Material for preparing polymeric air fibers, and preparation method therefor and use thereof

By doping modified ceramic powder and magnetic iron oxide into polymer air fibers and treating them with chitosan solution, a polymer air fiber material with excellent mechanical and antibacterial properties was prepared. This solved the problems of complex preparation process and insufficient mechanical durability, and achieved the environmental protection, comfort and support effects of the mattress.

WO2026056576A1PCT designated stage Publication Date: 2026-03-19YIN HUI
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Patent Information

Application Number
PCT/CN2025/112444
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-09-14
Filing Date
2025-08-04
Publication Date
2026-03-19

AI Technical Summary

Technical Problem

The preparation process of high-polymer air fibers is complex and requires harsh conditions, which can easily lead to product quality problems, high costs, insufficient mechanical durability, and easy collapse after long-term use.

Method used

Modified ceramic powder was uniformly dispersed in TPEE air fiber membrane. Antibacterial TiO2/ZnO/ZrO2 ceramic powder was doped, magnetic iron oxide was deposited, and after surface modification, water-soluble chitosan solution was added to prepare polymer air fiber material. The TPEE air fiber membrane was obtained by heating reaction with genipin solution.

Benefits of technology

The mechanical and antibacterial properties of the material have been improved, the photocatalytic activity has been broadened, and it has far-infrared heating function, which can improve sleep and regulate immunity. The resulting mattress is more environmentally friendly, hygienic, and comfortable, and has better support and rigidity for long-term use.

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Abstract

The present invention belongs to the technical field of home furnishings, and provides a material for preparing polymeric air fibers, and a preparation method therefor and the use thereof. The preparation method comprises: preparing a ceramic powder doped with antibacterial TiO2 / ZnO / ZrO2; depositing magnetic ferroferric oxide thereon; after the surface is modified by tannic acid, adding same to a water-soluble chitosan solution; immersing same in a TPEE air fiber membrane prepared by means of melt-blowing; uniformly adding a genipin solution dropwise; heating and reacting same; and taking out the membrane, washing and drying same to obtain a material for preparing polymeric air fibers. The TPEE air fiber membrane prepared in the present invention has good mechanical properties, and the modified ceramic powder is uniformly dispersed in the TPEE air fiber membrane, achieving good antibacterial, environmental protection, immunity regulation, magnetic therapy, far-infrared heating and other effects, such that the prepared material for preparing polymeric air fibers has better overall performance. Thus, the material is a good mattress support material, and has broad application prospects.
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Description

Material for making high polymer air fiber and preparation method and application thereof TECHNICAL FIELD

[0001] The present application relates to the technical field of home furnishing, in particular to a material for making high polymer air fiber and a preparation method and application thereof. BACKGROUND

[0002] The softness and hardness of a mattress can affect sleep quality, and is an important indicator of mattress comfort evaluation. Both softness and hardness can cause discomfort after waking up, and even affect the user's physical health. High polymer air fiber is a new type of mattress material, which has many characteristics and advantages. According to search results, air fiber mattresses are usually made of high polymer materials, forming a 3D fiber weaving structure. Air fiber mattress is a modern sleep solution that combines comfort, support and easy cleaning, providing a healthy and comfortable sleep environment for users. The main advantages of this mattress include:

[0003] 1. Good air permeability and strong support: Air fiber mattress has good air permeability due to its special structure, and provides sufficient support, making sleep more comfortable. The air permeability of this mattress helps to keep the mattress dry, reduces the feeling of dampness and stuffiness, and also helps to reduce the breeding of mites.

[0004] 2. Washable: Compared with traditional mattresses, air fiber mattresses can be directly washed with water, which makes it more convenient to clean the mattress, and also can more effectively remove stains and allergens.

[0005] 3. Adjustable hardness: Some air fiber mattresses are designed with different hardness areas, and users can adjust the hardness of the mattress according to their own preferences and physical needs to achieve the best sleep experience.

[0006] 4. Environmentally friendly materials: Air fiber mattresses are usually made of environmentally friendly materials, which do not contain formaldehyde, latex and other substances that may cause allergies, making them a better choice for people with allergies.

[0007] 5. Lightweight and easy to move: Due to the special nature of the material, air fiber mattresses are usually lighter than traditional mattresses, making them easy to move and place.

[0008] 6. Suitable for specific groups: Air fiber mattresses are particularly suitable for teenagers whose bones are still developing, people with back problems or poor sleep quality, and users who prefer a harder mattress. TECHNICAL PROBLEM

[0009] However, the preparation process of the high polymer air fiber is complex and the conditions are harsh, which can easily lead to product quality problems, and the cost is high, the mechanical durability is insufficient, and the long-term use is prone to collapse and other problems. Technical solution

[0010] The application aims to provide a material for making high polymer air fibers and a preparation method and application thereof, which has good mechanical properties, and the modified ceramic powder is uniformly dispersed in the TPEE air fiber film, thereby achieving good antibacterial, environmental protection, immune regulation, magnetic therapy, far infrared heating and other effects, so that the material for making high polymer air fibers has better comprehensive performance, is a better mattress support material and has a wide application prospect.

[0011] The technical solution of the application is implemented as follows:

[0012] The application provides a preparation method of a material for making high polymer air fibers, which comprises the following steps: preparing doped antibacterial TiO2 / ZnO / ZrO2 ceramic powder, depositing magnetic ferroferric oxide, adding the modified tannic acid to the surface, adding water-soluble chitosan solution, immersing a TPEE air fiber film prepared by melt blowing into the solution, uniformly adding genipin solution, heating and reacting, taking out the film, washing, drying and obtaining the material for making high polymer air fibers.

[0013] As a further improvement of the application, the following steps are included:

[0014] S1. Preparation of doped antibacterial far infrared ceramic powder: tetrabutyl titanate, zinc acetate and zirconium acetate are added into ethanol, polyvinyl alcohol and thiourea are added, stirring is performed until they are uniformly mixed, hydrochloric acid solution is added dropwise, stirring and reaction are performed, centrifugation is performed, washing and drying are performed, calcination is performed, ball milling is performed and the doped antibacterial far infrared ceramic powder is prepared;

[0015] S2. Preparation of magnetic doped antibacterial far infrared ceramic powder: the doped antibacterial far infrared ceramic powder is added into water, under the protection of inert gas, iron chloride and ferrous chloride are added, ammonia water is added dropwise, heating and stirring are performed, centrifugation is performed, washing and drying are performed, calcination is performed and the magnetic doped antibacterial far infrared ceramic powder is prepared;

[0016] S3. Preparation of modified ceramic powder: the magnetic doped antibacterial far infrared ceramic powder is added into water, tannic acid and a catalyst are added, heating and stirring are performed, magnetic separation is performed, washing and drying are performed and the modified ceramic powder is prepared;

[0017] S4. Melt blowing: TPEE is added into a screw injection molding machine, heating and melt blowing are performed, stretching is performed under the action of hot air, traction by a draft gas is performed, blowing is performed towards a roller and the TPEE air fiber film is collected on the roller and becomes the TPEE air fiber film by self thermal bonding;

[0018] S5. Preparation of the material for making high polymer air fibers: water-soluble chitosan is dissolved in water, the modified ceramic powder is added, stirring and mixing are uniformly performed, the TPEE air fiber film is immersed, genipin solution is uniformly added dropwise, heating and reaction are performed, the film is taken out, washing and drying are performed and the material for making high polymer air fibers is prepared.

[0019] As a further improvement of the present application, the mass ratio of the tetrabutyl titanate, zinc acetate, zirconium acetate, polyvinyl alcohol and thiourea in step S1 is 10-13:3-5:2-4:0.5-1:0.2-0.4, the concentration of the hydrochloric acid solution is 1.5-2.5 mol / L, the calcination temperature is 400-600℃, the time is 2-3h, and the ball milling time is 1-2h.

[0020] As a further improvement of the present application, the mass ratio of the doped antibacterial far infrared ceramic powder, ferric chloride, ferrous chloride and ammonia in step S2 is 10-12:3.24:1.26:4-6, the temperature of the heating and stirring reaction is 70-80℃, the time is 3-5h, the calcination temperature is 400-500℃, and the time is 1-2h.

[0021] As a further improvement of the present application, the mass ratio of the magnetic doped antibacterial far infrared ceramic powder, tannic acid and catalyst in step S3 is 10:3-4:0.5-1, the catalyst is Tris-HCl solution with pH=8.5-9.5, the temperature of the heating and stirring reaction is 35-45℃, and the time is 2-4h.

[0022] As a further improvement of the present application, the melting temperature in step S4 is 205-215℃.

[0023] As a further improvement of the present application, the water-soluble chitosan in step S5 is carboxymethyl chitosan or chitosan hydrochloride, the mass ratio of the water-soluble chitosan, modified ceramic powder and TPEE air fiber membrane is 7-10:2-3:15-20, the concentration of the genipin solution is 0.1-0.2wt%, the temperature of the heating reaction is 35-45℃, and the time is 1-2h.

[0024] As a further improvement of the present application, it specifically comprises the following steps:

[0025] S1. Preparation of doped antibacterial far infrared ceramic powder: 10-13 parts by weight of tetrabutyl titanate, 3-5 parts by weight of zinc acetate, 2-4 parts by weight of zirconium acetate are added to ethanol, 0.5-1 parts by weight of polyvinyl alcohol and 0.2-0.4 parts by weight of thiourea are added, stirred and mixed uniformly, 10-12 parts by weight of 1.5-2.5 mol / L hydrochloric acid solution is added dropwise, stirred for 3-5h, centrifuged, washed, dried, calcined at 400-600℃ for 2-3h, and ball milled for 1-2h to obtain the doped antibacterial far infrared ceramic powder;

[0026] S2. Preparation of the magnetic doped antibacterial far infrared ceramic powder: 10-12 parts by weight of the doped antibacterial far infrared ceramic powder is added to water, 3.24 parts by weight of ferric chloride and 1.26 parts by weight of ferrous chloride are added under inert gas protection, 4-6 parts by weight of ammonia water is added dropwise, heated to 70-80 DEG C, stirred for 3-5 h, centrifuged, washed, dried, calcined at 400-500 DEG C for 1-2 h, and the magnetic doped antibacterial far infrared ceramic powder is prepared;

[0027] S3. Preparation of the modified ceramic powder: 10 parts by weight of the magnetic doped antibacterial far infrared ceramic powder is added to water, 3-4 parts by weight of tannic acid and 0.5-1 parts by weight of the catalyst are added, heated to 35-45 DEG C, stirred for 2-4 h, separated by a magnet, washed, dried, and the modified ceramic powder is prepared;

[0028] The catalyst is Tris-HCl solution with pH=8.5-9.5;

[0029] S4. Melt blowing: TPEE is added to a screw injection molding machine, heated to 205-215 DEG C, melt blown, after stretching under the action of hot air, drawn by a draft gas flow, blown to a roller, and collected on the roller to become a TPEE air fiber membrane by self thermal bonding;

[0030] S5. Preparation of the material for making the polymer air fiber: 7-10 parts by weight of water-soluble chitosan is dissolved in water, 2-3 parts by weight of the modified ceramic powder is added, stirred and mixed uniformly, immersed in 15-20 parts by weight of the TPEE air fiber membrane, 10 parts by weight of 0.1-0.2 wt% genipin solution is added dropwise uniformly, heated to 35-45 DEG C, reacted for 1-2 h, the membrane is taken out, washed, dried, and the material for making the polymer air fiber is prepared.

[0031] The application further protects a material for making the polymer air fiber prepared by the above preparation method.

[0032] The application further protects the application of the above material for making the polymer air fiber in preparing a mattress. Beneficial effects

[0033] The application has the following beneficial effects:

[0034] The TPEE air fiber is a 3D stereoscopic net-like fiber structure material, the raw material thermoplastic polyester elastomer is integrally formed in water by heating and extrusion, has good elasticity and air permeability, can be directly combined with a fabric layer to form a mattress, and can be used for a mattress padding layer, and helps to obtain good sleep quality.

[0035] The application prepares a material for making high polymer air fibers, and TPEE air fiber membranes are prepared by melt blowing with TPEE thermoplastic polyester elastomer (linear block copolymer) as the material, the specific surface area of the fiber membranes is large, the prepared TPEE air fiber membranes have good mechanical properties, large elasticity, and high rigidity maintenance in long-term use, so that the comfort of the prepared mattress is obviously improved.

[0036] The application prepares doped antibacterial TiO2 / ZnO / ZrO2 ceramic powder through a sol-gel reaction, and the prepared TiO2 / ZnO / ZrO2 ceramic powder is doped with C, N and S elements by adding thiourea and calcining, the doping of these non-metallic elements changes the crystal structure of TiO2 and ZnO, and can inhibit the recombination rate of photo-generated electrons and holes, compared with pure TiO2 and ZnO, the photocatalytic activity is significantly enhanced, the corresponding defects of the photocatalysts TiO2 and ZnO are solved, and the application is greatly widened, so that the prepared doped antibacterial TiO2 / ZnO / ZrO2 ceramic powder can photocatalytically degrade pollutants such as formaldehyde under the action of visible light, the prepared mattress is more environmentally friendly, and at the same time, has better antibacterial performance, so that the prepared mattress is more hygienic and safe. At the same time, the prepared TiO2 / ZnO / ZrO2 ceramic powder has certain far infrared emission function and can slowly produce heat, so that the user feels comfortable when using the mattress.

[0037] Further, the surface of the TiO2 / ZnO / ZrO2 ceramic powder is deposited with magnetic ferroferric oxide, a magnetic field is formed, the sleep state is improved, falling asleep is promoted, and the sleep time is prolonged, muscle spasm is relieved, muscle tension is reduced, and the immune function is regulated.

[0038] The surface of the prepared magnetic doped antibacterial far infrared ceramic powder is modified by tannic acid, so that the surface of the particles has adhesion and rich hydroxyl groups, can be fixed on chitosan through hydrogen bond action with the amino and carboxyl groups of chitosan, and the water-soluble chitosan is penetrated into the TPEE air fiber membrane and cross-linked and adsorbed on the TPEE air fiber membrane under the action of genipin, so as to enhance the mechanical properties of the TPEE air fiber membrane, and the modified ceramic powder is uniformly dispersed in the TPEE air fiber membrane, and good antibacterial, environmental protection, immune regulation, magnetic therapy, far infrared heating and other effects are achieved, so that the prepared material for making high polymer air fibers has better comprehensive performance, is a better mattress support material, and has wide application prospect. BRIEF DESCRIPTION OF DRAWINGS

[0039] In order to make the technical solutions in the embodiments of the present application or the prior art clearer, the accompanying drawings needed in the embodiments or prior art description will be briefly introduced. Obviously, the accompanying drawings in the following description only represent some of the embodiments of the present application, and all other embodiments obtained by a person of ordinary skill in the art without any creative effort based on these accompanying drawings also belong to the protection scope of the present application.

[0040] Figure 1 is a photo of the TPEE air fiber membrane prepared in Embodiment 1 of the present application. Embodiment of the present application

[0041] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments only represent some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without any creative effort also belong to the protection scope of the present application.

[0042] The TPEE is Arnitel® TPEE UM551-V.

[0043] Embodiment 1

[0044] The present embodiment provides a preparation method of a material for preparing a high molecular air fiber, which specifically comprises the following steps:

[0045] S1. Preparation of doped antibacterial far infrared ceramic powder: 10 g of tetrabutyl titanate, 3 g of zinc acetate, and 2 g of zirconium acetate are added into 500 mL of ethanol, 0.5 g of polyvinyl alcohol and 0.2 g of thiourea are added, stirring and mixing for 20 min, 10 g of 1.5 mol / L hydrochloric acid solution is added dropwise, stirring and reacting for 3 h, centrifuging, washing, drying, calcining at 400℃ for 2 h, and ball milling for 1 h to obtain the doped antibacterial far infrared ceramic powder;

[0046] S2. Preparation of magnetic doped antibacterial far infrared ceramic powder: 10 g of the doped antibacterial far infrared ceramic powder is added into 500 mL of water, 3.24 g of ferric chloride and 1.26 g of ferrous chloride are added under nitrogen protection, 4 g of ammonia water is added dropwise, heated to 70℃, stirring and reacting for 3 h, centrifuging, washing, drying, and calcining at 400℃ for 1 h to obtain the magnetic doped antibacterial far infrared ceramic powder;

[0047] S3. Preparation of modified ceramic powder: 10 g of the magnetic doped antibacterial far infrared ceramic powder is added into 500 mL of water, 3 g of tannic acid and 0.5 g of catalyst are added, heated to 35℃, stirring and reacting for 2 h, magnetically separated, washed, and dried to obtain the modified ceramic powder;

[0048] The catalyst is Tris-HCl solution with pH=8.5;

[0049] S4. Melt blowing: TPEE was added into a screw injection molding machine, heated to 205℃, melt blown, after stretching under the action of hot air, drawn by a draft airflow, blown to a roller, and collected on the roller, and self-adhered into a TPEE air fiber membrane by heat, Figure 1 is a photo of the prepared TPEE air fiber membrane;

[0050] S5. Preparation of a material for making a polymer air fiber: 7g carboxymethyl chitosan was dissolved in 500mL water, 2g modified ceramic powder was added, stirred and mixed for 10min, 15g TPEE air fiber membrane was immersed, 10g 0.1wt% genipin solution was added dropwise, heated to 35℃, and reacted for 1h, the membrane was taken out, washed, and dried to prepare a material for making a polymer air fiber.

[0051] Example 2

[0052] The embodiment provides a preparation method of a material for making a polymer air fiber, which specifically comprises the following steps:

[0053] S1. Preparation of doped antibacterial far infrared ceramic powder: 13g tetrabutyl titanate, 5g zinc acetate, and 4g zirconium acetate were added into 500mL ethanol, 1g polyvinyl alcohol and 0.4g thiourea were added, stirred and mixed for 20min, 12g 2.5mol / L hydrochloric acid solution was added dropwise, stirred and reacted for 5h, centrifuged, washed, dried, calcined at 600℃ for 3h, and ball milled for 2h to prepare the doped antibacterial far infrared ceramic powder;

[0054] S2. Preparation of magnetic doped antibacterial far infrared ceramic powder: 12g doped antibacterial far infrared ceramic powder was added into 500mL water, 3.24g ferric chloride and 1.26g ferrous chloride were added under nitrogen protection, 6g ammonia water was added dropwise, heated to 80℃, stirred and reacted for 5h, centrifuged, washed, dried, and calcined at 500℃ for 2h to prepare the magnetic doped antibacterial far infrared ceramic powder;

[0055] S3. Preparation of modified ceramic powder: 10g magnetic doped antibacterial far infrared ceramic powder was added into 500mL water, 4g tannic acid and 1g catalyst were added, heated to 45℃, stirred and reacted for 4h, magnetically separated, washed, and dried to prepare the modified ceramic powder;

[0056] The catalyst is Tris-HCl solution with pH=9.5;

[0057] S4. Melt blowing: TPEE was added into a screw injection molding machine, heated to 215℃, melt blown, after stretching under the action of hot air, drawn by a draft airflow, blown to a roller, and collected on the roller, and self-adhered into a TPEE air fiber membrane by heat;

[0058] S5. Preparation of the material for making polymer air fiber: 10 g of carboxymethyl chitosan was dissolved in 500 mL of water, 3 g of modified ceramic powder was added, stirred and mixed for 10 min, 20 g of TPEE air fiber membrane was immersed, 10 g of 0.2 wt% genipin solution was added dropwise, heated to 45℃, reacted for 2 h, the membrane was taken out, washed and dried to prepare the material for making polymer air fiber.

[0059] Example 3

[0060] The embodiment provides a preparation method of a material for making polymer air fiber, which specifically comprises the following steps:

[0061] S1. Preparation of doped antibacterial far infrared ceramic powder: 11 g of tetrabutyl titanate, 4 g of zinc acetate and 3 g of zirconium acetate were added to 500 mL of ethanol, 0.7 g of polyvinyl alcohol and 0.3 g of thiourea were added, stirred and mixed for 20 min, 11 g of 2 mol / L hydrochloric acid solution was added dropwise, stirred and reacted for 4 h, centrifuged, washed, dried, calcined at 500℃ for 2.5 h, and ball milled for 1.5 h to prepare the doped antibacterial far infrared ceramic powder;

[0062] S2. Preparation of magnetic doped antibacterial far infrared ceramic powder: 11 g of the doped antibacterial far infrared ceramic powder was added to 500 mL of water, 3.24 g of iron chloride and 1.26 g of ferrous chloride were added under nitrogen protection, 5 g of ammonia water was added dropwise, heated to 75℃, stirred and reacted for 4 h, centrifuged, washed, dried, and calcined at 450℃ for 1.5 h to prepare the magnetic doped antibacterial far infrared ceramic powder;

[0063] S3. Preparation of modified ceramic powder: 10 g of the magnetic doped antibacterial far infrared ceramic powder was added to 500 mL of water, 3.5 g of tannic acid and 0.7 g of catalyst were added, heated to 40℃, stirred and reacted for 3 h, magnetically separated, washed and dried to prepare the modified ceramic powder;

[0064] The catalyst is Tris-HCl solution with pH=9;

[0065] S4. Melt blowing: TPEE was added to a screw injection molding machine, heated to 210℃, and melt blown. After stretching under the action of hot air, it was pulled by a drawing gas flow, blown to a roller, and collected on the roller to become a TPEE air fiber membrane by self thermal bonding;

[0066] S5. Preparation of the material for making polymer air fiber: 10 g of carboxymethyl chitosan was dissolved in 500 mL of water, 3 g of modified ceramic powder was added, stirred and mixed for 10 min, 20 g of TPEE air fiber membrane was immersed, 10 g of 0.2 wt% genipin solution was added dropwise, heated to 45℃, reacted for 2 h, the membrane was taken out, washed and dried to prepare the material for making polymer air fiber.

[0067] Comparative Example 1

[0068] The difference compared with Example 3 is that no thiourea is added in step S1.

[0069] The details are as follows:

[0070] S1. Preparation of antibacterial far infrared ceramic powder: 11 g of tetrabutyl titanate, 4 g of zinc acetate, and 3 g of zirconium acetate were added to 500 mL of ethanol, 0.7 g of polyvinyl alcohol was added, and the mixture was stirred for 20 min, 11 g of 2 mol / L hydrochloric acid solution was added dropwise, and the reaction was stirred for 4 h, centrifuged, washed, dried, calcined at 500°C for 2.5 h, and ball milled for 1.5 h to obtain the antibacterial far infrared ceramic powder.

[0071] Comparative Example 2

[0072] The difference compared with Example 3 is that step S2 is not performed.

[0073] The details are as follows:

[0074] S1. Preparation of doped antibacterial far infrared ceramic powder: 11 g of tetrabutyl titanate, 4 g of zinc acetate, and 3 g of zirconium acetate were added to 500 mL of ethanol, 0.7 g of polyvinyl alcohol and 0.3 g of thiourea were added, and the mixture was stirred for 20 min, 11 g of 2 mol / L hydrochloric acid solution was added dropwise, and the reaction was stirred for 4 h, centrifuged, washed, dried, calcined at 500°C for 2.5 h, and ball milled for 1.5 h to obtain the doped antibacterial far infrared ceramic powder;

[0075] S2. Preparation of modified ceramic powder: 10 g of doped antibacterial far infrared ceramic powder was added to 500 mL of water, 3.5 g of tannic acid and 0.7 g of catalyst were added, heated to 40°C, stirred for 3 h, centrifuged, washed, and dried to obtain the modified ceramic powder;

[0076] The catalyst is Tris-HCl solution with pH=9;

[0077] S3. Melt blowing: TPEE was added to a screw injection molding machine, heated to 210°C, and melt blown. After stretching under the action of hot air, it was pulled by a drawing gas stream, blown onto a roller, and collected on the roller to form a TPEE air fiber membrane by self-heating and bonding.

[0078] S4. Preparation of material for making polymer air fibers: 8.5 g of carboxymethyl chitosan was dissolved in 500 mL of water, 2.5 g of modified ceramic powder was added, stirred for 10 min, 17 g of TPEE air fiber membrane was immersed, 10 g of 0.15 wt% genipin solution was added dropwise, heated to 40°C, and reacted for 1.5 h. The membrane was taken out, washed, and dried to obtain the material for making polymer air fibers.

[0079] Comparative Example 3

[0080] The difference compared with Example 3 is that step S3 is not performed.

[0081] The details are as follows:

[0082] S1. Preparation of doped antibacterial far infrared ceramic powder: 11 g of tetrabutyl titanate, 4 g of zinc acetate, and 3 g of zirconium acetate were added to 500 mL of ethanol, 0.7 g of polyvinyl alcohol and 0.3 g of thiourea were added, and stirred and mixed for 20 min, 11 g of 2 mol / L hydrochloric acid solution was added dropwise, and stirred and reacted for 4 h, centrifuged, washed, dried, calcined at 500°C for 2.5 h, and ball milled for 1.5 h to obtain the doped antibacterial far infrared ceramic powder;

[0083] S2. Preparation of magnetic doped antibacterial far infrared ceramic powder: 11 g of the doped antibacterial far infrared ceramic powder was added to 500 mL of water, 3.24 g of ferric chloride and 1.26 g of ferrous chloride were added under nitrogen protection, 5 g of ammonia water was added dropwise, heated to 75°C, stirred and reacted for 4 h, centrifuged, washed, dried, and calcined at 450°C for 1.5 h to obtain the magnetic doped antibacterial far infrared ceramic powder;

[0084] S3. Melt blowing: TPEE was added to a screw injection molding machine, heated to 210°C, and melt blown. After stretching under the action of hot air, it was pulled by a drawing gas flow, blown towards a roller, and collected on the roller to form a TPEE air fiber membrane by self thermal bonding;

[0085] S4. Preparation of material for making polymer air fibers: 8.5 g of carboxymethyl chitosan was dissolved in 500 mL of water, 2.5 g of magnetic doped antibacterial far infrared ceramic powder was added, stirred and mixed for 10 min, 17 g of TPEE air fiber membrane was immersed, 10 g of 0.15wt% genipin solution was added dropwise, heated to 40°C, and reacted for 1.5 h. The membrane was taken out, washed, and dried to obtain the material for making polymer air fibers.

[0086] Comparative Example 4

[0087] The difference compared with Example 3 is that no modified ceramic powder is added in step S5.

[0088] The details are as follows:

[0089] S5. Preparation of material for making polymer air fibers: 8.5 g of carboxymethyl chitosan was dissolved in 500 mL of water, stirred and mixed for 10 min, 17 g of TPEE air fiber membrane was immersed, 10 g of 0.15wt% genipin solution was added dropwise, heated to 40°C, and reacted for 1.5 h. The membrane was taken out, washed, and dried to obtain the material for making polymer air fibers.

[0090] Comparative Example 5

[0091] The difference compared with Example 3 is that no carboxymethyl chitosan is added in step S5.

[0092] The details are as follows:

[0093] S5. Preparation of the material for making polymer air fiber: 2.5 g of modified ceramic powder is added to 500 mL of water, stirred and mixed for 10 min, immersed in 17 g of TPEE air fiber membrane, heated to 40℃, reacted for 1.5 h, the membrane is taken out, washed, dried, and the material for making polymer air fiber is prepared.

[0094] Test Example 1

[0095] The material for making polymer air fiber prepared by Examples 1-3 and Comparative Examples 1-5 is tested by using the oscillation method (GB / T20944.3-2008).

[0096] Test bacteria: Escherichia coli ATCC25922, Staphylococcus aureus ATCC6538.

[0097] The results are shown in Table 1.

[0098] Table 1

[0099] From the above table, it can be seen that the material for making polymer air fiber prepared by Examples 1-3 of the present application has good antibacterial performance.

[0100] Test Example 2

[0101] The material for making polymer air fiber prepared by Examples 1-3 and Comparative Examples 1-5 of the present application is used as a support layer of a mattress, with a thickness of 6 cm and a density of 55 kg / m 3 , sponge is used as a bedding layer, with a thickness of 4 cm and a density of 20 kg / cm 3 , and cotton is used as a surface layer to prepare a mattress, and the mattress is tested.

[0102] The thermal comfort test instrument selects an iButton temperature recorder from the United States, and the specific parameters are as follows: the temperature measurement range is -35 to 70℃, the sampling speed is 1 time / min, the sampling resolution is 0.5℃, and the accuracy is ±0.5℃. Before testing, the mattress needs to be placed in an environment with a room temperature of (23±0.5)℃ and a relative humidity of (50±5)% for 24h. The test points are selected from four parts of the human body in contact with the mattress when the human body is supine, which are the back, the temperature recorder is attached to the surface of the bed sheet at the test point with a thin breathable adhesive tape, and the experiment starts after the indoor environment meets the experimental conditions, and each experiment lasts for 30min. After the data collection is completed, analysis is performed. The overall interface temperature is calculated from the local interface temperature. During the experiment, the subject is tested for subjective temperature sensation and subjective thermal comfort evaluation, and the average value is taken. The subjective temperature sensation evaluation scale is shown in Table 2, and the subjective comfort evaluation scale is shown in Table 3.

[0103] Table 2

[0104] Table 3

[0105] The back temperature change results are shown in Table 4.

[0106] Table 4

[0107]

[0108] Back temperature change table

[0109] From the above table, it can be seen that the mattress prepared from the material for preparing the high molecular air fiber prepared in examples 1-3 has a higher temperature and is more suitable.

[0110] The score results are shown in Table 4.

[0111] Table 5

[0112] From the above table, it can be seen that the mattress prepared from the material for preparing the high molecular air fiber prepared in examples 1-3 has a moderate subjective temperature and is more comfortable.

[0113] Test example 3

[0114] The material for preparing the high molecular air fiber prepared in examples 1-3 and comparative examples 1-5 is used as a support layer of the mattress, with a thickness of 6cm and a density of 55kg / m 3 , sponge is used as a bedding layer, with a thickness of 4cm and a density of 20kg / cm 3 , and cotton is used as a surface layer to prepare the mattress, and the mattress is tested.

[0115] The test uses MCK-Z-I type intelligent display control instrument to measure the force-displacement curve of the mattress sample. The test is carried out in an environment with a room temperature (23±2) ℃ and a relative humidity (50±5) %. Before the test, the pressure plate is adjusted to be high, the mattress sample is placed on the test table, and the position of the pressure plate is adjusted to be just in the middle of the mattress sample. During the test, the subsidence of the mattress sample at a force of 110N is measured for 3 times, and the average value is taken to calculate the comprehensive stiffness K value of the mattress sample. The K value is proportional to the hardness of the mattress. The larger the comprehensive stiffness K value is, the harder the mattress is. The smaller the comprehensive stiffness K value is, the softer the mattress is.

[0116] The results are shown in Table 6.

[0117] Table 6

[0118] From the above table, it can be seen that the mattress prepared from the material for preparing the high molecular air fiber prepared in Examples 1-3 has a better comprehensive stiffness K value.

[0119] The above description is merely preferred embodiments of the present application, but not to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method for producing a material for making a high molecular air fiber, characterized by, Comprising the following steps: S1. Preparation of doped antibacterial far infrared ceramic powder: tetrabutyl titanate, zinc acetate, zirconium acetate are added to ethanol, polyvinyl alcohol and thiourea are added, stirred and mixed uniformly, hydrochloric acid solution is added dropwise, stirred and reacted, centrifuged, washed, dried, calcined, ball milled, and doped antibacterial far infrared ceramic powder is prepared; S2. Preparation of magnetic doped antibacterial far infrared ceramic powder: the doped antibacterial far infrared ceramic powder is added to water, and under the protection of inert gas, iron chloride and ferrous chloride are added, ammonia water is added dropwise, heated and stirred to react, centrifuged, washed, dried, and calcined to obtain magnetic doped antibacterial far infrared ceramic powder; S3. Preparation of modified ceramic powder: the magnetic doped antibacterial far infrared ceramic powder is added to water, tannic acid and catalyst are added, heated and stirred to react, separated by magnet, washed and dried to obtain modified ceramic powder; S4. Melt blowing: TPEE is added to a screw injection molding machine, heated and melted to spin, stretched under the action of hot air, pulled by a drawing gas flow, blown to a roller, and collected on the roller to form a TPEE air fiber membrane by self thermal bonding; S5. Preparation of material for making polymer air fiber: water-soluble chitosan is dissolved in water, modified ceramic powder is added, stirred and mixed uniformly, the TPEE air fiber membrane is immersed, genipin solution is added dropwise, heated to react, the membrane is taken out, washed and dried to obtain the material for making polymer air fiber.

2. The production method according to claim 1, characterized by, The mass ratio of tetrabutyl titanate, zinc acetate, zirconium acetate, polyvinyl alcohol and thiourea in step S1 is 10-13:3-5:2-4:0.5-1:0.2-0.4, the concentration of the hydrochloric acid solution is 1.5-2.5 mol / L, the calcination temperature is 400-600℃, the time is 2-3h, and the ball milling time is 1-2h.

3. The production method according to claim 1, characterized by, The mass ratio of doped antibacterial far infrared ceramic powder, iron chloride, ferrous chloride and ammonia water in step S2 is 10-12:3.24:1.26:4-6, the heating and stirring reaction temperature is 70-80℃, the time is 3-5h, the calcination temperature is 400-500℃, and the time is 1-2h. The mass ratio of magnetic doped antibacterial far infrared ceramic powder, tannic acid and catalyst in step S3 is 10:3-4:0.5-1, the catalyst is Tris-HCl solution with pH=8.5-9.5, the heating and stirring reaction temperature is 35-45℃, and the time is 2-4h.

4. The method of claim 1, wherein, The melting temperature in step S4 is 205-215℃.

5. The preparation method according to claim 1, characterized in that, The water-soluble chitosan in step S5 is carboxymethyl chitosan or chitosan hydrochloride, the mass ratio of water-soluble chitosan, modified ceramic powder and TPEE air fiber membrane is 7-10:2-3:15-20, the concentration of genipin solution is 0.1-0.2wt%, the heating reaction temperature is 35-45℃, and the time is 1-2h.

6. The method of claim 1, wherein, Specifically comprising the following steps:

7. The preparation method according to claim 1, characterized in that, ​ S1. Preparation of doped antibacterial far infrared ceramic powder: 10-13 parts by weight of tetrabutyl titanate, 3-5 parts by weight of zinc acetate, 2-4 parts by weight of zirconium acetate are added to ethanol, 0.5-1 parts by weight of polyvinyl alcohol and 0.2-0.4 parts by weight of thiourea are added, stirred and mixed uniformly, 10-12 parts by weight of 1.5-2.5 mol / L hydrochloric acid solution is added dropwise, stirred for 3-5 h, centrifuged, washed, dried, calcined at 400-600℃ for 2-3 h, ball milled for 1-2 h, and the doped antibacterial far infrared ceramic powder is prepared; S2. Preparation of magnetic doped antibacterial far infrared ceramic powder: 10-12 parts by weight of doped antibacterial far infrared ceramic powder is added to water, under inert gas protection, 3.24 parts by weight of iron chloride and 1.26 parts by weight of ferrous chloride are added, 4-6 parts by weight of ammonia water is added dropwise, heated to 70-80℃, stirred for 3-5 h, centrifuged, washed, dried, calcined at 400-500℃ for 1-2 h, and the magnetic doped antibacterial far infrared ceramic powder is prepared; S3. Preparation of modified ceramic powder: 10 parts by weight of magnetic doped antibacterial far infrared ceramic powder is added to water, 3-4 parts by weight of tannic acid and 0.5-1 parts by weight of catalyst are added, heated to 35-45℃, stirred for 2-4 h, separated by magnet, washed, and dried to obtain the modified ceramic powder; The catalyst is Tris-HCl solution with pH=8.5-9.5; S4. Melt blowing: TPEE is added to a screw injection molding machine, heated to 205-215℃, and melt blown. After stretching under the action of hot air, it is drawn by a drawing gas flow, blown towards a roller, and collected on the roller to form a TPEE air fiber membrane by self thermal bonding; S5. Preparation of a material for making polymer air fibers: 7-10 parts by weight of water-soluble chitosan is dissolved in water, 2-3 parts by weight of modified ceramic powder is added, stirred and mixed uniformly, 15-20 parts by weight of TPEE air fiber membrane is immersed, 10 parts by weight of 0.1-0.2wt% genipin solution is added dropwise, heated to 35-45℃, reacted for 1-2 h, the membrane is taken out, washed, dried, and the material for making polymer air fibers is prepared.

8. A material for making polymer air fibers prepared by the preparation method of any one of claims 1-7.

9. Use of the material for making polymer air fibers of claim 8 in preparing a mattress.

Citation Information

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