Manufacturing method of longitudinal filament electrostatic fiber bundle
By modifying the structure of tourmaline powder and core-sheath composite fibers, the problem of poor compatibility of tourmaline powder in fibers was solved, achieving high-efficiency charge storage and improved filtration efficiency, as well as improved mechanical and heat resistance properties of the fibers.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-23
- Publication Date
- 2026-03-13
AI Technical Summary
Unmodified tourmaline powder has poor compatibility in fibers, leading to agglomeration and a decline in fiber mechanical properties, which affects the charge storage and filtration efficiency of electrostatic electret fibers.
Tourmaline powder is treated with a modifier to improve its compatibility in a polyethylene matrix by combining the phosphate structure with the quaternary ammonium salt structure. Uniform dispersion and efficient charge storage are achieved through a core-sheath composite fiber structure and gradient filtration channel design.
It improves fiber compatibility and dispersibility, enhances charge storage performance and filtration efficiency, reduces airflow resistance, and extends service life.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] This invention belongs to the field of dielectric fiber technology, specifically, it relates to a method for manufacturing longitudinal filament electrostatic fiber bundles. Background Technology
[0002] Electrostatic electret fiber bundles, as a core filtration material, achieve highly efficient physical adsorption of submicron-sized particles by injecting and storing persistent electrostatic charges within the fibers, without significantly increasing air resistance. To impart better charge storage capacity to the fibers, functional fillers with spontaneous polarization properties can be added during fiber preparation. Tourmaline, as a natural mineral crystal, is considered a highly promising electret filler due to its permanent spontaneous polarization effect, ability to release negative ions, and pyroelectric / piezoelectric properties. Theoretically, incorporating it into the fiber matrix in powder form can significantly enhance the fiber's charge storage capacity. However, unmodified tourmaline powder has a hydrophilic and highly polar surface, while electrostatic electret fibers are typically nonpolar or weakly polar polymers, resulting in a significant difference in surface energy and severe compatibility issues. During melt blending and spinning, untreated tourmaline powder is prone to agglomeration, failing to function as an effective charge trap for uniform distribution and becoming stress concentration points, significantly deteriorating the fiber's mechanical properties. To address these technical shortcomings, this invention provides a method for manufacturing longitudinal filament electrostatic fiber bundles. Summary of the Invention
[0003] The purpose of this invention is to provide a method for manufacturing longitudinal filament electrostatic fiber bundles to solve the problems mentioned in the background art.
[0004] The objective of this invention can be achieved through the following technical solutions: A method for preparing a longitudinal filament electrostatic fiber bundle includes the following steps: The first step involves activating 2-chloroethyl phosphoric acid and then reacting it with 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide via a nucleophilic substitution reaction. The resulting product is then hydrolyzed to obtain an intermediate. The second step involves reacting the intermediate with tri-hexadecylamine as a quaternary ammonium salt to obtain the modifier. The third step is to load the modifier onto the surface of the filler to obtain the modified filler; Step 4: Melt extrusion granulation of polyethylene, modified filler, and antioxidant to obtain core layer masterbatch, and melt extrusion granulation of polypropylene and antioxidant to obtain skin layer masterbatch; Step 5: The core masterbatch and the sheath masterbatch are melt-spun to obtain core-sheath composite modified fibers. Then, the core-sheath composite modified fibers are stacked to obtain fiber bundles. The fiber bundles are then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundles.
[0005] Preferably, the filler is at least one of black tourmaline, magnesium tourmaline, and lithium tourmaline.
[0006] Preferably, the antioxidant is at least one of antioxidant 1010, antioxidant 1076, and antioxidant 168.
[0007] Preferably, the temperature conditions for the melt extrusion of the core layer masterbatch are 170–200°C.
[0008] Preferably, the temperature conditions for the melt extrusion of the skin masterbatch are 190–220°C.
[0009] Preferably, the parameters for melt spinning are: spinning temperature 200-230℃, draw ratio 2.5-4.0, and winding speed 800-1500 m / min.
[0010] Preferably, the modifier is loaded onto the filler surface in the following manner: The filler is crushed, washed, and dried to obtain filler powder. The filler powder, modifier, and N,N-dimethylformamide are then mixed in a container and ultrasonically dispersed. The mixture is then reacted at a temperature of 45–85℃ for 6–24 hours. After the reaction is completed, the solid is filtered to separate the solid and then washed with anhydrous ethanol and deionized water in sequence before drying to obtain the modified filler.
[0011] Preferably, the mass ratio of the modifier to the filler powder is 4-10:8-15.
[0012] Preferably, the core-sheath composite modified fiber is laminated in the following manner: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
[0013] Preferably, the parameters for the corona electret treatment are: voltage 30-60 kV and treatment time 10-60 s.
[0014] Preferably, the parameters for the water electret treatment are: water pressure 5-15 MPa and treatment time 5-15 s.
[0015] Preferably, the heat treatment parameters are: temperature 80–100°C, time 5–15 min.
[0016] Preferably, the mass ratio of polyethylene, modified filler, and antioxidant used is 100:8-15:0.3-1.
[0017] Preferably, the mass ratio of polypropylene to antioxidant used is 100:0.3 to 0.8.
[0018] Preferably, the mass ratio of the core layer masterbatch to the skin layer masterbatch is 60-70:30-40.
[0019] The beneficial effects of this invention are: This invention prepares a modifier capable of being loaded onto the surface of tourmaline. This modifier contains both a phosphate structure and a quaternary ammonium salt structure. The phosphate structure can form stable coordination bonds with metal ions on the tourmaline surface, while the quaternary ammonium salt structure can further stabilize the bond between the modifier and the tourmaline surface through electrostatic adsorption, laying the foundation for subsequent functionalization. After loading and modifying tourmaline, the long-chain alkyl structure in the modifier effectively improves the compatibility between tourmaline and the polyethylene matrix. This improved compatibility promotes the uniform dispersion of the modified tourmaline powder within the polyethylene matrix. Uniform dispersion not only helps improve the loading efficiency of the filler and enhances the breaking strength of the finished fiber, but also improves the dielectric properties and charge storage properties of the finished fiber, enhances its heat resistance, and reduces the charge storage density decay rate of the finished fiber under high-temperature operating conditions.
[0020] The modifier of this invention not only improves the compatibility and dispersibility of modified tourmaline powder in polyethylene matrix, but also significantly enhances pseudocapacitive performance and is used for efficient capacitive ion adsorption due to the extended π-conjugated plane and increased redox active sites of the sulfur-oxygen heterocyclic structure. Meanwhile, the quaternary ammonium salt structure can build an electrostatic field inside the fiber, significantly improving electrocatalytic performance. The synergistic effect of the two can further enhance the local charge storage capacity of the fiber and improve the electrostatic dust removal efficiency.
[0021] This invention uses polypropylene as the sheath, providing excellent mechanical strength, heat resistance, and spinnability; and polyethylene loaded with modified tourmaline as the core layer, serving as the functional core for charge generation and storage. This structure protects the sensitive internal functional fillers and charges while ensuring the overall spinnability and mechanical properties of the fiber.
[0022] Fibers of different fineness are layered according to function (windward coarse layer, core high-efficiency layer, and leeward support layer) and then stacked using a cross-laying technique. This design creates a three-dimensional gradient filtration channel that progresses from loose to dense, and from coarse interception to high-efficiency electrostatic adsorption. This enables the progressively efficient capture of particles of different sizes, effectively reducing airflow resistance and extending service life while ensuring extremely high filtration efficiency. Detailed Implementation
[0023] This invention provides a method for fabricating longitudinal filament electrostatic fiber bundles. Those skilled in the art can refer to the content of this document and appropriately modify the process parameters to achieve the desired result. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art and fall within the scope of protection of this invention. The method and application of this invention have been described through preferred embodiments. Those skilled in the art can clearly modify or appropriately change and combine the method and application described herein without departing from the content, spirit, and scope of this invention to realize and apply the technology of this invention.
[0024] It should be understood that the expression “one or more of…” individually includes each of the objects described after the expression, as well as various different combinations of two or more of the described objects, unless otherwise understood from the context and usage. The expression “and / or” combined with three or more described objects should be understood to have the same meaning, unless otherwise understood from the context.
[0025] The terms “including,” “having,” or “containing,” including the use of their grammatical synonyms, should generally be understood as open-ended and non-restrictive, for example, not excluding other unstated elements or steps, unless otherwise specifically stated or understood from the context.
[0026] In this application, the term "and / or" describes the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. A and B can be singular or plural.
[0027] In this application, "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of single or multiple items.
[0028] It should be understood that the order of the steps or the order in which certain actions are performed is not important as long as the invention remains operational. Furthermore, two or more steps or actions can be performed simultaneously.
[0029] The use of any and all instances or exemplary language such as “e.g.” or “including” in this document is merely intended to better illustrate the invention and is not intended to limit the scope of the invention unless the claims are made. No language in this specification should be construed as indicating that any unclaimed element is essential to the practice of the invention.
[0030] Furthermore, the numerical ranges and parameters used to define the present invention are approximate values, and the relevant values in the specific embodiments have been presented as precisely as possible. However, any value inevitably contains standard deviations due to individual test methods. Therefore, unless explicitly stated otherwise, it should be understood that all ranges, quantities, values, and percentages used in this disclosure are modified with the word "approximately". Here, "approximately" generally means that the actual value is within plus or minus 10%, 5%, 1%, or 0.5% of a specific value or range.
[0031] It should be understood that in the various embodiments of this application, the order of the above processes does not imply the order of execution. Some or all steps may be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.
[0032] The embodiments and comparative examples of this invention describe some examples, in which the embodiments illustrate certain implementations of the invention. However, this does not mean that the effects of the invention can only be achieved in these examples.
[0033] To further illustrate the present invention, the following describes in detail a method for manufacturing a longitudinal filament electrostatic fiber bundle provided by the present invention, in conjunction with embodiments. Example 1
[0034] A method for preparing a longitudinal filament electrostatic fiber bundle includes the following steps: Step 1: By mass, 1.4 parts of 2-chloroethyl phosphoric acid, 3.4 parts of thionyl chloride, and 0.2 parts of N,N-dimethylformamide were mixed in a reaction vessel under ice-water bath conditions. After stirring, the ice-water bath was removed, and the mixture was reacted at 50°C for 4 hours. After the reaction, excess thionyl chloride was removed by rotary evaporation. The remaining liquid was then mixed with 1 part of 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide, 0.9 parts of triethylamine, and 20 parts of N,N-dimethylformamide in a new reaction vessel. The mixture was stirred, and the mixture was reacted at room temperature for 2 hours. Then, 4 parts of deionized water were added to the system, and the reaction was continued at room temperature for 4 hours. After the reaction, the mixture was extracted with ethyl acetate. The organic phase was then separated, and the solvent was removed by rotary evaporation. The remaining solid was eluted by silica gel column chromatography to obtain the intermediate.
[0035] Step 2: According to the mass fraction, 1.4 parts of intermediate, 5 parts of tri-hexadecylamine, 1 part of potassium carbonate, and 30 parts of N,N-dimethylformamide are mixed in a reaction vessel. After stirring, the mixture is reacted at 60°C for 24 hours. After the reaction is completed, the reaction solution is poured into n-hexane to precipitate. After filtering and separating the precipitate, the precipitate is washed successively with dilute hydrochloric acid and deionized water and then dried to obtain the modifier.
[0036] The third step involves crushing, cleaning, and drying the filler to obtain filler powder by mass fraction. Then, 8 parts of filler powder, 4 parts of modifier, and 60 parts of N,N-dimethylformamide are mixed in a container, ultrasonically dispersed evenly, and reacted at 45°C for 24 hours. After the reaction is completed, the solid is filtered to separate it, and the obtained solid is washed with anhydrous ethanol and deionized water in sequence and then dried to obtain modified filler.
[0037] Step 4: Based on the mass fractions, melt extrude and granulate 100 parts polyethylene, 8 parts modified filler, and 0.3 parts antioxidant to obtain core layer masterbatch, and melt extrude and granulate 100 parts polypropylene and 0.3 parts antioxidant to obtain skin layer masterbatch. Step 5: According to the mass fraction, 60 parts of core layer masterbatch and 40 parts of sheath masterbatch are melt-spun to obtain core-sheath composite modified fiber. Then, the core-sheath composite modified fiber is stacked to obtain fiber bundle. The fiber bundle is then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundle.
[0038] In this embodiment, the filler used is black tourmaline, and the antioxidant used is a mixture of antioxidant 1010 and antioxidant 168 in a mass ratio of 4:1.
[0039] In this embodiment, the temperature conditions for the melt extrusion of the core layer masterbatch are 170°C, the temperature conditions for the melt extrusion of the skin layer masterbatch are 190°C, and the parameters for the melt spinning are: spinning temperature 200°C, draw ratio 2.5, and winding speed 800 m / min.
[0040] In this embodiment, the method of stacking the core-sheath composite modified fibers is as follows: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
[0041] In this embodiment, the parameters for corona electret treatment are: voltage 30KV, treatment time 60s, and the parameters for water electret treatment are: water pressure 5MPa, treatment time 15s. Example 2
[0042] A method for preparing a longitudinal filament electrostatic fiber bundle includes the following steps: Step 1: By mass, 1.4 parts of 2-chloroethyl phosphoric acid, 3.4 parts of thionyl chloride, and 0.2 parts of N,N-dimethylformamide were mixed in a reaction vessel under ice-water bath conditions. After stirring, the ice-water bath was removed, and the mixture was reacted at 50°C for 4 hours. After the reaction, excess thionyl chloride was removed by rotary evaporation. The remaining liquid was then mixed with 1 part of 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide, 0.9 parts of triethylamine, and 20 parts of N,N-dimethylformamide in a new reaction vessel. The mixture was stirred, and the mixture was reacted at room temperature for 2 hours. Then, 4 parts of deionized water were added to the system, and the reaction was continued at room temperature for 4 hours. After the reaction, the mixture was extracted with ethyl acetate. The organic phase was then separated, and the solvent was removed by rotary evaporation. The remaining solid was eluted by silica gel column chromatography to obtain the intermediate.
[0043] Step 2: According to the mass fraction, 1.4 parts of intermediate, 5 parts of tri-hexadecylamine, 1 part of potassium carbonate, and 30 parts of N,N-dimethylformamide are mixed in a reaction vessel. After stirring, the mixture is reacted at 60°C for 24 hours. After the reaction is completed, the reaction solution is poured into n-hexane to precipitate. After filtering and separating the precipitate, the precipitate is washed successively with dilute hydrochloric acid and deionized water and then dried to obtain the modifier.
[0044] The third step involves crushing, cleaning, and drying the filler to obtain filler powder by mass fraction. Then, 8 parts of filler powder, 4 parts of modifier, and 60 parts of N,N-dimethylformamide are mixed in a container, ultrasonically dispersed evenly, and reacted at 45°C for 24 hours. After the reaction is completed, the solid is filtered to separate it, and the obtained solid is washed with anhydrous ethanol and deionized water in sequence and then dried to obtain modified filler.
[0045] Step 4: Based on the mass fractions, melt extrude and granulate 100 parts polyethylene, 8 parts modified filler, and 0.3 parts antioxidant to obtain core layer masterbatch, and melt extrude and granulate 100 parts polypropylene and 0.3 parts antioxidant to obtain skin layer masterbatch. Step 5: According to the mass fraction, 60 parts of core layer masterbatch and 40 parts of sheath masterbatch are melt-spun to obtain core-sheath composite modified fiber. Then, the core-sheath composite modified fiber is stacked to obtain fiber bundle. The fiber bundle is then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundle.
[0046] In this embodiment, the filler used is magnesium tourmaline, and the antioxidant used is a mixture of antioxidant 1010 and antioxidant 168 in a mass ratio of 4:1.
[0047] In this embodiment, the temperature conditions for the melt extrusion of the core layer masterbatch are 170°C, the temperature conditions for the melt extrusion of the skin layer masterbatch are 190°C, and the parameters for the melt spinning are: spinning temperature 200°C, draw ratio 2.5, and winding speed 800 m / min.
[0048] In this embodiment, the method of stacking the core-sheath composite modified fibers is as follows: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
[0049] In this embodiment, the parameters for corona electret treatment are: voltage 30KV, treatment time 60s, and the parameters for water electret treatment are: water pressure 5MPa, treatment time 15s. Example 3
[0050] A method for preparing a longitudinal filament electrostatic fiber bundle includes the following steps: Step 1: By mass, 2.5 parts of 2-chloroethyl phosphoric acid, 6 parts of thionyl chloride, and 0.4 parts of N,N-dimethylformamide were mixed in a reaction vessel under ice-water bath conditions. After stirring, the ice-water bath was removed, and the mixture was reacted at 55°C for 3 hours. After the reaction, excess thionyl chloride was removed by rotary evaporation. The remaining liquid was then mixed with 1.75 parts of 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide, 1.6 parts of triethylamine, and 35 parts of N,N-dimethylformamide in a new reaction vessel. The mixture was stirred, and the mixture was reacted at room temperature for 1.5 hours. Then, 7 parts of deionized water were added to the system, and the reaction was continued at room temperature for 3 hours. After the reaction, the mixture was extracted with ethyl acetate. The organic phase was then separated, and the solvent was removed by rotary evaporation. The remaining solid was eluted by silica gel column chromatography to obtain the intermediate.
[0051] Step 2: According to the mass fraction, 2.5 parts of intermediate, 9 parts of tri-hexadecylamine, 1.75 parts of potassium carbonate, and 55 parts of N,N-dimethylformamide are mixed in a reaction vessel. After stirring, the mixture is reacted at 80℃ for 17 hours. After the reaction is completed, the reaction solution is poured into n-hexane to precipitate. After filtering and separating the precipitate, the precipitate is washed with dilute hydrochloric acid and deionized water in sequence and then dried to obtain the modifier.
[0052] The third step involves crushing, cleaning, and drying the filler to obtain filler powder by mass fraction. Then, 11.5 parts of filler powder, 7 parts of modifier, and 90 parts of N,N-dimethylformamide are mixed in a container, ultrasonically dispersed, and reacted at 65°C for 15 hours. After the reaction is completed, the solid is filtered to separate it, and the obtained solid is washed with anhydrous ethanol and deionized water in sequence and then dried to obtain modified filler.
[0053] Step 4: Based on mass parts, melt extrude and granulate 100 parts polyethylene, 11.5 parts modified filler, and 0.65 parts antioxidant to obtain core layer masterbatch, and melt extrude and granulate 100 parts polypropylene and 0.55 parts antioxidant to obtain skin layer masterbatch. Step 5: According to the mass fraction, 65 parts of core layer masterbatch and 35 parts of sheath masterbatch are melt-spun to obtain core-sheath composite modified fiber. Then, the core-sheath composite modified fiber is stacked to obtain fiber bundle. The fiber bundle is then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundle.
[0054] In this embodiment, the filler used is lithium tourmaline, and the antioxidant used is a mixture of antioxidant 1076 and antioxidant 168 in a mass ratio of 3:1.
[0055] In this embodiment, the core layer masterbatch melt extrusion temperature is 185℃, the skin layer masterbatch melt extrusion temperature is 205℃, and the melt spinning parameters are: spinning temperature 215℃, draw ratio 3.25, and winding speed 1150 m / min.
[0056] In this embodiment, the method of stacking the core-sheath composite modified fibers is as follows: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
[0057] In this embodiment, the parameters for corona electret treatment are: voltage 45KV, treatment time 35s, and the parameters for water electret treatment are: water pressure 10MPa, treatment time 10s. Example 4
[0058] A method for preparing a longitudinal filament electrostatic fiber bundle includes the following steps: Step 1: By mass, 2.5 parts of 2-chloroethyl phosphoric acid, 6 parts of thionyl chloride, and 0.4 parts of N,N-dimethylformamide were mixed in a reaction vessel under ice-water bath conditions. After stirring, the ice-water bath was removed, and the mixture was reacted at 55°C for 3 hours. After the reaction, excess thionyl chloride was removed by rotary evaporation. The remaining liquid was then mixed with 1.75 parts of 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide, 1.6 parts of triethylamine, and 35 parts of N,N-dimethylformamide in a new reaction vessel. The mixture was stirred, and the mixture was reacted at room temperature for 1.5 hours. Then, 7 parts of deionized water were added to the system, and the reaction was continued at room temperature for 3 hours. After the reaction, the mixture was extracted with ethyl acetate. The organic phase was then separated, and the solvent was removed by rotary evaporation. The remaining solid was eluted by silica gel column chromatography to obtain the intermediate.
[0059] Step 2: According to the mass fraction, 2.5 parts of intermediate, 9 parts of tri-hexadecylamine, 1.75 parts of potassium carbonate, and 55 parts of N,N-dimethylformamide are mixed in a reaction vessel. After stirring, the mixture is reacted at 80℃ for 17 hours. After the reaction is completed, the reaction solution is poured into n-hexane to precipitate. After filtering and separating the precipitate, the precipitate is washed with dilute hydrochloric acid and deionized water in sequence and then dried to obtain the modifier.
[0060] The third step involves crushing, cleaning, and drying the filler to obtain filler powder by mass fraction. Then, 11.5 parts of filler powder, 7 parts of modifier, and 90 parts of N,N-dimethylformamide are mixed in a container, ultrasonically dispersed, and reacted at 65°C for 15 hours. After the reaction is completed, the solid is filtered to separate it, and the obtained solid is washed with anhydrous ethanol and deionized water in sequence and then dried to obtain modified filler.
[0061] Step 4: Based on mass parts, melt extrude and granulate 100 parts polyethylene, 11.5 parts modified filler, and 0.65 parts antioxidant to obtain core layer masterbatch, and melt extrude and granulate 100 parts polypropylene and 0.55 parts antioxidant to obtain skin layer masterbatch. Step 5: According to the mass fraction, 65 parts of core layer masterbatch and 35 parts of sheath masterbatch are melt-spun to obtain core-sheath composite modified fiber. Then, the core-sheath composite modified fiber is stacked to obtain fiber bundle. The fiber bundle is then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundle.
[0062] In this embodiment, the filler is a mixture of black tourmaline and lithium tourmaline in a mass ratio of 1:1, and the antioxidant is a mixture of antioxidant 1076 and antioxidant 168 in a mass ratio of 3:1.
[0063] In this embodiment, the core layer masterbatch melt extrusion temperature is 185℃, the skin layer masterbatch melt extrusion temperature is 205℃, and the melt spinning parameters are: spinning temperature 215℃, draw ratio 3.25, and winding speed 1150 m / min.
[0064] In this embodiment, the method of stacking the core-sheath composite modified fibers is as follows: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
[0065] In this embodiment, the parameters for corona electret treatment are: voltage 45KV, treatment time 35s, and the parameters for water electret treatment are: water pressure 10MPa, treatment time 10s. Example 5
[0066] A method for preparing a longitudinal filament electrostatic fiber bundle includes the following steps: Step 1: By mass, 3.6 parts of 2-chloroethyl phosphoric acid, 8.6 parts of thionyl chloride, and 0.6 parts of N,N-dimethylformamide were mixed in a reaction vessel under ice-water bath conditions. After stirring, the ice-water bath was removed, and the mixture was reacted at 60°C for 2 hours. After the reaction, excess thionyl chloride was removed by rotary evaporation. The remaining liquid was then mixed with 2.5 parts of 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide, 2.3 parts of triethylamine, and 50 parts of N,N-dimethylformamide in a new reaction vessel. The mixture was stirred, and the mixture was reacted at room temperature for 1 hour. Then, 10 parts of deionized water were added to the system, and the reaction was continued at room temperature for 2 hours. After the reaction, the mixture was extracted with ethyl acetate. The organic phase was then separated, and the solvent was removed by rotary evaporation. The remaining solid was eluted by silica gel column chromatography to obtain the intermediate.
[0067] Step 2: According to the mass fractions, 3.6 parts of intermediate, 13 parts of tri-hexadecylamine, 2.5 parts of potassium carbonate, and 80 parts of N,N-dimethylformamide are mixed in a reaction vessel. After stirring, the mixture is reacted at 100℃ for 10 hours. After the reaction is completed, the reaction solution is poured into n-hexane to precipitate. After filtering to separate the precipitate, the precipitate is washed successively with dilute hydrochloric acid and deionized water and then dried to obtain the modifier.
[0068] The third step involves crushing, cleaning, and drying the filler to obtain filler powder by mass fraction. Then, 15 parts of filler powder, 10 parts of modifier, and 120 parts of N,N-dimethylformamide are mixed in a container, ultrasonically dispersed evenly, and reacted at 85°C for 6 hours. After the reaction is completed, the solid is filtered to separate it, and the obtained solid is washed with anhydrous ethanol and deionized water in sequence and then dried to obtain modified filler.
[0069] Step 4: Based on the mass fractions, melt extrude and granulate 100 parts polyethylene, 15 parts modified filler, and 1 part antioxidant to obtain core layer masterbatch, and melt extrude and granulate 100 parts polypropylene and 0.8 parts antioxidant to obtain skin layer masterbatch. Step 5: According to the mass fraction, 70 parts of core layer masterbatch and 30 parts of sheath masterbatch are melt-spun to obtain core-sheath composite modified fiber. Then, the core-sheath composite modified fiber is stacked to obtain fiber bundle. The fiber bundle is then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundle.
[0070] In this embodiment, the filler is a mixture of black tourmaline and magnesium tourmaline in a mass ratio of 1:1, and the antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a mass ratio of 3.5:1.
[0071] In this embodiment, the core layer masterbatch melt extrusion temperature is 200℃, the skin layer masterbatch melt extrusion temperature is 220℃, and the melt spinning parameters are: spinning temperature 230℃, draw ratio 4.0, and winding speed 1500 m / min.
[0072] In this embodiment, the method of stacking the core-sheath composite modified fibers is as follows: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
[0073] In this embodiment, the parameters for corona electret treatment are: voltage 60KV, treatment time 10s, and the parameters for water electret treatment are: water pressure 15MPa, treatment time 5s. Example 6
[0074] A method for preparing a longitudinal filament electrostatic fiber bundle includes the following steps: Step 1: By mass, 3.6 parts of 2-chloroethyl phosphoric acid, 8.6 parts of thionyl chloride, and 0.6 parts of N,N-dimethylformamide were mixed in a reaction vessel under ice-water bath conditions. After stirring, the ice-water bath was removed, and the mixture was reacted at 60°C for 2 hours. After the reaction, excess thionyl chloride was removed by rotary evaporation. The remaining liquid was then mixed with 2.5 parts of 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide, 2.3 parts of triethylamine, and 50 parts of N,N-dimethylformamide in a new reaction vessel. The mixture was stirred, and the mixture was reacted at room temperature for 1 hour. Then, 10 parts of deionized water were added to the system, and the reaction was continued at room temperature for 2 hours. After the reaction, the mixture was extracted with ethyl acetate. The organic phase was then separated, and the solvent was removed by rotary evaporation. The remaining solid was eluted by silica gel column chromatography to obtain the intermediate.
[0075] Step 2: According to the mass fractions, 3.6 parts of intermediate, 13 parts of tri-hexadecylamine, 2.5 parts of potassium carbonate, and 80 parts of N,N-dimethylformamide are mixed in a reaction vessel. After stirring, the mixture is reacted at 100℃ for 10 hours. After the reaction is completed, the reaction solution is poured into n-hexane to precipitate. After filtering to separate the precipitate, the precipitate is washed successively with dilute hydrochloric acid and deionized water and then dried to obtain the modifier.
[0076] The third step involves crushing, cleaning, and drying the filler to obtain filler powder by mass fraction. Then, 15 parts of filler powder, 10 parts of modifier, and 120 parts of N,N-dimethylformamide are mixed in a container, ultrasonically dispersed evenly, and reacted at 85°C for 6 hours. After the reaction is completed, the solid is filtered to separate it, and the obtained solid is washed with anhydrous ethanol and deionized water in sequence and then dried to obtain modified filler.
[0077] Step 4: Based on the mass fractions, melt extrude and granulate 100 parts polyethylene, 15 parts modified filler, and 1 part antioxidant to obtain core layer masterbatch, and melt extrude and granulate 100 parts polypropylene and 0.8 parts antioxidant to obtain skin layer masterbatch. Step 5: According to the mass fraction, 70 parts of core layer masterbatch and 30 parts of sheath masterbatch are melt-spun to obtain core-sheath composite modified fiber. Then, the core-sheath composite modified fiber is stacked to obtain fiber bundle. The fiber bundle is then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundle.
[0078] In this embodiment, the filler is a mixture of magnesium tourmaline and lithium tourmaline in a mass ratio of 1:1, and the antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a mass ratio of 3.5:1.
[0079] In this embodiment, the core layer masterbatch melt extrusion temperature is 200℃, the skin layer masterbatch melt extrusion temperature is 220℃, and the melt spinning parameters are: spinning temperature 230℃, draw ratio 4.0, and winding speed 1500 m / min.
[0080] In this embodiment, the method of stacking the core-sheath composite modified fibers is as follows: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
[0081] In this embodiment, the parameters for corona electret treatment are: voltage 60KV, treatment time 10s, and the parameters for water electret treatment are: water pressure 15MPa, treatment time 5s.
[0082] Comparative Example 1 The difference between this comparative example and Example 6 is that no modifier is prepared and no tourmaline powder is modified, while the mass fractions of the remaining raw materials and the preparation conditions remain unchanged.
[0083] Experimental Example 1 The initial filtration efficiency of the electrostatic fiber bundles prepared in Examples 1-6 and Comparative Example 1 on 0.3 μm NaCl aerosol particles was tested at an air velocity of 32 L / min. The filtration efficiency was repeated after hot air treatment (60℃, 24 h). The longitudinal tensile strength of each component of the electrostatic fiber was tested according to the national standard GB / T 24218.3-2010 "Textiles - Nonwovens - Test Methods - Part 3: Determination of breaking strength and elongation at break". The test results are shown in Table 1. Table 1
[0084] As can be seen from Table 1, the fiber bundles of the present invention in Examples 1 to 6 all have better initial filtration efficiency and heat resistance, and are relatively less prone to breakage. However, the fiber bundles in Comparative Example 1 have poor compatibility with the internal components of the filler, tourmaline, which has not been modified, resulting in a significant decrease in the heat resistance and breaking strength of the finished fiber.
[0085] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A method for fabricating a longitudinal filament electrostatic fiber bundle, characterized in that, Includes the following steps: The first step involves activating 2-chloroethyl phosphoric acid and then reacting it with 3-hydroxy-2,3-dihydrothiophene 1,1-dioxide via a nucleophilic substitution reaction. The resulting product is then hydrolyzed to obtain an intermediate. The second step involves reacting the intermediate with tri-hexadecylamine as a quaternary ammonium salt to obtain the modifier. The third step is to load the modifier onto the surface of the filler to obtain the modified filler; Step 4: Melt extrusion granulation of polyethylene, modified filler, and antioxidant to obtain core layer masterbatch, and melt extrusion granulation of polypropylene and antioxidant to obtain skin layer masterbatch; Step 5: The core masterbatch and the sheath masterbatch are melt-spun to obtain core-sheath composite modified fibers. Then, the core-sheath composite modified fibers are stacked to obtain fiber bundles. The fiber bundles are then subjected to corona electret treatment, water electret treatment and heat treatment in sequence to obtain longitudinal filament electrostatic fiber bundles.
2. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The filler is at least one of black tourmaline, magnesium tourmaline, and lithium tourmaline, and the antioxidant is at least one of antioxidant 1010, antioxidant 1076, and antioxidant 168.
3. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The core layer masterbatch is melt-extruded at a temperature of 170–200°C, the skin layer masterbatch is melt-extruded at a temperature of 190–220°C, and the melt spinning parameters are: spinning temperature 200–230°C, draw ratio 2.5–4.0, and winding speed 800–1500 m / min.
4. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The method of laminating the core-sheath composite modified fibers is as follows: Based on the different fiber fineness, fibers with a fineness ≥3D and ≤10D are divided into the windward layer (coarse efficiency layer), fibers with a fineness >1.5D and <3D are divided into the leeward layer (support layer), and fibers with a fineness ≤1.5D are divided into the core layer (high efficiency layer). Then, the three types of fibers are opened, mixed, and carded to obtain the corresponding fiber webs. Then, according to the cross-laying technology, the three types of fiber webs are stacked in the order of windward layer fiber web → core layer fiber web → leeward layer fiber web.
5. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The parameters for the corona electret treatment are: voltage 30-60 kV, treatment time 10-60 s.
6. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The parameters for the water electret treatment are: water pressure 5-15 MPa, treatment time 5-15 s.
7. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The parameters for the heat treatment are: temperature 80–100℃, time 5–15 min.
8. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The mass ratio of polyethylene, modified filler, and antioxidant used is 100:8-15:0.3-1; the mass ratio of polypropylene and antioxidant used is 100:0.3-0.8; and the mass ratio of core layer masterbatch and skin layer masterbatch used is 60-70:30-40.
9. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 1, characterized in that, The modifier is loaded onto the filler surface in the following manner: The filler is crushed, washed, and dried to obtain filler powder. The filler powder, modifier, and N,N-dimethylformamide are then mixed in a container and ultrasonically dispersed. The mixture is then reacted at a temperature of 45–85℃ for 6–24 hours. After the reaction is completed, the solid is filtered to separate the solid and then washed with anhydrous ethanol and deionized water in sequence before drying to obtain the modified filler.
10. The method for preparing a longitudinal filament electrostatic fiber bundle according to claim 9, characterized in that, The mass ratio of the modifier to the filler powder used is 4-10:8-15.