and 150g Tween 80 into 300g paraffin, and stirring to obtain a uniform system as an oil phase;
s3: adding the water phase into the oil phase, and stirring uniformly to obtain a semitransparent white oil water-in-water type reverse microemulsion;
s4: adding 0.15g of glutaraldehyde as a cross-linking agent into the system, carrying out constant-temperature water bath at 40 ℃, mechanically stirring, washing particles with isopropanol after reaction, removing a surfactant and an organic matter, and drying in a vacuum drying oven at 60 ℃.
EXAMPLES example 13
The embodiment of the invention provides a polypropylene composite material, which comprises polypropylene resin, an antioxidant 1010 and a biodegradation accelerator, wherein the antioxidant 1010 and the biodegradation accelerator account for 1 weight percent of the polypropylene resin; wherein the melt index of the polypropylene composite material is 1500g/10 min; the processing aid is antioxidant 1010; the biodegradation accelerator is of a core-shell structure as shown in figure 1, wherein a core body comprises a mixture of ferric stearate and furylboric acid diester in a mass ratio of 1: 2; the shell layer comprises gelatin with a freezing value of 200. The grain size of the core body of the biodegradation accelerator is 1.3 mu m +/-100 nm, and the grain size of the biodegradation accelerator is 1.8 mu m +/-200 nm.
The polypropylene composite material provided by the embodiment of the invention is prepared by stirring the components and the content ratio for 15min at the rotating speed of 2500r/min, taking out, drying for 2h at about 100 ℃, and then extruding and granulating by a double-screw extruder at the processing temperature of 200-210 ℃.
The preparation method of the biodegradation accelerator comprises the following steps:
s1: weighing 3g of gelatin powder with the freezing value of 200, adding the gelatin powder into 250ml of water, heating to 70 ℃, stirring until no bubbles are generated, adding 3g of nickel stearate and 6g of furoylboric acid diester, and uniformly dispersing to obtain a water phase;
s2: adding 150g span and 150g Tween 80 into 300g paraffin, and stirring to obtain a uniform system as an oil phase;
s3: adding the water phase into the oil phase, and stirring uniformly to obtain a semitransparent white oil water-in-water type reverse microemulsion;
s4: adding 0.1g genipin as a cross-linking agent into the system, carrying out constant-temperature water bath at 40 ℃, mechanically stirring, washing particles with isopropanol after reaction, removing a surfactant and an organic matter, and drying in a vacuum drying oven at 60 ℃.
2. Polypropylene based meltblown nonwoven examples
Example 21
The embodiment of the invention provides polypropylene-based melt-blown nonwoven fabric, which is prepared from the polypropylene composite material provided by the embodiment 11 according to the following preparation process steps and conditions of the melt-blown nonwoven fabric:
s5: drying the polypropylene composite particles provided in example 11 at 70 ℃ until the water content is less than or equal to 3%; carrying out melting treatment on corresponding melt spinning direct injection production equipment to obtain a melt;
s6, filtering and spinning treatment:
the melt passes through a melt filter, the filtering precision is 20 mu m, the diameter of a filter screen is 100 mu m, the pressure before filtering is 2.5 +/-MPa, the pressure after filtering is 6.00MPa, the rotating speed range of a metering pump is 17rpm, and the extrusion amount is 16 g/min; controlling the temperature of the metering section at 220 ℃, then sending the melt into a spinning manifold for melt-blowing process, controlling the temperature of the manifold at 200 ℃, the pressure of the manifold at 3.5MPa, controlling the aperture of a spinneret plate at 0.2mm, and controlling the number of holes at 11840; forming discontinuous microfibers;
cooling and drawing treatment: after being extruded from a spinneret orifice, the fibers are formed by traction and shaping through a suction air duct, and then are uniformly distributed on a web-forming conveyor belt through a cooling fan, wherein the air quantity of the suction air duct is 850m3Min, wind pressure 6 kPa;
web-forming prepressing treatment and hot rolling consolidation treatment: then collecting the mixture on a lapping device, and utilizing the preheating of hot air to generate self-bonding and coiling; the rotating speed of the prepressing roll is 15m/min, the pressure is 0.7MPa, the pressure of the hot pressing roll is 7MPa, the temperature of the upper roll and the lower roll is 83 ℃ and 82 ℃ respectively, and the surface density of the polypropylene-based melt-blown non-woven fabric capable of being biodegraded in an anaerobic mode is 20g/m2。
Example 22
The embodiment of the invention provides a polypropylene-based melt-blown nonwoven fabric, which is prepared from the polypropylene composite material provided in the embodiment 12 according to the following preparation process steps and conditions of the melt-blown nonwoven fabric, and the finished product of the polypropylene-based melt-blown nonwoven fabric is shown in fig. 5:
s5: drying the polypropylene composite particles provided in example 12 at 70 ℃ until the water content is less than or equal to 3%; carrying out melting treatment on corresponding melt spinning direct injection production equipment to obtain a melt;
s6. the filtration spinning treatment, the cooling drawing treatment, the web-formation pre-pressing treatment and the hot rolling consolidation treatment were carried out in accordance with step S6 in example 21, respectively.
Example 23
The embodiment of the invention provides polypropylene-based melt-blown nonwoven fabric, which is prepared from the polypropylene composite material provided by the embodiment 13 according to the following preparation process steps and conditions of the melt-blown nonwoven fabric:
s5: drying the polypropylene composite particles provided in example 12 at 70 ℃ until the water content is less than or equal to 3%; carrying out melting treatment on corresponding melt spinning direct injection production equipment to obtain a melt;
s6. the filtration spinning treatment, the cooling drawing treatment, the web-formation pre-pressing treatment and the hot rolling consolidation treatment were carried out in accordance with step S6 in example 21, respectively.
Correlation characteristic test
1. SEM of polypropylene based meltblown nonwoven:
commercially available polypropylene-based meltblown nonwoven fabrics without added biodegradation accelerator and the polypropylene-based meltblown nonwoven fabrics provided in examples 21 to 23 were subjected to SEM analysis, and SEM photographs are shown in fig. 4. As can be seen from the SEM photographs shown in fig. 4, the SEM photographs of the polypropylene-based meltblown nonwoven fabrics provided in examples 21 to 23 are very close to the SEM images of the commercially available polypropylene-based meltblown nonwoven fabrics without adding the biodegradation accelerator, and thus it is found that the addition of the biodegradation accelerator does not have a great influence on the spinnability of the polypropylene meltblown nonwoven fabrics and good compatibility between the biodegradation accelerator and the polypropylene matrix is maintained. Among them, the polypropylene melt-blown nonwoven fabric provided in example 21 has more uniform fiber size, and the main reason for this is probably because the biodegradable promoter contained in the anaerobic biodegradable polypropylene composite material provided in example 11 of the present invention has relatively smaller particle size and less influence on the spinning process.
2. Anaerobic degradation experiments on polypropylene-based meltblown nonwovens:
the polypropylene-based meltblown nonwoven fabrics provided in examples 21 to 23 and cellulose and commercially available polypropylene-based meltblown nonwoven fabrics were subjected to anaerobic biodegradation tests under the same conditions, and the results of the tests are shown in Table 1 below, when the test duration was 45 days and the respective indices in Table 1 were measured according to ASTM-D5511.
As can be seen from table 1, under the same degradation conditions, the cellulose degradation rate reached 93.67%, while the degradation rate of the commercial control sample without the addition of the biodegradation accelerator was 0. The polypropylene-based melt-blown non-woven fabrics provided by the embodiments 21-23 of the invention have been degraded to different degrees, which proves that the addition of the biodegradation accelerator can improve the degradation capability of the polypropylene melt-blown non-woven fabrics to a certain extent, wherein the degradation effect of the embodiment 21 is most obvious and reaches 11.86%.
TABLE 1
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. An anaerobically biodegradable polypropylene composite material comprises polypropylene resin, a processing aid and a biodegradation accelerator, wherein the content of the biodegradation accelerator is 1% -5% of that of the polypropylene resin, and the biodegradation accelerator comprises the degradation accelerator and bacterial signal conduction molecules.
2. The polypropylene composite according to claim 1, wherein: the biodegradation accelerator comprises a core body and a shell layer coating the core body; wherein the material of the core comprises the degradation promoting agent and a bacterial signaling molecule, and the degradation promoting agent forms a mixture with the bacterial signaling molecule; the material of the shell layer comprises a high polymer material for providing nutrients; and/or
The melt index of the polypropylene resin is 1200-1800 g/10 min.
3. The polypropylene composite according to claim 2, wherein: the weight ratio of the degradation promoter to the bacterial signaling molecule is 1: (1-4); and/or
The degradation promoter comprises a metal stearate; and/or
The bacterial signaling molecule comprises at least one of 3, 5-dimethyl-pentenyl-dihydro-2 (3H) furan, N-acylhomoserine lactone, furan acyl boronic acid diester; and/or
The high polymer material is a natural high polymer material.
4. The polypropylene composite according to claim 3, wherein: the metal stearate comprises at least one of ferric stearate salt, copper stearate salt, cobalt stearate salt and nickel stearate salt;
the natural polymer material comprises at least one of starch, gelatin, chitosan and sodium alginate.
5. Polypropylene composite according to any of claims 2-4 wherein: the particle size of the core body is 600nm-4 mu m; and/or
The thickness of the shell layer is 200nm-2 μm; and/or
The grain size of the biodegradation accelerator is 800 nm-6 mu m.
6. The polypropylene composite according to any one of claims 1 to 4, wherein: the processing aid comprises at least one of a dispersant, a lubricant, a nucleating agent and an antioxidant; and/or
The processing aid accounts for 0.5-2% of the weight of the polypropylene composite material.
7. A polypropylene-based meltblown nonwoven characterized by: the polypropylene-based melt-blown nonwoven fabric is made of the polypropylene composite material according to any one of claims 1 to 6.
8. A preparation method of polypropylene-based melt-blown non-woven fabric comprises the following steps:
subjecting the polypropylene composite according to any one of claims 1 to 6 to a melt treatment to obtain a melt;
and sequentially carrying out filtering spinning treatment, cooling traction treatment, net forming pre-pressing treatment and hot rolling consolidation treatment on the melt.
9. The method of claim 8, wherein: the filtering precision in the filtering spinning process is 18-22 mu m, the diameter of the filter screen is 90-110mm, the pressure intensity before filtering is 2.4-2.6MPa, the pressure intensity after filtering is 5.9-6.1MPa, the rotating speed of the metering pump is 15-20 rpm, the temperature of the metering section is 200-240 ℃, the temperature of the spinning box body is 180-220 ℃, the pressure intensity of the box body is 3.3-3.7MPa, the aperture of the spinneret plate is 0.1-0.2 mm, and the number of the holes is 10000-12000; and/or
The air volume of the suction air channel in the cooling and traction treatment process is 800-900 m3Min, and the wind pressure is 5-6 kPa; and/or
The rotating speed of the conveying belt for web-forming prepressing treatment is 10-20 m/min, and the pressure is 0.6-0.8 MPa; and/or
The rolling pressure of the hot rolling consolidation treatment is 5.5-8 MPa, and the temperature of the upper roller and/or the lower roller is 80-85 ℃.
10. A meltblown nonwoven article characterized by: is made of a polypropylene-based meltblown nonwoven fabric comprising the polypropylene-based meltblown nonwoven fabric according to claim 7 or produced by the production method according to any one of claims 8 to 9.
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