Method for preparing cool-feeling hole-cutting liquid surface layer material through emulsion electrostatic spinning and application of cool-feeling hole-cutting liquid surface layer material

Abstract

The invention relates to the technical field of composite materials, in particular to a method for preparing a cool-feeling hole-cutting liquid surface layer material by emulsion electrostatic spinning, which comprises the following steps: by taking an emulsified polyurethane solution as a raw material, introducing hydrophobic modified xylitol and a soft component; the preparation method comprises the following steps: spraying and coating a non-woven fabric with an emulsion through electrostatic spinning of the emulsion to obtain a nanofiber non-woven fabric composite material, and then carrying out hydrophobic modification and fine punching treatment to prepare a punching liquid surface layer material with cool feeling, softness, low reverse osmosis, high fluid absorption speed and biodegradability. The material can be applied to the fields of high-end hygienic products, medical treatment, clothing, air filtration and the like, and has a wide application prospect.

Description

Technical Field

[0001] The present invention relates to the technical field of composite materials, and in particular to a method for preparing a cool-feeling pore-cutting liquid surface layer material by emulsion electrostatic spinning and an application thereof. Background Art

[0002] Polyurethane composites are widely used in the preparation of daily necessities, but traditional methods make it difficult to improve their spinnability under certain functional requirements. There are deficiencies in imparting specific functions (such as a cool feeling) and optimizing material properties (such as softness, water resistance, fluid absorption efficiency, etc.), especially when used as skin-friendly layer materials.

[0003] For example, patent application CN1445390A discloses a method and apparatus for producing polyurethane elastic nonwoven fabrics by melt-blowing. Polyurethane particles are fed into a screw extruder, heated and melted at 180-260°C, and then extruded from spinnerets in a die head. Hot air flows from both sides of the spinnerets stretch the melt into ultrafine fibers, which then self-bond to form the polyurethane elastic nonwoven fabric of the present invention. This product offers excellent softness and comfort, but its functionality is limited, resulting in a poor user experience.

[0004] Therefore, the existing technology for the above problems still needs to be improved and developed. Summary of the Invention

[0005] The present invention aims to overcome the shortcomings of the prior art by providing a method and application for preparing a cooling, cut-hole liquid surface material by emulsion electrospinning. This cooling, cut-hole liquid surface material significantly improves the spinnability of polyurethane composites and exhibits a sustained cooling effect, high fluid absorption efficiency, and excellent properties such as softness, reverse osmosis, and biodegradability.

[0006] In order to achieve the above object, the present invention is implemented through the following technical solutions: The present invention provides a method for preparing a cool, pore-cutting liquid surface layer material by emulsion electrospinning, comprising the following steps: S1. Weigh a certain amount of polyurethane and dissolve it in an organic solvent to prepare a polyurethane solution.

[0007] S2. Add the polyurethane solution and emulsifier obtained in step S1 into an emulsifying kettle and shear at high speed to obtain a polyurethane emulsion.

[0008] S3. Refluxing siloxane with xylitol to obtain hydrophobically modified xylitol; S4. The hydrophobically modified xylitol prepared in step S3 is added together with a softener to the polyurethane emulsion prepared in step S2, and the mixture is stirred thoroughly to uniformly disperse the mixture to obtain a mixed emulsion.

[0009] S5. The mixed emulsion obtained in step S4 is sprayed onto the surface of the non-woven fabric using an emulsion electrospinning device to obtain a nanofiber non-woven fabric composite material.

[0010] S6. Immerse the nanofiber nonwoven fabric composite material in a solution containing a hydrophobic finishing agent. After sufficient immersion, remove excess solution by roller squeezing and dry the composite material to obtain a hydrophobically modified nanofiber nonwoven fabric composite material.

[0011] S7. Mechanically cut holes in the hydrophobically modified nanofiber non-woven fabric composite material obtained in step S6 to obtain a cool hole-cut liquid surface layer material.

[0012] According to the above scheme, the concentration of the polyurethane solution prepared in step S1 is 150-250 mg / ml.

[0013] According to the above scheme, the emulsifier in step S2 is selected from one of nonionic emulsifiers or cationic emulsifiers, the weight ratio of the polyurethane solution to the emulsifier is 100:5-10, the high-speed shearing is 1200 revolutions per minute, and the shearing time is 30-45 minutes.

[0014] According to the above scheme, the siloxane in step S3 is one or two of fluorosilicone, dimethylsiloxane and hexamethylsiloxane, the molar ratio of xylitol to siloxane is 1:0.9-1.1, the reflux reaction time is 12-24 hours, and the reaction temperature is 70°C.

[0015] According to the above scheme, the weight ratio of the polyurethane emulsified solution prepared in step S2 to the hydrophobically modified xylitol and softener prepared in step S3 is 100:20-35:10.

[0016] According to the above scheme, the electrospinning voltage in step S5 is 15-20 kV, the flow rate is 0.5-1.5 mL / h, and the receiving distance is 15-20 cm.

[0017] According to the above solution, the non-woven fabric in step S5 is selected from hot air non-woven fabric, spunbond non-woven fabric or spunlace non-woven fabric.

[0018] According to the above scheme, the hydrophobic finishing agent in step S6 is one or more of amino silicone oil, hydroxyl-terminated polysiloxane, alkoxysilane, C6 short-chain fluoride, fluorine-free water-repellent finishing agent, calcium stearate, stearic acid amide, acrylate copolymer, polyurethane-organic silicon block copolymer, organosilicon-fluorocarbon composite finishing agent, and nano-silica composite finishing agent. The mass-volume concentration of the hydrophobic finishing agent solution is 6-8.0 g / L, the immersion time is 0.1-5 min, and after sufficient immersion, the nanofiber non-woven fabric composite material after removing excess solution by a pressing roller is dried at 80-150°C for 10-15 min to obtain a hydrophobically modified nanofiber non-woven fabric composite material.

[0019] According to the above scheme, the cutting process in step S7 is one of laser cutting, mechanical cutting, and ultrasonic cutting, and regular holes are accurately cut into the hydrophobically modified nanofiber non-woven fabric composite material. The preset cutting parameters are: the hole shape is circular, the hole diameter is 1mm-8mm, and the hole spacing is 1-8mm.

[0020] According to the above scheme, the cool-feeling perforated liquid surface layer material is used in sanitary products such as sanitary napkins, menstrual pants, incontinence napkins, incontinence pants, diapers, disposable underwear, and wound dressings.

[0021] The beneficial effects of the present invention are: (1) The present invention significantly improves the spinnability of polyurethane by constructing an emulsion system. Using the emulsified polyurethane solution as the raw material, the diameter, porosity and other parameters of the fiber can be precisely adjusted to meet the needs of different application scenarios.

[0022] (2) The present invention performs hydrophobic modification on xylitol, which has a cooling effect, by introducing siloxane hydrophobic groups into its molecules to change its surface properties, making it easier to disperse evenly in the nanofiber nonwoven fabric and continuously exerting a cooling effect.

[0023] (3) The present invention performs hydrophobic finishing on the nanofiber nonwoven fabric composite material to form an extremely low surface energy molecular layer on its surface, which effectively blocks water penetration, improves waterproof performance, and reduces liquid surface residue.

[0024] (4) The present invention uses a large number of tiny holes constructed by mechanically cutting the nanofiber non-woven fabric composite material, which greatly increases the liquid infiltration rate. In the fields of sanitary products, medical wound dressings, etc., it can quickly absorb liquid and promote diffusion or discharge. Combined with the structure of the non-woven fabric, it also helps liquid conduction, further improving the absorption efficiency.

[0025] (5) The present invention reasonably selects polyurethane raw materials and additives to prepare a cutting liquid surface material that is biodegradable and meets environmental protection requirements. DETAILED DESCRIPTION

[0026] In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with examples, but the present invention is not limited to the following examples. Example

[0027] This embodiment provides a method for preparing a cool, pore-cutting liquid surface layer material by emulsion electrospinning: S1. Weigh 15 g of polyurethane and dissolve it in 100 ml of N,N-dimethylformamide to prepare a polyurethane solution with a concentration of 150 mg / ml.

[0028] S2. 100 parts by weight of the polyurethane solution obtained in step S1 and 5 parts by weight of a nonionic emulsifier polyoxy-10-nonyl ether were added to an emulsifier, and high-speed shearing was performed at 1200 revolutions per minute for 30 minutes to obtain a polyurethane emulsion.

[0029] S3. The fluorosilicone and xylitol were mixed in a molar ratio of 1:0.9 and refluxed at 70°C for 13 hours to obtain a hydrophobically modified xylitol; S4. The polyurethane emulsified solution prepared in step S2 and the hydrophobically modified xylitol and softener prepared in step 3 are added to the polyurethane emulsion prepared in step S2 in a weight ratio of 100:20:10, and stirred thoroughly to uniformly disperse them to obtain a mixed emulsion.

[0030] S5. The mixed emulsion prepared in step S4 was sprayed onto the surface of a polypropylene hot air nonwoven fabric with a total weight of 20 g / m² using an emulsion electrospinning device at an electrospinning voltage of 15 kV, a flow rate of 0.5 mL / h, and a receiving distance of 15 cm to prepare a nanofiber nonwoven fabric composite material.

[0031] S6. Immerse the nanofiber nonwoven fabric composite material obtained in step S5 in an amino silicone oil solution with a mass-volume concentration of 6.0 g / L for 0.1 min. After sufficient immersion, remove excess solution from the nanofiber nonwoven fabric composite material by squeezing with a roller and dry it at 80°C for 10 min to obtain a hydrophobically modified nanofiber nonwoven fabric composite material.

[0032] S7. The hydrophobically modified nanofiber nonwoven composite material obtained in step S6 is mechanically cut using a CNC blade cutting device. The preset cutting parameters are: circular hole shape, hole diameter of 1 mm and hole spacing of 1 mm to obtain a cooling hole-cut liquid surface material. Example

[0033] This embodiment provides a method for preparing a cool, pore-cutting liquid surface layer material by emulsion electrospinning: S1. Weigh 20 g of polyurethane and dissolve it in 100 ml of N,N-dimethylformamide to prepare a polyurethane solution with a concentration of 200 mg / ml.

[0034] S2. 100 parts by weight of the polyurethane solution obtained in step S1 and 7.5 parts by weight of a cationic emulsifier cetyltrimethylammonium bromide were added to an emulsifying vessel and sheared at 1200 rpm for 37.5 minutes to obtain a polyurethane emulsion.

[0035] S3. Dimethylsiloxane and xylitol were mixed in a molar ratio of 1:1 and refluxed at 70°C for 18 hours to obtain hydrophobically modified xylitol; S4. The polyurethane emulsified solution obtained in step S2 and the hydrophobically modified xylitol and softener obtained in step S3 are added to the reactor in a weight ratio of 100:30:10, and stirred thoroughly to uniformly disperse them to obtain a mixed emulsion.

[0036] S5. The mixed emulsion obtained in step S4 was sprayed onto the surface of a polypropylene spunbond nonwoven fabric having a gram weight of 30 g / m² using an emulsion electrospinning device at an electrospinning voltage of 17.5 kV, a flow rate of 1 mL / h, and a receiving distance of 17.5 cm to obtain a nanofiber nonwoven composite material.

[0037] S6. Immerse the nanofiber nonwoven fabric composite material obtained in step S5 in a stearic acid amide solution with a mass-volume concentration of 7.0 g / L for 3 minutes. After sufficient immersion, remove excess solution from the nanofiber nonwoven fabric composite material by a pressing roller and dry it at 115°C for 12.5 minutes to obtain a hydrophobically modified nanofiber nonwoven fabric composite material.

[0038] S7. The hydrophobically modified nanofiber nonwoven composite material obtained in step S6 is mechanically cut using a CNC blade cutting device, with the preset cutting parameters being: a circular hole shape, a hole diameter of 4.5 mm, and a hole spacing of 4.5 mm. Example

[0039] This embodiment provides a method for preparing a cool, pore-cutting liquid surface layer material by emulsion electrospinning: S1. Weigh 25 g of polyurethane and dissolve it in 100 ml of N,N-dimethylformamide to prepare a polyurethane solution with a concentration of 250 mg / ml.

[0040] S2. 100 parts by weight of the polyurethane solution obtained in step S1 and 10 parts by weight of a cationic emulsifier, cetyltrimethylammonium bromide, were added to an emulsifying vessel and sheared at 1200 rpm for 45 minutes to obtain a polyurethane emulsion.

[0041] S3 vinyl dimethylsiloxane and hexamethylsiloxane were mixed in a molar ratio of 1:1, and then mixed with xylitol in a molar ratio of 1:1.1, and the mixture was refluxed at 70 ° C for 24 hours to obtain hydrophobically modified xylitol; S4. The polyurethane emulsified solution obtained in step S2 and the hydrophobically modified xylitol and softener obtained in step S3 are added to the reactor in a weight ratio of 100:35:10, and stirred thoroughly to uniformly disperse them to obtain a mixed emulsion.

[0042] S5. The mixed emulsion prepared in step S4 was sprayed onto the surface of a 100% pure polyester spunlace nonwoven fabric with a weight of 40 g / m² using an emulsion electrospinning device at an electrospinning voltage of 20 kV, a flow rate of 1.5 mL / h, and a receiving distance of 20 cm to produce a nanofiber nonwoven composite material.

[0043] S6. Immerse the nanofiber nonwoven fabric composite material obtained in step S5 in an acrylic ester copolymer solution with a mass-volume concentration of 8.0 g / L for 5 minutes. After sufficient immersion, remove excess solution from the nanofiber nonwoven fabric composite material by a pressing roller and dry it at 150°C for 15 minutes to obtain a hydrophobically modified nanofiber nonwoven fabric composite material.

[0044] S7. The hydrophobically modified nanofiber nonwoven composite material obtained in step S6 is mechanically cut using a CNC blade cutting device. The preset cutting parameters are: circular hole shape, hole diameter of 8 mm and hole spacing of 8 mm to obtain a cool hole-cut liquid surface material.

[0045] Comparative Example 1 The steps and process parameters are basically the same as those in Example 3, except that the xylitol is not subjected to hydrophobic treatment.

[0046] Comparative Example 2 The steps and process parameters are basically the same as those in Example 3, except that the nanofiber nonwoven fabric composite material prepared in step S5 is not immersed in a fluorine-containing hydrophobic finishing agent solution for treatment.

[0047] Comparative Example 3 The steps and process parameters are basically the same as those in Example 3, except that the nanofiber non-woven fabric composite material prepared in step S6 is not subjected to mechanical pore cutting.

[0048] The liquid surface layer materials prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to physical property tests of cooling sensation, absorption rate and reverse osmosis value. The test methods and test data are as follows: 1) Cooling sensation: Tested in accordance with GB / T 35263-2017 3) Absorption rate: Use a pipette to draw 5 ml of test liquid and inject it into the center of the test sample. Start timing at the same time and record the time it takes for the liquid to disappear. 4) Reverse Osmosis Value: Pipette 5 ml of test liquid into the center of the test sample. After leaving the sample for five minutes, place a piece of filter paper in the center of the test sample and press the filter paper with a 2.5 kg weight for 2 minutes. Measure the weight gain of the filter paper. Repeat three times. The total weight gain of the three times is the reverse osmosis value.

[0049] Table 1 Sample <![CDATA[Cooling sensation Qmax (W / cm 2 )]]> Absorption rate / s Reverse osmosis value / g Example 1 0.285 6 0.06 Example 1 0.292 4 0.05 Example 1 0.302 3 0.03 Comparative Example 1 0.258 3 0.04 Comparative Example 2 0.295 3 0.35 Comparative Example 3 0.298 12 0.06 As can be seen from the above, the cooling pore-cut liquid surface layer material prepared by the present method has excellent liquid absorption performance and reverse osmosis performance, and has a good cooling effect; by comparing Examples 1-3 with Comparative Example 1, it can be seen that the product with the addition of hydrophobically modified xylitol has better cooling performance; by comparing Examples 1-3 with Comparative Example 2, it can be seen that the reverse osmosis value of the product impregnated with the hydrophobic finishing agent solution is reduced by 0.29g compared with the product not impregnated with the hydrophobic finishing agent solution, and the reverse osmosis performance is significantly improved; by comparing Examples 1-3 with Comparative Example 3, it can be seen that the absorption speed of the product with fine pores is increased by up to 9S compared with the product without fine pores, and has excellent absorption rate improvement.

[0050] The above description is only a preferred embodiment of the present invention. Therefore, any equivalent changes or modifications made according to the structure, characteristics and principles described in the scope of the patent application of the present invention are included in the scope of the patent application of the present invention.

Claims

1. A method for preparing a cool, pore-cutting liquid surface material by emulsion electrospinning, characterized in that: The following steps are involved: S1. Weigh a certain amount of polyurethane and dissolve it in an organic solvent to prepare a polyurethane solution; S2. The polyurethane solution obtained in step S1 and the emulsifier are added to an emulsifier and sheared at high speed to obtain a polyurethane emulsion; S3. Refluxing siloxane with xylitol to obtain hydrophobically modified xylitol; S4. The hydrophobically modified xylitol prepared in step S3 is added together with a softener to the polyurethane emulsion prepared in step S2 and stirred thoroughly to obtain a uniform dispersion to obtain a mixed emulsion; S5. The mixed emulsion obtained in step S4 is sprayed onto the surface of the nonwoven fabric using an emulsion electrospinning device to obtain a nanofiber nonwoven composite material; S6. The nanofiber nonwoven composite material is immersed in a hydrophobic finishing agent solution, fully impregnated, and then the excess solution is removed by roller extrusion and dried to obtain a hydrophobically modified nanofiber nonwoven composite material; S7. Cut holes in the hydrophobically modified nanofiber non-woven fabric composite material obtained in step S6 to obtain a cool hole-cut liquid surface layer material.

2. The method for preparing a cool-feeling cut-hole liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: The concentration of the polyurethane solution prepared in step S1 is 150-250 mg / ml.

3. The method for preparing a cool cut-hole liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: In step S2, the emulsifier is selected from one of a nonionic emulsifier and a cationic emulsifier, the weight ratio of the polyurethane solution to the emulsifier is 100:5-10, the high-speed shearing is 1200 revolutions per minute, and the shearing time is 30-45 minutes.

4. The method for preparing a cool, pore-cutting liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: The siloxane in step S3 is one or two of fluorosilicone, dimethylsiloxane and hexamethylsiloxane, the molar ratio of xylitol to siloxane is 1:0.9-1.1, the reflux reaction time is 12-24 hours, and the reaction temperature is 70°C.

5. The method for preparing a cool, pore-cutting liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: The weight ratio of the polyurethane emulsified solution prepared in step S2 to the hydrophobically modified xylitol and softener prepared in step S3 is 100:20-35:

10.

6. The method for preparing a cool-feeling cut-hole liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: In step S5, the electrospinning voltage is 15-20 kV, the flow rate is 0.5-1.5 mL / h, and the receiving distance is 15-20 cm.

7. The method for preparing a cool cut-hole liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: The non-woven fabric in step S5 is selected from hot air non-woven fabric, spunbond non-woven fabric or spunlace non-woven fabric.

8. The method for preparing a cool, pore-cutting liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: The hydrophobic finishing agent in step S6 is one or more of amino silicone oil, hydroxyl-terminated polysiloxane, alkoxysilane, C6 short-chain fluoride, fluorine-free water-repellent finishing agent, calcium stearate, stearamide, acrylate copolymer, polyurethane-silicone block copolymer, silicone-fluorocarbon composite finishing agent, and nano-silica composite finishing agent. The mass-volume concentration of the hydrophobic finishing agent solution is 6-8.0 g / L, the immersion time is 0.1-5 min, and the nanofiber non-woven fabric composite material after removing excess solution by a pressing roller is dried at 80-150° C. for 10-15 min to obtain a hydrophobically modified nanofiber non-woven fabric composite material.

9. The method for preparing a cool-feeling cut-hole liquid surface layer material by emulsion electrospinning according to claim 1, characterized in that: The cutting process in step S7 is one of laser cutting, mechanical cutting, and ultrasonic cutting, and the hydrophobically modified nanofiber non-woven fabric composite material is precisely cut into regular holes. The preset cutting parameters are: the hole shape is circular, the hole diameter is 1mm-8mm, and the hole spacing is 1-8mm.

10. Use of the cool perforated liquid surface layer material prepared according to any one of claims 1 to 9 in sanitary products such as sanitary napkins, menstrual pants, incontinence napkins, incontinence pants, diapers, disposable underwear, and wound dressings.