Anti-lodging and antibacterial PBT double-end one-step chemically rounded toothbrush filament and preparation method thereof

Abstract

The present invention provides a kind of anti-lodging antibacterial PBT double-end one-step chemical rounding toothbrush filament and its preparation method, and relates to the technical field of chemical fiber monofilament. The toothbrush filament provided by the present invention includes by weight: 70-80 parts of polybutylene terephthalate, 1-3 parts of anti-lodging agent, 1-2 parts of compatibilizer, 1-2 parts of antioxidant, 1-3 parts of antibacterial agent; the anti-lodging agent is a mixture of bamboo powder and modified bamboo powder, wherein the preparation method of the modified bamboo powder includes: ultrasonically dispersing bamboo powder with an average particle size of 40-50 microns in anhydrous ethanol to obtain a bamboo powder dispersion; after adding a silane coupling agent to the bamboo powder dispersion and ultrasonically mixing, separating and drying to obtain activated bamboo powder; after stirring and mixing the activated bamboo powder with an amino acid solution, reacting under neutral conditions for 4-6h, filtering and separating and drying to obtain modified bamboo powder. The present invention can improve the convenience and economy of anti-lodging treatment of toothbrush filaments, and is conducive to large-scale industrial production.

Description

Technical Field

[0001] The invention relates to the technical field of chemical fiber monofilaments, and in particular to an anti-lodging and antibacterial PBT double-end one-step chemically rounded toothbrush filament and a preparation method thereof. Background Art

[0002] Toothbrushes are an indispensable toothbrushing tool in people's daily lives. The quality of toothbrushes mainly depends on the quality of the brush filaments. Currently, toothbrush filaments mainly include polyester fibers and nylon fibers. Among them, polyester fibers are mainly PBT fibers. Compared with nylon fibers, the biggest advantage of PBT fibers is that they can be sharpened at the ends using sodium hydroxide solution as a chemical sharpening agent. After sharpening, the polyester fibers are cone-shaped. When made into toothbrushes, they can reduce damage to the gums and can penetrate into the gaps between teeth, which has a better cleaning effect.

[0003] However, the anti-lodging performance of PBT filaments is poor, which greatly restricts the further promotion and use of PBT brush filaments. The Chinese invention patent with publication number CN116288803A provides an anti-lodging PBT / PA12 sharpened toothbrush filament, which is prepared by mixing PBT and PA12 and adding an amphiphilic block copolymer with a structure similar to nylon 12 and PBT, in order to improve the compatibility of the three after blending, thereby improving the anti-lodging performance of the toothbrush filament.

[0004] However, the preparation of amphiphilic block copolymers is rather complicated, which greatly increases the economic and time costs of toothbrush filaments during the preparation process, making it difficult to carry out large-scale industrial promotion. Therefore, it is urgent to provide a relatively simple method for anti-lodging treatment of toothbrush filaments to improve the above problems. Summary of the invention

[0005] The object of the present invention is to provide a lodging-resistant and antibacterial PBT double-end one-step chemically rounded toothbrush filament and a preparation method thereof, which can improve the convenience and economy of anti-lodging treatment of toothbrush filaments and is conducive to large-scale industrial production.

[0006] In the first aspect, the present invention provides an anti-lodging and antibacterial PBT double-end one-step chemically rounded toothbrush filament, which comprises, by weight: 70-80 parts of polybutylene terephthalate, 1-3 parts of an anti-lodging agent, 1-2 parts of a compatibilizer, 1-2 parts of an antioxidant, and 1-3 parts of an antibacterial agent; the anti-lodging agent is a mixture of bamboo powder and modified bamboo powder, wherein the preparation method of the modified bamboo powder comprises: ultrasonically dispersing bamboo powder with an average particle size of 40-50 microns in anhydrous ethanol to obtain a bamboo powder dispersion; adding a silane coupling agent to the bamboo powder dispersion, ultrasonically mixing, separating and drying to obtain activated bamboo powder; stirring and mixing the activated bamboo powder with an amino acid solution, reacting under neutral conditions for 4-6 hours, and filtering, separating and drying to obtain the modified bamboo powder.

[0007] Optionally, the mass ratio of bamboo powder to modified bamboo powder in the anti-lodging agent is (0.3-1.2): (0.7-1.8).

[0008] Optionally, before the bamboo powder with an average particle size of 40-50 microns is ultrasonically dispersed in anhydrous ethanol, the bamboo powder is preheated at 80-90° C. for 2-3 hours.

[0009] Optionally, the silane coupling agent includes at least one of KH-550, KH-560, KH-570, A-171, and A-151.

[0010] Optionally, the amino acid solute in the amino acid solution includes at least one of lysine, glycine, alanine and arginine.

[0011] Optionally, the preparation method of the anti-lodging agent includes: mixing bamboo powder and modified bamboo powder and dispersing them in anhydrous ethanol to prepare a mixed suspension, and spray-drying the mixed suspension at an inlet air temperature of 120-150°C, an outlet air temperature of 60-80°C, and a pressure of 2-4 bar to obtain the anti-lodging agent.

[0012] Optionally, the compatibilizer is maleic anhydride grafted polypropylene.

[0013] Optionally, the antioxidant includes at least one of antioxidant 1010 and antioxidant 168 .

[0014] Optionally, the antibacterial agent includes at least one of silver nanoparticles and graphene oxide.

[0015] In a second aspect, the present invention provides a method for preparing anti-lodging antibacterial PBT double-end one-step chemically rounded toothbrush filaments, comprising the following steps:

[0016] After polybutylene terephthalate, an anti-lodging agent, a compatibilizer, an antioxidant and an antibacterial agent are mixed in a screw extruder, the mixture is sequentially passed through extrusion zones at 240° C., 245° C., 255° C., 265° C. and 270° C., and then the mixture is subjected to spinning cooling and forming and then cut into toothbrush filaments;

[0017] After curing the toothbrush filaments in a constant temperature environment of 30°C for 8 hours, multiple toothbrush filaments are wrapped into a brush wire cake using polytetrafluoroethylene, and both ends of the brush wire cake are exposed 0.1-5 mm outside the polytetrafluoroethylene; the brush wire cake is immersed in a 30% sodium hydroxide solution, ultrasonically treated at 80°C for 30 minutes, and then rinsed with clean water to obtain anti-lodging and antibacterial PBT double-end one-step chemically rounded toothbrush filaments. DETAILED DESCRIPTION

[0018] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Unless otherwise defined, the technical terms or scientific terms used herein should be the common meanings understood by people with general skills in the field to which the present invention belongs.

[0019] The invention provides an anti-lodging antibacterial PBT double-end one-step chemically rounded toothbrush filament, which comprises, by weight: 70-80 parts of polybutylene terephthalate, 1-3 parts of an anti-lodging agent, 1-2 parts of a compatibilizer, and 1-2 parts of

[0020] Antioxidant, 1-3 parts antibacterial agent.

[0021] In fact, polybutylene terephthalate (PBT) is the main base material for manufacturing toothbrush filaments. It has good tensile strength and impact strength, which enables the prepared toothbrush filaments to maintain their shape and function during use. In addition, PBT material also has excellent heat resistance and chemical resistance, so when people use the toothbrush filaments with toothpaste to clean their teeth, it will not damage the toothbrush filaments themselves, and it is conducive to high-temperature disinfection of the toothbrush filaments.

[0022] In fact, adding anti-lodging agent to the toothbrush filament can significantly improve the anti-lodging performance of the toothbrush filament, so that the toothbrush filament can still maintain the uprightness and elasticity of the bristles during teeth cleaning, thereby improving the performance and durability of the toothbrush filament.

[0023] Specifically, the anti-lodging agent is a mixture of bamboo powder and modified bamboo powder, wherein the preparation method of the modified bamboo powder includes: ultrasonically dispersing bamboo powder with an average particle size of 40-50 microns in anhydrous ethanol to obtain a bamboo powder dispersion; adding a silane coupling agent to the bamboo powder dispersion and ultrasonically mixing it, and then separating and drying it to obtain activated bamboo powder; stirring and mixing the activated bamboo powder and an amino acid solution, reacting them under neutral conditions for 4-6 hours, and then filtering, separating and drying it to obtain the modified bamboo powder.

[0024] In some embodiments, the mass ratio of bamboo powder to modified bamboo powder in the anti-lodging agent is (0.3-1.2): (0.7-1.8).

[0025] In some implementations, before the bamboo powder having an average particle size of 40-50 microns is ultrasonically dispersed in anhydrous ethanol, the bamboo powder is preheated at 80-90° C. for 2-3 hours.

[0026] In some embodiments, the preparation method of the anti-lodging agent includes: mixing bamboo powder and modified bamboo powder and dispersing them in anhydrous ethanol to prepare a mixed suspension, and spray-drying the mixed suspension at an inlet air temperature of 120-150°C, an outlet air temperature of 60-80°C, and a pressure of 2-4 bar to obtain the anti-lodging agent.

[0027] In some embodiments, the silane coupling agent includes at least one of KH-550, KH-560, KH-570, A-171, and A-151, and the amino acid solute in the amino acid solution includes at least one of lysine, glycine, alanine, and arginine.

[0028] In some embodiments, the compatibilizer is maleic anhydride grafted polypropylene, the antioxidant includes at least one of antioxidant 1010 and antioxidant 168, and the antibacterial agent includes at least one of silver nanoparticles and graphene oxide.

[0029] In fact, the present invention also provides a method for preparing anti-lodging antibacterial PBT double-end one-step chemically rounded toothbrush filaments, comprising the following steps:

[0030] After polybutylene terephthalate, an anti-lodging agent, a compatibilizer, an antioxidant and an antibacterial agent are mixed in a screw extruder, the mixture is sequentially passed through extrusion zones at 240° C., 245° C., 255° C., 265° C. and 270° C., and then the mixture is subjected to spinning cooling and forming and then cut into toothbrush filaments;

[0031] After curing the toothbrush filaments in a constant temperature environment of 30°C for 8 hours, multiple toothbrush filaments are wrapped into a brush wire cake using polytetrafluoroethylene, and both ends of the brush wire cake are exposed 0.1-5 mm outside the polytetrafluoroethylene; the brush wire cake is immersed in a 30% sodium hydroxide solution, ultrasonically treated at 80°C for 30 minutes, and then rinsed with clean water to obtain anti-lodging and antibacterial PBT double-end one-step chemically rounded toothbrush filaments.

[0032] Example 1 to Example 5

[0033] Embodiments 1 to 5 of the present invention respectively provide an anti-lodging and antibacterial PBT double-ended one-step chemically rounded toothbrush filament, and the specific components and amounts thereof are shown in Table 1 below.

[0034] Table 1 Components and dosages of Examples 1 to 5

[0035]

[0036] The PBT used in Examples 1 to 5 was purchased from Shanghai Mingzhi Plastics Co., Ltd. and the manufacturer was S600F20 NC010 produced by DuPont of the United States. The bamboo powder used was purchased from 300 mesh bamboo powder of Yaoyang Mineral Products Processing Plant in Lingshou County. The compatibilizer used was maleic anhydride grafted polypropylene selected from Dongguan Xinrui New Materials Co., Ltd. JYN5002. The antioxidant used was antioxidant 1010. The antibacterial agent used was nano-silver particles purchased from Jiangsu Xianfeng Nanomaterial Technology Co., Ltd.

[0037] The preparation method of the anti-lodging agent used in Examples 1 to 5 comprises:

[0038] S1. Preheat 300-mesh bamboo powder (purchased from Yaoyang Mineral Products Processing Plant, Lingshou County) at 85° C. and dehydrate for 2 h, then add the bamboo powder into anhydrous ethanol at a solid-liquid ratio of 0.08 g / mL, and disperse it ultrasonically at a frequency of 20 kHz for 20 min to obtain a bamboo powder dispersion;

[0039] S2. After adding KH-550 (the mass ratio of bamboo powder to KH-550 is 1:0.2) into the bamboo powder dispersion, dissolving and dispersing at a frequency of 20 kHz, stirring and reacting at 40° C. for 4 h, filtering and separating, and using deionized water and anhydrous ethanol to circulate and rinse the precipitate, the separated precipitate was dried in a vacuum drying oven at 60° C. to constant weight, thereby obtaining activated bamboo powder;

[0040] S3, ultrasonically mixing the activated component with a lysine aqueous solution (the mass ratio of the activated component to lysine is 1:0.2), adjusting the pH to 7.0, stirring and reacting at 40°C for 5 hours, filtering and separating, and rinsing with deionized water, and drying the separated precipitate in a vacuum drying oven at 60°C to constant weight to obtain modified bamboo powder;

[0041] S4. The modified bamboo powder and the bamboo powder are mixed and dispersed in anhydrous ethanol to prepare a mixed suspension. A spray drying device is used to set the inlet air temperature to 120° C., the outlet air temperature to 70° C., and the pressure to 3 bar, and the mixed suspension is spray-dried to obtain an anti-lodging agent.

[0042] The preparation method of the anti-lodging antibacterial PBT double-end one-step chemically rounded toothbrush filaments in Examples 1 to 5 comprises the following steps: after mixing polybutylene terephthalate, an anti-lodging agent, a compatibilizer, an antioxidant and an antibacterial agent in a screw extruder, passing through extrusion zones of 240°C, 245°C, 255°C, 265°C and 270°C in sequence, spinning cooling molding and then cutting into toothbrush filaments; after curing the toothbrush filaments in a constant temperature environment of 30°C for 8 hours, using polytetrafluoroethylene to wrap multiple toothbrush filaments into a brush filament cake, and both ends of the brush filament cake are exposed to the outside of the polytetrafluoroethylene by 5 mm; immersing the brush filament cake in a 30% sodium hydroxide solution, ultrasonically treating it at 80°C for 30 minutes, and then rinsing it with clean water to obtain the anti-lodging antibacterial PBT double-end one-step chemically rounded toothbrush filaments.

[0043] Comparative Example 1

[0044] This comparative example 1 provides a PBT double-ended one-step chemically rounded toothbrush filament, which is different from Example 2 in that no modified bamboo powder is added in comparative example 1, and the anti-lodging agent is 1.7 parts of 300-mesh bamboo powder.

[0045] Comparative Example 2

[0046] Comparative Example 2 provides a PBT double-ended one-step chemically rounded toothbrush filament, which is different from Example 2 in that no bamboo powder is added in Comparative Example 2, and the anti-lodging agent is 1.7 parts of modified bamboo powder.

[0047] Comparative Example 3

[0048] This comparative example 3 provides a PBT double-ended one-step chemically rounded toothbrush filament, which is different from Example 2 in that no anti-lodging agent is added in comparative example 3.

[0049] Performance Testing

[0050] The toothbrush filaments prepared in Examples 1 to 5 and Comparative Examples 1 to 3 were sterilized at 150°C under high pressure, and then added with 100 cfu / mL of Escherichia coli and Staphylococcus aureus solutions, respectively. After treatment at 25°C for 10 hours, the liquid was aspirated for pouring culture to count the live bacteria, and the sterilization rate was calculated. The results are shown in Table 2 below.

[0051] The toothbrush filaments prepared in Examples 1 to 5 and Comparative Examples 1 to 3 were respectively made into standard toothbrushes of the same specifications, and a lodging ratio test was performed at a speed of 13 mm / s using a weight of 335 g on the toothbrush filaments. The test time was 24 hours, and the test was repeated five times to take the average value. The lodging ratios are shown in Table 3 below. After the toothbrush filaments were aged in an oxygen atmosphere at 50°C for 48 hours, the lodging test was repeated, and the results are shown in Table 3 below.

[0052] The toothbrush filaments prepared in Examples 1 to 5 and Comparative Examples 1 to 3 were subjected to wear tests on the rounded ends of the toothbrush filaments based on the method described in GB / T3960-2016 "Test Method for Sliding Friction and Wear of Plastics". Ten tests were performed and the average wear mass was calculated. The results are shown in Table 4 below.

[0053] Table 2 Sterilization rate test results

[0054]

[0055]

[0056] Table 3 Lodging resistance test results

[0057] Lodging rate / % Lodging rate after aging / % Lodging rate / % Lodging rate after aging / % Example 1 2.31 2.59 Example 5 4.98 5.92 Example 2 2.34 2.51 Comparative Example 1 5.31 6.24 Example 3 2.30 2.55 Comparative Example 2 2.56 5.27 Example 4 2.62 5.36 Comparative Example 3 8.67 12.98

[0058] Table 4 Wear test

[0059] Wear mass / g Wear mass / g Example 1 0.127 Example 5 0.268 Example 2 0.134 Comparative Example 1 0.297 Example 3 0.129 Comparative Example 2 0.189 Example 4 0.118 Comparative Example 3 0.472

[0060] Although the embodiments of the present invention are described in detail above, it is obvious to those skilled in the art that various modifications and variations can be made to these embodiments. However, it should be understood that such modifications and variations are within the scope and spirit of the present invention as described in the claims. Moreover, the present invention described herein may have other embodiments and may be implemented or realized in a variety of ways.

Claims

1. A lodging-resistant and antibacterial PBT double-ended one-step chemically rounded toothbrush filament, characterized in that: The invention comprises, by weight, 70-80 parts of polybutylene terephthalate, 1-3 parts of an anti-lodging agent, 1-2 parts of a compatibilizer, 1-2 parts of an antioxidant, and 1-3 parts of an antibacterial agent; the anti-lodging agent is a mixture of bamboo powder and modified bamboo powder, wherein the preparation method of the modified bamboo powder comprises: ultrasonically dispersing bamboo powder with an average particle size of 40-50 microns in anhydrous ethanol to obtain a bamboo powder dispersion; adding a silane coupling agent to the bamboo powder dispersion, ultrasonically mixing the mixture, separating and drying the mixture to obtain activated bamboo powder; stirring and mixing the activated bamboo powder with an amino acid solution, reacting the mixture under neutral conditions for 4-6 hours, and filtering and separating and drying the mixture to obtain the modified bamboo powder; the mass ratio of bamboo powder to modified bamboo powder in the anti-lodging agent is (0.3-1.2):(0.7-1.8); and the compatibilizer is maleic anhydride grafted polypropylene.

2. The toothbrush filament according to claim 1, characterized in that: Before ultrasonically dispersing bamboo powder with an average particle size of 40-50 μm in anhydrous ethanol, the bamboo powder was preheated at 80-90° C. for 2-3 h.

3. The toothbrush filament according to claim 1, characterized in that: The silane coupling agent includes at least one of KH-550, KH-560, KH-570, A-171, and A-151.

4. The toothbrush filament according to claim 1, characterized in that: The amino acid solute in the amino acid solution includes at least one of lysine, glycine, alanine and arginine.

5. The toothbrush filament according to claim 1, characterized in that: The preparation method of the anti-lodging agent comprises: mixing bamboo powder and modified bamboo powder and dispersing them in anhydrous ethanol to prepare a mixed suspension, and spray-drying the mixed suspension at an inlet air temperature of 120-150° C., an outlet air temperature of 60-80° C. and a pressure of 2-4 bar to prepare the anti-lodging agent.

6. The toothbrush filament according to claim 1, characterized in that: The antioxidant includes at least one of antioxidant 1010 and antioxidant 168 .

7. The toothbrush filament according to claim 1, characterized in that: The antibacterial agent includes at least one of silver nanoparticles and graphene oxide.

8. A method for preparing the anti-lodging and antibacterial PBT double-end one-step chemically rounded toothbrush filaments according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: mixing polybutylene terephthalate, an anti-lodging agent, a compatibilizer, an antioxidant and an antibacterial agent in a screw extruder, passing through extrusion zones at 240°C, 245°C, 255°C, 265°C and 270°C in sequence, performing spinning cooling and forming, and then cutting into toothbrush filaments; curing the toothbrush filaments in a constant temperature environment at 30°C for 8 hours, using polytetrafluoroethylene to wrap a plurality of toothbrush filaments into a brush filament cake, with 0.1-5 mm of both ends of the brush filament cake exposed outside the polytetrafluoroethylene; immersing the brush filament cake in a 30% sodium hydroxide solution, ultrasonically treating the filament cake at 80°C for 30 minutes, and then rinsing the filament cake with clean water to obtain anti-lodging and antibacterial PBT double-end one-step chemically rounded toothbrush filaments.

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