Negative oxygen ion fabric and preparation method thereof

Abstract

The present invention discloses a negative oxygen ion fabric and a preparation method thereof, belonging to the technical field of negative oxygen ion fabric preparation. The preparation method of the negative oxygen ion fabric comprises the following steps: step (1): ultrasonically dispersing microcapsule composite negative oxygen ions in distilled water, placing the microcapsule composite negative oxygen ions in a spray gun, and evenly spraying the microcapsule composite negative oxygen ions on the surface of a cotton fabric. The operation is repeated, and the microcapsule composite negative oxygen ions are then dried to obtain a negative oxygen ion layer; step (2): evenly coating both sides of a polyester fabric with an environmentally friendly adhesive, then bonding the microcapsule composite negative oxygen ion layer to the negative oxygen ion layer and allowing the negative oxygen ion layer to stand to obtain a negative oxygen ion fabric. The fabric prepared by this method can release negative oxygen ions for a long time and also has excellent antibacterial, waterproof and environmentally friendly properties.

Description

Technical Field

[0001] The present invention belongs to the technical field of preparation of negative oxygen ion fabrics, and in particular relates to a negative oxygen ion fabric and a preparation method thereof. Background Art

[0002] With the acceleration of urbanization and the intensification of environmental pollution, people are increasingly aware of the importance of air quality to their health. Negative oxygen ions, as a naturally occurring health factor, can effectively neutralize positive ions in the air, reducing harmful substances such as dust, bacteria, and viruses, thereby improving indoor air quality and safeguarding human respiratory health. Integrating negative oxygen ion technology into textiles, allowing people to enjoy the health benefits of negative oxygen ions in their daily lives, is undoubtedly an innovative endeavor. With intensifying market competition and diversifying consumer demands, traditional textiles are struggling to meet market demands for functionality, environmental friendliness, and comfort. Consequently, textile companies are pursuing technological innovation and industrial upgrading to develop new products with differentiated competitive advantages. The emergence of negative oxygen ion fabrics not only enhances the basic properties of traditional textiles but also imparts new health benefits, injecting new vitality into the textile industry. Furthermore, the rapid development of materials science, nanotechnology, and biotechnology has provided a rich technical and material foundation for textile innovation. Negative oxygen ion materials can be successfully incorporated into textiles through various techniques, such as co-spinning and surface coating modification, achieving the sustained release of negative oxygen ions.

[0003] Patent CN 107323019 B discloses a formula, preparation method, and products of negative oxygen ion-functional fabrics. The formula comprises a face adhesive film, a base adhesive, and fabrics. The face adhesive film comprises the following components in parts by weight: 20-65 parts one-component polyurethane; 25-75 parts organic solvent; and 5-10 parts energy powder. The base adhesive comprises the following components in parts by weight: 30-55 parts two-component polyurethane; 30-65 parts organic solvent; and 5-15 parts bridging agent. The invention also discloses a preparation method and products of negative oxygen ion-functional fabrics using the above formula. The preparation process is easy to control, and the resulting negative oxygen ion-functional fabrics not only benefit human health and are environmentally friendly, but also exhibit hydrolysis resistance, aging resistance, wear resistance, high stability, and low cost. However, the antibacterial properties, negative oxygen ion retention, and environmental performance of the negative oxygen ion-functional fabrics prepared using this method still require improvement. Summary of the Invention

[0004] The purpose of the present invention is to provide a negative oxygen ion fabric and a preparation method thereof, which are used to solve the technical problems of the negative oxygen ion fabric in the prior art, such as poor antibacterial performance, short duration of negative oxygen ions, and poor environmental performance.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The present invention provides a negative oxygen ion fabric, comprising a negative oxygen ion layer and a base fabric layer. The negative oxygen ion layer is tightly bonded to both sides of the base fabric layer by an environmentally friendly adhesive. The negative oxygen ion layer is prepared by microcapsule composite negative oxygen ions and cotton fabric, and the base fabric is composed of polyester fabric.

[0007] Preferably, the method for preparing the environmentally friendly adhesive comprises the following steps:

[0008] Q1: Dehydrated polycaprolactone triol and isophorone diisocyanate are added to a container, followed by dibutyltin dilaurate, and heated for reaction. After the reaction is completed, intermediate product 1 is obtained.

[0009] Q2: Add guar gum and 2,2-dimethylolpropionic acid to intermediate product 1, continue stirring and reacting, cool down after the reaction, add triethylamine to neutralize the reaction, then add ethylenediamine, emulsify and disperse with deionized water, and then stop stirring to obtain intermediate product 2;

[0010] Q3: Place the intermediate product 2 in a rotary evaporator, heat and react to obtain an environmentally friendly adhesive.

[0011] In the above process, the environmentally friendly adhesive is prepared by the prepolymer synthesis method. First, polycaprolactone triol and isophorone diisocyanate are added to a container to react to generate intermediate product 1. Then, a chain extender 2,2-dihydroxymethylpropionic acid and guar gum are added to react. Then, a neutralizing agent triethylamine is added for neutralization reaction. Subsequently, ethylenediamine is added for chain extension, and deionized water is used for emulsification and dispersion to finally obtain the environmentally friendly adhesive.

[0012] Preferably, in Q1, the dehydration treatment process is: placing polycaprolactone triol in a microwave oven at 110-130°C and heating it for 10-12 minutes, the molar ratio of polycaprolactone triol to isophorone diisocyanate is (0.9-1.1): (1.8-2.2), the heating reaction temperature is 80-85°C, and the time is 90-120 minutes.

[0013] Preferably, in Q2, the molar ratio of guar gum, 2,2-dihydroxymethylpropionic acid, intermediate 1, triethylamine and ethylenediamine is (1-2): (1.1-1.9): (0.9-2.1): (1-2): (0.9-2.1), the stirring reaction time is continued for 90-120 minutes, the temperature is lowered to 60-65°C, the neutralization reaction time is 20-40 minutes, and the emulsification dispersion time is 30-45 minutes; in Q3, the heating temperature is 80-90°C, and the reaction time is 1-2 hours.

[0014] Preferably, the method for preparing the microcapsule composite negative oxygen ion comprises the following steps:

[0015] S1: adding agar to distilled water, heating and stirring to dissolve, adding white mineral oil to obtain an agar mixed solution, adding sorbitan oleate and gelatin solution to the agar mixed solution, heating and stirring, mixing uniformly, adjusting the pH, cooling, adding glutaraldehyde for cross-linking, continuing to adjust the pH, stirring, washing, filtering, and drying to obtain agar / gelatin microcapsules;

[0016] S2: Dissolve anhydrous citric acid and negative oxygen ion powder in distilled water, add agar / gelatin microcapsules and chitosan quaternary ammonium salt, stir, and then add them to the β-cyclodextrin solution, continue stirring, cool, filter, wash, and dry to obtain microcapsule composite negative oxygen ions.

[0017] In the above process, the pH is adjusted to cause agar and gelatin to undergo a complex coacervation reaction, and then glutaraldehyde is added as a cross-linking agent. The aldehyde groups contained therein react with the amino groups in the agar mixed solution containing gelatin through an amine-aldehyde condensation reaction to form a C=N bond. As the pH is adjusted to alkaline, agar / gelatin microcapsules are gradually formed, and negative oxygen ion powder is loaded on the agar / gelatin microcapsules and covered with chitosan quaternary ammonium salt. β-cyclodextrin as the outermost embedding material can effectively improve the chemical stability of the chitosan quaternary ammonium salt and effectively prolong the sustained-release time of the negative oxygen ions, thereby finally obtaining microcapsule composite negative oxygen ions.

[0018] Preferably, in S1, the amount ratio of agar, distilled water and white mineral oil is (5-8) g: (100-120) mL: (8-10) mL, the heating temperature is 80-90°C, the volume ratio of sorbitan oleate, gelatin solution, agar mixed solution and glutaraldehyde is (5-8) mL: (100-120) mL: (110-130) mL: (5-7) mL, the concentration of the gelatin solution is 0.05 g / mL, the heating and stirring temperature is 50-55°C, the time is 2-4 h, the pH is adjusted to 3.8-4.1 with 10vt% hydrochloric acid, the volume fraction of glutaraldehyde is 37vt%, and the pH is further adjusted to 8-9 with 20vt% sodium hydroxide. The drying temperature is 50-60°C.

[0019] Preferably, in S2, the dosage ratio of anhydrous citric acid, negative oxygen ion powder, distilled water, agar / gelatin microcapsules, chitosan quaternary ammonium salt and β-cyclodextrin solution is (0.5-0.7) g: (1-2) g: (100-110) mL: (2.0-2.5) g: (2-3) g: (100-120) mL, the stirring time is 30-50 min, the concentration of the β-cyclodextrin solution is 18.5 g / L, and the stirring time is continued for 1-2 h.

[0020] Preferably, the method for preparing the negative oxygen ion fabric comprises the following steps:

[0021] Step (1): ultrasonically dispersing the microcapsule composite negative oxygen ions in distilled water and then placing the microcapsule composite negative oxygen ions in a spray gun, spraying the microcapsule composite negative oxygen ions uniformly on the surface of the cotton cloth, repeating the operation, and then drying the microcapsule composite negative oxygen ion layer to obtain a negative oxygen ion layer;

[0022] Step (2): evenly coating both sides of the polyester fabric with an environmentally friendly adhesive, and then bonding it with the negative oxygen ion layer and allowing it to stand to obtain a negative oxygen ion fabric.

[0023] Preferably, in step (1), the ratio of microcapsule composite negative oxygen ions to distilled water is (30-40) g: (20-30) mL, the operation is repeated 3-5 times, the drying temperature is 80-90° C., and the drying time is 6-8 h.

[0024] Preferably, in the step (2), during the bonding process, the polyester fabric is bonded to the side of the negative oxygen ion layer that is not sprayed with microcapsule composite negative oxygen ions, and the standing time is 8-12 hours.

[0025] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0026] 1. The present invention first uses polycaprolactone triol, isophorone diisocyanate, guar gum and 2,2-dihydroxymethylpropionic acid as raw materials to prepare an environmentally friendly adhesive, then uses gelatin, agar, negative oxygen ion powder, chitosan quaternary ammonium salt and β-cyclodextrin as raw materials to prepare microcapsule composite negative oxygen ions, and the microcapsule composite negative oxygen ions are evenly sprayed on the surface of cotton cloth, and then the environmentally friendly adhesive is coated on both sides of the polyester fabric, and the cotton cloth and the polyester fabric are bonded to obtain a fabric with excellent antibacterial properties, sustained release properties, environmental protection and high concentration of negative oxygen ions.

[0027] 2. The present invention uses polycaprolactone triol, isophorone diisocyanate, 2,2-dihydroxymethylpropionic acid and guar gum as raw materials, and prepares an environmentally friendly adhesive through a prepolymer synthesis method. The environmentally friendly adhesive is used to bond the negative oxygen ion layer and the base fabric layer, which can effectively improve the environmental friendliness and waterproofness of the negative oxygen ion fabric.

[0028] 3. The present invention uses agar, gelatin, negative oxygen ion powder, chitosan quaternary ammonium salt and β-cyclodextrin as raw materials to prepare microcapsule composite negative oxygen ions, which are sprayed on the surface of cotton cloth, which can effectively improve the durability and antibacterial properties of the negative oxygen ion fabric in releasing negative oxygen ions. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0030] Figure 1 It is a schematic diagram of the cross-sectional structure of the negative oxygen ion fabric of the present invention.

[0031] Description of the accompanying drawings: 1. Negative oxygen ion layer, 2. Base fabric layer. DETAILED DESCRIPTION

[0032] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only 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 making creative efforts are within the scope of protection of the present invention.

[0033] Example 1

[0034] See Figure 1 As shown, the negative oxygen ion fabric of this embodiment includes a negative oxygen ion layer 1 and a base fabric layer 2. The negative oxygen ion layer is tightly bonded to both sides of the base fabric layer through an environmentally friendly adhesive. The negative oxygen ion layer is prepared by microcapsule composite negative oxygen ions and cotton cloth, and the base fabric is composed of polyester fabric.

[0035] Example 2

[0036] This embodiment discloses a method for preparing an environmentally friendly adhesive, comprising the following steps:

[0037] Q1: Polycaprolactone triol with an average relative molecular mass of 550 g / mol was placed in a microwave oven at 120°C and heated for 10 minutes. Then, 1.38 g of polycaprolactone triol and 1.11 g of isophorone diisocyanate were added to the container, followed by 0.1 mL of dibutyltin dilaurate and butanone to reduce the viscosity. The mixture was heated at 85°C for 90 minutes. After the reaction, intermediate product 1 was obtained.

[0038] Q2: 1.5 g of guar gum and 1.09 g of 2,2-dimethylolpropionic acid were added to 7.81 g of intermediate product 1, and the mixture was stirred and reacted for 120 min. Acetone was added during the stirring process to control the viscosity. After the reaction was completed, the temperature was lowered to 60°C, 0.83 g of triethylamine was added, and the mixture was neutralized and reacted for 20 min. Subsequently, 0.49 g of ethylenediamine was added, and the mixture was emulsified and dispersed with deionized water for 30 min. Then, stirring was stopped to obtain intermediate product 2;

[0039] Q3: Place the intermediate product 2 in a rotary evaporator and heat at 90°C for 1 hour to obtain an environmentally friendly adhesive.

[0040] This embodiment discloses a method for preparing microcapsule composite negative oxygen ions, comprising the following steps:

[0041] S1: 6.5 g of agar was added to 110 mL of distilled water, heated and stirred at 90°C to dissolve, and then 9 mL of white mineral oil was added to obtain an agar mixed solution. 6.5 mL of sorbitan oleate and 115 mL of a 0.05 g / mL gelatin solution were added to 120 mL of the agar mixed solution, heated and stirred at 55°C for 3 h, mixed evenly, and adjusted to pH 3.9 with 10% by volume hydrochloric acid. After cooling, 6 mL of 37% by volume glutaraldehyde was added for cross-linking. The pH was further adjusted to pH 8 with 20% by volume sodium hydroxide. The mixture was stirred, washed, filtered, and dried at 50°C to obtain agar / gelatin microcapsules.

[0042] S2: Dissolve 0.6g of anhydrous citric acid and 1.5g of negative oxygen ion powder in 105mL of distilled water, add 2.3g of agar / gelatin microcapsules and 2.5g of chitosan quaternary ammonium salt, stir for 30min, then add it to 110mL of β-cyclodextrin solution with a concentration of 18.5g / L, continue stirring for 2h, cool, filter, wash, and dry to obtain microcapsule composite negative oxygen ions.

[0043] This embodiment discloses a method for preparing a negative oxygen ion fabric, comprising the following steps:

[0044] Step (1): ultrasonically disperse 35 g of microcapsule composite negative oxygen ions in 25 mL of distilled water, place the mixture in a spray gun, and evenly spray it on the surface of the cotton cloth. Repeat the operation 5 times, and then dry it at 80°C for 6 h to obtain a negative oxygen ion layer.

[0045] Step (2): Evenly apply environmentally friendly adhesive on both sides of the polyester fabric, and then bond it to the negative oxygen ion layer. During the bonding process, the polyester fabric is bonded to the side of the negative oxygen ion layer that is not sprayed with microcapsule composite negative oxygen ions, and the fabric is left to stand for 12 hours to obtain a negative oxygen ion fabric.

[0046] Example 3

[0047] This embodiment discloses a method for preparing an environmentally friendly adhesive, comprising the following steps:

[0048] Q1: Polycaprolactone triol with an average relative molecular mass of 550 g / mol was placed in a microwave oven at 120°C and heated for 10 minutes. Then, 1.24 g of polycaprolactone triol and 1.00 g of isophorone diisocyanate were added to the container, followed by 0.1 mL of dibutyltin dilaurate and butanone to reduce the viscosity. The mixture was heated at 85°C for 90 minutes. After the reaction, intermediate product 1 was obtained.

[0049] Q2: 1.0 g guar gum and 1.80 g 2,2-dimethylolpropionic acid were added to 4.69 g of intermediate product 1, and the mixture was stirred and reacted for 120 min. Acetone was added during the stirring process to control the viscosity. After the reaction, the temperature was lowered to 60°C, and 0.55 g triethylamine was added to neutralize the mixture for 20 min. Subsequently, 0.29 g ethylenediamine was added, and the mixture was emulsified and dispersed with deionized water for 30 min. Then, stirring was stopped to obtain intermediate product 2.

[0050] Q3: Place the intermediate product 2 in a rotary evaporator and heat at 90°C for 1 hour to obtain an environmentally friendly adhesive.

[0051] This embodiment discloses a method for preparing microcapsule composite negative oxygen ions, comprising the following steps:

[0052] S1: 5 g of agar was added to 100 mL of distilled water, heated and stirred at 90°C for dissolution, and then 8 mL of white mineral oil was added to obtain an agar mixed solution. 6 mL of sorbitan oleate and 100 mL of a 0.05 g / mL gelatin solution were added to 110 mL of the agar mixed solution, heated and stirred at 55°C for 3 h, mixed evenly, and adjusted to pH 3.9 with 10% hydrochloric acid. After cooling, 5 mL of 37% glutaraldehyde was added for cross-linking. The pH was further adjusted to pH 8 with 20% sodium hydroxide. The mixture was stirred, washed, filtered, and dried at 50°C to obtain agar / gelatin microcapsules.

[0053] S2: Dissolve 0.5g of anhydrous citric acid and 1.0g of negative oxygen ion powder in 100mL of distilled water, add 2.0g of agar / gelatin microcapsules and 2.0g of chitosan quaternary ammonium salt, stir for 30min, then add it to 100mL of β-cyclodextrin solution with a concentration of 18.5g / L, continue stirring for 2h, cool, filter, wash, and dry to obtain microcapsule composite negative oxygen ions.

[0054] This embodiment discloses a method for preparing a negative oxygen ion fabric, comprising the following steps:

[0055] Step (1): ultrasonically disperse 30 g of microcapsule composite negative oxygen ions in 20 mL of distilled water, place the mixture in a spray gun, and evenly spray it on the surface of the cotton cloth. Repeat the operation 5 times, and then dry it at 80°C for 6 h to obtain a negative oxygen ion layer.

[0056] Step (2): Evenly apply environmentally friendly adhesive on both sides of the polyester fabric, and then bond it to the negative oxygen ion layer. During the bonding process, the polyester fabric is bonded to the side of the negative oxygen ion layer that is not sprayed with microcapsule composite negative oxygen ions, and the fabric is left to stand for 12 hours to obtain a negative oxygen ion fabric.

[0057] Example 4

[0058] This embodiment discloses a method for preparing an environmentally friendly adhesive, comprising the following steps:

[0059] Q1: Polycaprolactone triol with an average relative molecular mass of 550 g / mol was placed in a microwave oven at 120°C and heated for 10 minutes. Then, 1.51 g of polycaprolactone triol and 1.22 g of isophorone diisocyanate were added to the container, followed by 0.1 mL of dibutyltin dilaurate and butanone to reduce the viscosity. The mixture was heated at 85°C for 90 minutes. After the reaction, intermediate product 1 was obtained.

[0060] Q2: 2 g of guar gum and 1.38 g of 2,2-dimethylolpropionic acid were added to 10.93 g of intermediate product 1, and the reaction was continued with stirring for 120 min. Acetone was added during the stirring process to control the viscosity. After the reaction was completed, the temperature was lowered to 60°C, 1.10 g of triethylamine was added, and the reaction was neutralized for 20 min. Subsequently, 0.68 g of ethylenediamine was added, and the mixture was emulsified and dispersed with deionized water for 30 min. Then, stirring was stopped to obtain intermediate product 2;

[0061] Q3: Place the intermediate product 2 in a rotary evaporator and heat at 90°C for 1 hour to obtain an environmentally friendly adhesive.

[0062] This embodiment discloses a method for preparing microcapsule composite negative oxygen ions, comprising the following steps:

[0063] S1: 8 g of agar was added to 120 mL of distilled water, heated and stirred at 90°C for dissolution, and then 10 mL of white mineral oil was added to obtain an agar mixed solution. 7 mL of sorbitan oleate and 120 mL of a 0.05 g / mL gelatin solution were added to 130 mL of the agar mixed solution, heated and stirred at 55°C for 3 h, mixed evenly, and adjusted to pH 3.9 with 10% by volume hydrochloric acid. After cooling, 7 mL of 37% by volume glutaraldehyde was added for cross-linking. The pH was further adjusted to pH 8 with 20% by volume sodium hydroxide. The mixture was stirred, washed, filtered, and dried at 50°C to obtain agar / gelatin microcapsules.

[0064] S2: Dissolve 0.7 g of anhydrous citric acid and 1.4 g of negative oxygen ion powder in 110 mL of distilled water, add 2.5 g of agar / gelatin microcapsules and 3 g of chitosan quaternary ammonium salt, stir for 30 minutes, then add it to 120 mL of β-cyclodextrin solution with a concentration of 18.5 g / L, continue stirring for 2 hours, cool, filter, wash, and dry to obtain microcapsule composite negative oxygen ions.

[0065] This embodiment discloses a method for preparing a negative oxygen ion fabric, comprising the following steps:

[0066] Step (1): ultrasonically disperse 40 g of microcapsule composite negative oxygen ions in 30 mL of distilled water, place the mixture in a spray gun, and evenly spray it on the surface of the cotton cloth. Repeat the operation 5 times, and then dry it at 80°C for 6 h to obtain a negative oxygen ion layer.

[0067] Step (2): Evenly apply environmentally friendly adhesive on both sides of the polyester fabric, and then bond it to the negative oxygen ion layer. During the bonding process, the polyester fabric is bonded to the side of the negative oxygen ion layer that is not sprayed with microcapsule composite negative oxygen ions, and the fabric is left to stand for 12 hours to obtain a negative oxygen ion fabric.

[0068] Comparative Example 5

[0069] This embodiment discloses a method for preparing an environmentally friendly adhesive, comprising the following steps:

[0070] Q1: Polycaprolactone triol with an average relative molecular mass of 550 g / mol was placed in a microwave oven at 120°C and heated for 10 minutes. Then, 1.32 g of polycaprolactone triol and 1.09 g of isophorone diisocyanate were added to the container, followed by 0.1 mL of dibutyltin dilaurate and butanone to reduce the viscosity. The mixture was heated at 85°C for 90 minutes. After the reaction, intermediate product 1 was obtained.

[0071] Q2: 1.1 g of guar gum and 0.97 g of 2,2-dimethylolpropionic acid were added to 5.27 g of intermediate product 1, and the mixture was stirred and reacted for 120 min. Acetone was added during the stirring process to control the viscosity. After the reaction, the temperature was lowered to 60°C, and 0.75 g of triethylamine was added to neutralize the mixture for 20 min. Subsequently, 0.37 g of ethylenediamine was added, and the mixture was emulsified and dispersed with deionized water for 30 min. Then, stirring was stopped to obtain intermediate product 2.

[0072] Q3: Place the intermediate product 2 in a rotary evaporator and heat at 90°C for 1 hour to obtain an environmentally friendly adhesive.

[0073] This embodiment discloses a method for preparing microcapsule composite negative oxygen ions, comprising the following steps:

[0074] S1: 6.0 g of agar was added to 105 mL of distilled water, heated and stirred at 90°C for dissolution, and then 8.5 mL of white mineral oil was added to obtain an agar mixed solution. 5 mL of sorbitan oleate and 105 mL of a 0.05 g / mL gelatin solution were added to 115 mL of the agar mixed solution, heated and stirred at 55°C for 3 h, mixed evenly, and adjusted to pH 3.9 with 10% hydrochloric acid. After cooling, 5.5 mL of 37% glutaraldehyde was added for cross-linking. The pH was further adjusted to pH 8 with 20% sodium hydroxide. The mixture was stirred, washed, filtered, and dried at 50°C to obtain agar / gelatin microcapsules.

[0075] S2: Dissolve 0.55g of anhydrous citric acid and 2g of negative oxygen ion powder in 108mL of distilled water, add 2.1g of agar / gelatin microcapsules and 2.1g of chitosan quaternary ammonium salt, stir for 30min, then add it to 105mL of β-cyclodextrin solution with a concentration of 18.5g / L, continue stirring for 2h, cool, filter, wash, and dry to obtain microcapsule composite negative oxygen ions.

[0076] This embodiment discloses a method for preparing a negative oxygen ion fabric, comprising the following steps:

[0077] Step (1): ultrasonically disperse 32 g of microcapsule composite negative oxygen ions in 22 mL of distilled water, place the mixture in a spray gun, and evenly spray it on the surface of the cotton cloth. Repeat the operation 5 times, and then dry it at 80°C for 6 h to obtain a negative oxygen ion layer.

[0078] Step (2): Evenly apply environmentally friendly adhesive on both sides of the polyester fabric, and then bond it to the negative oxygen ion layer. During the bonding process, the polyester fabric is bonded to the side of the negative oxygen ion layer that is not sprayed with microcapsule composite negative oxygen ions, and the fabric is left to stand for 12 hours to obtain a negative oxygen ion fabric.

[0079] Comparative Example 6

[0080] This embodiment discloses a method for preparing an environmentally friendly adhesive, comprising the following steps:

[0081] Q1: Polycaprolactone triol with an average relative molecular mass of 550 g / mol was placed in a microwave oven at 120°C and heated for 10 minutes. Then, 1.47 g of polycaprolactone triol and 1.13 g of isophorone diisocyanate were added to the container, followed by 0.1 mL of dibutyltin dilaurate and butanone to reduce the viscosity. The mixture was heated at 85°C for 90 minutes. After the reaction, intermediate product 1 was obtained.

[0082] Q2: 1.7 g of guar gum and 1.12 g of 2,2-dimethylolpropionic acid were added to 8.78 g of intermediate product 1, and the reaction was continued with stirring for 120 min. Acetone was added during the stirring process to control the viscosity. After the reaction was completed, the temperature was lowered to 60°C, 0.98 g of triethylamine was added, and the reaction was neutralized for 20 min. Subsequently, 0.52 g of ethylenediamine was added, and the mixture was emulsified and dispersed with deionized water for 30 min. Then, stirring was stopped to obtain intermediate product 2;

[0083] Q3: Place the intermediate product 2 in a rotary evaporator and heat at 90°C for 1 hour to obtain an environmentally friendly adhesive.

[0084] This embodiment discloses a method for preparing microcapsule composite negative oxygen ions, comprising the following steps:

[0085] S1: 7 g of agar was added to 115 mL of distilled water, heated and stirred at 90°C for dissolution, and then 9.5 mL of white mineral oil was added to obtain an agar mixed solution. 8 mL of sorbitan oleate and 110 mL of a 0.05 g / mL gelatin solution were added to 125 mL of the agar mixed solution, heated and stirred at 55°C for 3 h, mixed evenly, and adjusted to pH 3.9 with 10% by volume hydrochloric acid. After cooling, 6.5 mL of 37% by volume glutaraldehyde was added for cross-linking. The pH was further adjusted to pH 8 with 20% by volume sodium hydroxide. The mixture was stirred, washed, filtered, and dried at 50°C to obtain agar / gelatin microcapsules.

[0086] S2: Dissolve 0.65g of anhydrous citric acid and 1.8g of negative oxygen ion powder in 102mL of distilled water, add 2.4g of agar / gelatin microcapsules and 2.7g of chitosan quaternary ammonium salt, stir for 30min, then add it to 115mL of β-cyclodextrin solution with a concentration of 18.5g / L, continue stirring for 2h, cool, filter, wash, and dry to obtain microcapsule composite negative oxygen ions.

[0087] This embodiment discloses a method for preparing a negative oxygen ion fabric, comprising the following steps:

[0088] Step (1): ultrasonically disperse 38 g of microcapsule composite negative oxygen ions in 27 mL of distilled water, place the mixture in a spray gun, and evenly spray it on the surface of the cotton cloth. Repeat the operation 5 times, and then dry it at 80°C for 6 h to obtain a negative oxygen ion layer.

[0089] Step (2): Evenly apply environmentally friendly adhesive on both sides of the polyester fabric, and then bond it to the negative oxygen ion layer. During the bonding process, the polyester fabric is bonded to the side of the negative oxygen ion layer that is not sprayed with microcapsule composite negative oxygen ions, and the fabric is left to stand for 12 hours to obtain a negative oxygen ion fabric.

[0090] Comparative Example 1

[0091] Comparative Example 1 Compared with Example 2, in the process of preparing the environmentally friendly adhesive in Comparative Example 1, no polycaprolactone triol was added, and other conditions remained unchanged.

[0092] Comparative Example 2

[0093] Comparative Example 2 Compared with Example 2, in the process of preparing the environmentally friendly adhesive in Comparative Example 2, guar gum was not added, and other conditions remained unchanged.

[0094] Comparative Example 3

[0095] Comparative Example 3 Compared with Example 2, in the process of preparing the environmentally friendly adhesive in Comparative Example 3, no 2,2-dihydroxymethylpropionic acid was added, and other conditions remained unchanged.

[0096] Comparative Example 4

[0097] Comparative Example 4 Compared with Example 2, in the process of preparing microcapsule composite negative oxygen ions in Comparative Example 4, no agar was added, and other conditions remained unchanged.

[0098] Comparative Example 5

[0099] Comparative Example 5 Compared with Example 2, in the process of preparing microcapsule composite negative oxygen ions in Comparative Example 5, no negative oxygen ion powder is added, and other conditions remain unchanged.

[0100] Comparative Example 6

[0101] Comparative Example 6 Compared with Example 2, in the process of preparing microcapsule composite negative oxygen ions in Comparative Example 6, no chitosan quaternary ammonium salt was added, and other conditions remained unchanged.

[0102] Comparative Example 7

[0103] Comparative Example 7 Compared with Example 2, in the process of preparing the negative oxygen ion fabric in Comparative Example 7, no environmentally friendly adhesive is added, and other conditions remain unchanged.

[0104] Comparative Example 8

[0105] Comparative Example 8 Compared with Example 2, in the process of preparing the negative oxygen ion fabric in Comparative Example 8, no microcapsule composite negative oxygen ions are added, and other conditions remain unchanged.

[0106] The negative oxygen ion fabrics prepared in Examples 2-6 and Comparative Examples 1-8 were placed in a closed box respectively, and the negative oxygen ion concentrations at different times were detected using a negative oxygen ion detector. The antibacterial properties of the samples were tested according to WS / T 650-2019, and the waterproof properties of the samples were tested according to GB / T 4744-2013. The waterproof properties were judged according to the relationship between the hydrostatic pressure value P and the net water pressure resistance level. When P < 4 kPa, the hydrostatic pressure resistance level is level 0, indicating poor hydrostatic pressure resistance and poor waterproof effect. When 4 kPa ≤ P < 13 kPa, the hydrostatic pressure resistance level is level 1, indicating that it has hydrostatic pressure resistance and a general waterproof effect. When 13 kPa ≤ P < 20 kPa, the hydrostatic pressure resistance level is level 2, indicating that it has good hydrostatic pressure resistance and a general waterproof effect. The anti-hydrostatic pressure performance and waterproof effect are average. When 20kPa≤P<35kPa, the anti-hydrostatic pressure grade is level 3, indicating good anti-hydrostatic pressure performance and good waterproof effect. When 35kPa≤P<50kPa, the anti-hydrostatic pressure grade is level 4, indicating excellent anti-hydrostatic pressure performance and excellent waterproof effect. When 50kPa≤P, the anti-hydrostatic pressure grade is level 5, indicating excellent anti-hydrostatic pressure performance and excellent waterproof effect. The test results are shown in Table 1:

[0107] Table 1

[0108]

[0109] It can be seen from the test results in Table 1 that by using the method of Examples 2-6, the sustained-release time and antibacterial properties of negative oxygen ions in negative oxygen ion fabrics can be effectively improved. By comparing Comparative Example 1 with Examples 2-6, it can be found that adding polycaprolactone triol can effectively improve the waterproofness of negative oxygen ion fabrics; by comparing Comparative Example 2 with Examples 2-6, it can be found that adding guar gum can effectively improve the waterproofness of negative oxygen ion fabrics; by comparing Comparative Example 3 with Examples 2-6, it can be found that adding 2,2-dihydroxymethylpropionic acid can effectively improve the waterproofness of negative oxygen ion fabrics; by comparing Comparative Example 4 with Examples 2-6, it can be found that adding agar can effectively improve the sustained-release time of negative oxygen ions in negative oxygen ion fabrics; by comparing Comparative Example 5 with Examples 2-6, it can be found that It was found that adding negative oxygen ion powder can effectively increase the negative oxygen ion concentration and the sustained-release time of negative oxygen ions of negative oxygen ion fabrics; by comparing Comparative Example 6 with Examples 2-6, it can be found that adding chitosan quaternary ammonium salt can effectively increase the sustained-release time and antibacterial properties of negative oxygen ions; by comparing Comparative Example 7 with Examples 2-6, it can be found that adding environmentally friendly adhesives can effectively improve the waterproofness of negative oxygen ion fabrics; by comparing Comparative Example 8 with Examples 2-6, it can be found that adding microcapsule composite negative oxygen ions can effectively increase the negative oxygen ion concentration, sustained-release time and antibacterial properties of negative oxygen ion fabrics.

[0110] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

[0111] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A negative oxygen ion fabric, characterized in that: It includes a negative oxygen ion layer and a base fabric layer. The negative oxygen ion layer is tightly bonded to both sides of the base fabric layer by an environmentally friendly adhesive. The negative oxygen ion layer is made of microcapsule composite negative oxygen ions and cotton fabric, and the base fabric is made of polyester fabric. The preparation method of the negative oxygen ion fabric comprises the following steps: Step (1): ultrasonically disperse the microcapsule composite negative oxygen ions in distilled water and place them in a spray gun, spraying them evenly on the surface of the cotton cloth, repeating the operation, and then drying to obtain a negative oxygen ion layer; Step (2): evenly coating both sides of the polyester fabric with an environmentally friendly adhesive, then bonding it to the negative oxygen ion layer and allowing it to stand to obtain a negative oxygen ion fabric; The preparation method of the microcapsule composite negative oxygen ion comprises the following steps: S1: adding agar to distilled water, heating and stirring to dissolve, adding white mineral oil to obtain an agar mixed solution, adding sorbitan oleate and gelatin solution to the agar mixed solution, heating and stirring, mixing uniformly, adjusting the pH, cooling, adding glutaraldehyde for cross-linking, continuing to adjust the pH, stirring, washing, filtering, and drying to obtain agar / gelatin microcapsules; S2: dissolving anhydrous citric acid and negative oxygen ion powder in distilled water, adding agar / gelatin microcapsules and chitosan quaternary ammonium salt, stirring, and then adding them to the β-cyclodextrin solution, continuing to stir, cooling, filtering, washing, and drying to obtain microcapsule composite negative oxygen ions; In S1, the amount ratio of agar, distilled water, and white mineral oil is (5-8) g: (100-120) mL: (8-10) mL, the heating temperature is 80-90°C, the volume ratio of sorbitan oleate, gelatin solution, agar mixed solution, and glutaraldehyde is (5-8) mL: (100-120) mL: (110-130) mL: (5-7) mL, the concentration of the gelatin solution is 0.05 g / mL, the heating and stirring temperature is 50-55°C, the time is 2-4 hours, the pH is adjusted to 3.8-4.1 with 10% by volume hydrochloric acid, the volume fraction of glutaraldehyde is 37% by volume, and the pH is further adjusted to 8-9 with 20% by volume sodium hydroxide. The drying temperature is 50-60°C. In S2, the dosage ratio of anhydrous citric acid, negative oxygen ion powder, distilled water, agar / gelatin microcapsules, chitosan quaternary ammonium salt and β-cyclodextrin solution is (0.5-0.7) g: (1-2) g: (100-110) mL: (2.0-2.5) g: (2-3) g: (100-120) mL, the stirring time is 30-50 min, the concentration of the β-cyclodextrin solution is 18.5 g / L, and the stirring time is continued for 1-2 h.

2. A negative oxygen ion fabric according to claim 1, characterized in that: The preparation method of the environmentally friendly adhesive comprises the following steps: Q1: Dehydrated polycaprolactone triol and isophorone diisocyanate are added to a container, followed by dibutyltin dilaurate, and heated for reaction. After the reaction is completed, intermediate product 1 is obtained. Q2: Add guar gum and 2,2-dimethylolpropionic acid to intermediate product 1, continue stirring and reacting, cool down after the reaction, add triethylamine to neutralize the reaction, then add ethylenediamine, emulsify and disperse with deionized water, and then stop stirring to obtain intermediate product 2; Q3: Place the intermediate product 2 in a rotary evaporator and heat it to react to obtain an environmentally friendly adhesive; In Q1, the dehydration process is as follows: placing polycaprolactone triol in a microwave oven at 110-130°C for 10-12 minutes, wherein the molar ratio of polycaprolactone triol to isophorone diisocyanate is (0.9-1.1): (1.8-2.2), the heating reaction temperature is 80-85°C, and the heating time is 90-120 minutes; In Q2, the molar ratio of guar gum, 2,2-dihydroxymethylpropionic acid, intermediate 1, triethylamine and ethylenediamine is (1-2): (1.1-1.9): (0.9-2.1): (1-2): (0.9-2.1), the stirring reaction time is continued for 90-120 minutes, the temperature is lowered to 60-65°C, the neutralization reaction time is 20-40 minutes, and the emulsification dispersion time is 30-45 minutes; in Q3, the heating temperature is 80-90°C, and the reaction time is 1-2 hours.

3. The negative oxygen ion fabric according to claim 1, characterized in that: In the step (1), the ratio of the microcapsule composite negative oxygen ions to distilled water is (30-40) g: (20-30) mL, the operation is repeated 3-5 times, the drying temperature is 80-90°C, and the drying time is 6-8 hours.

4. The negative oxygen ion fabric according to claim 1, characterized in that: In the step (2), during the bonding process, the polyester fabric is bonded to the side of the negative oxygen ion layer that is not sprayed with microcapsule composite negative oxygen ions, and the standing time is 8-12 hours.

Images