ES large biological fiber containing biologically active ingredients and preparation method thereof
By pretreating bioactive molecules and blending them with polyethylene particles and polyester slices, ES large biofibers are prepared by composite spinning technology, which solves the problems of bioactive molecules being not resistant to high temperatures and products being not resistant to washing, and achieves efficient and long-lasting biological activity and excellent mechanical properties.
Patent Information
- Application Number
- CN202410945603.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-15
- Publication Date
- 2025-03-14
- Estimated Expiration
- 2044-07-15
AI Technical Summary
During the production process of existing ES large biofibers, the bioactive molecules are directly added to high temperatures and reduce their efficacy; the spinning ES fibers are modified, and the product is not resistant to washing and its efficacy is not long-lasting.
The bioactive molecules are pretreated by blending sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and bioactive molecules, and the pretreated bioactive ingredients are mixed with polyethylene particles and polyester slices through composite spinning equipment. ES large biofibers are prepared through melt extrusion, composite silk formation, cooling and drafting.
It improves the functional stability and durability of bioactive molecules, enhances the comprehensive performance of fibers such as antibacterial, anti-inflammatory, hygroscopic, and breathable. The product has excellent washing resistance and mechanical properties, and is suitable for a variety of application fields.
Smart Images

Figure BDA0004945530620000141
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of composite fibers, and more specifically, to an ES large biological fiber containing biologically active components and a preparation method thereof. Background Art
[0002] ES fiber is a two-component composite fiber with a skin-core structure developed by Chisso Corporation of Japan, in which the skin layer is made of PE and the core layer is made of PP or PET. ES fiber has the characteristics of good softness, low melting point of the outer layer, high melting point of the inner layer, and high strength. After subsequent thermal processing, part of the skin layer of ES fiber is melted and bonded, and the remaining fibers remain in the fiber state, which not only maintains the fluffy and soft characteristics of the fiber, but also does not destroy the structure of the fiber. It has high strength. Most of the existing ES fibers are used in disposable sanitary materials, including sanitary napkins, diapers, masks, etc. With the continuous improvement of the national economic level, the demand for disposable sanitary products continues to grow, and people have higher and higher requirements for the antibacterial properties, comfort and other functional properties of ES fibers.
[0003] ES large biofiber refers to an active fiber with biological functions produced by modification with bioactive molecules. Bioactive molecules refer to one or more bioactive substances with broad-spectrum antibacterial, antiviral, antioxidant and other effects obtained from natural plants by physical or chemical separation and extraction methods. Bioactive molecules generally have problems such as poor thermal stability and high temperature resistance. When directly added and melt-blended with spinning raw materials to prepare ES fibers, on the one hand, the bioactive molecules are easily carbonized or lost, reducing their efficacy; on the other hand, direct addition will also have adverse effects on the mechanical strength of ES fibers, the air permeability of fiber products, etc. In the prior art, bioactive molecules are often used to modify ES fibers that have completed spinning, but the ES fiber products obtained by direct modification generally have problems such as poor wash resistance and short-lasting efficacy. Based on the above statements, the present invention proposes an ES large biofiber containing bioactive ingredients and a preparation method thereof. Summary of the invention
[0004] In order to solve the problems that the direct addition of bioactive molecules in the existing ES large biofiber production process is not resistant to high temperatures, thereby reducing its efficacy; the ES fibers that have been spun are modified, the products are not resistant to washing, and the efficacy is not long-lasting, etc., the present invention provides an ES large biofiber containing bioactive ingredients and a preparation method thereof.
[0005] In order to achieve the above object, the present invention is implemented by the following technical solutions:
[0006] A ES large biological fiber containing biologically active ingredients and a preparation method thereof, comprising the following steps:
[0007] S1. Preparation of biologically active ingredients:
[0008] The bioactive molecules, sodium lignin sulfonate, and polyethylene glycol dimethanesulfonate are added to an ethanol solution and stirred evenly to obtain a mixed solution; the calcined diatomaceous earth is ground and modified, and then ultrasonically pre-dispersed with deionized water to obtain a dispersion solution; the dispersion solution is then added to the mixed solution and ultrasonically dispersed and mixed for 1-2 hours, and then spray-dried to obtain the dispersion solution;
[0009] S2, mixing the bioactive component with polyethylene particles to obtain a cortex material, and mixing the bioactive component with polyester chips to obtain a core material;
[0010] S3. Use composite spinning equipment to feed the skin layer material and the core layer material into two sets of screw extruders for melt extrusion respectively. The obtained skin layer melt and core layer melt are compounded into filaments through composite spinning components, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber.
[0011] Preferably, the bioactive molecule in step S1 includes at least one of chamomile extract, wormwood extract, peppermint extract, green tea extract, calendula extract, bamboo leaf extract, orange extract, protein, and tea tree oil.
[0012] Preferably, the bioactive molecules in step S1 include chamomile extract and tea tree oil in a mass ratio of 4-7:1.
[0013] Preferably, in step S1, the mass ratio of the bioactive molecule, sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and ethanol solution is 5-7:2-4:1:17-20.
[0014] Preferably, the grinding and modification of the calcined diatomite in step S1 specifically refers to: grinding the calcined diatomite and the modifier at a mass ratio of 3:0.3-0.5 for 1-2 hours, controlling the grinding pressure to 70-90 kPa and the grinding speed to 45-55 rpm.
[0015] Preferably, in step S1, the ultrasonic power is 320-380 W, the ultrasonic frequency is 20-40 kHz, and the ultrasonic time is 10-20 min.
[0016] Preferably, the spray pressure is 0.4-0.6 MPa, the feed rate is 10-15 mL / min, the air inlet temperature is 40-50° C., and the drying time is 30-40 min.
[0017] Preferably, the modifier comprises sodium polyacrylate and adipic acid dihydrazide in a mass ratio of 6.5-8.5:1.
[0018] Preferably, in step S1, the mass ratio of the calcined diatomite to the deionized water is 1:27-30; and the mass ratio of the dispersion to the mixed solution is 1.5-2:1.
[0019] Preferably, in step S2, the mass ratio of the bioactive component to the polyethylene particles is 1:10-15; the mass ratio of the bioactive component to the polyester chips is 1:22-28.
[0020] Preferably, in step S3, the mass ratio of the skin layer material to the core layer material is 1-2:1-2.5.
[0021] Preferably, in step S3, the spinning box temperature is 250-270°C, the spinning speed is 1000-1800m / min; the side blowing temperature is 18-22°C, the side blowing humidity is 80-90%, and the side blowing rate is 1.2-1.8m / s; the drafting multiple is 3.8-5.5 times, and the drafting temperature is 70-100°C.
[0022] An ES large biological fiber containing biologically active components is prepared by the above-mentioned method for preparing the ES large biological fiber containing biologically active components.
[0023] In summary, the present invention has the following beneficial effects:
[0024] 1. The present invention adopts chamomile extract and tea tree oil, both of which have significant antibacterial and anti-inflammatory effects, as biologically active molecules. The combination of the two can produce a synergistic effect, enhance the antibacterial effect, and effectively inhibit the growth of various bacteria and fungi; chamomile extract and tea tree oil are both natural ingredients with good biocompatibility. In addition to antibacterial and anti-inflammatory effects, they can also provide multiple functions such as soothing, repairing and cleaning, reduce irritation to human skin, and are suitable for the preparation and addition of disposable sanitary products.
[0025] 2. The present invention uses sodium lignin sulfonate, polyethylene glycol dimethane sulfonate and bioactive molecules to blend and pretreat the bioactive molecules; on the one hand, sodium lignin sulfonate and polyethylene glycol dimethane sulfonate are used as dispersants and protective agents, which can help the bioactive molecules to be uniformly dispersed in the solution while improving the compatibility of the bioactive molecules with diatomaceous earth, reducing the degradation and inactivation of the bioactive molecules in the subsequent processing process, and improving the efficacy stability and durability of the bioactive molecules; on the other hand, the addition of sodium lignin sulfonate and polyethylene glycol dimethane sulfonate can improve the hygroscopicity and air permeability of the fiber, enhance the mechanical strength and flexibility of the fiber, and improve the overall performance of the fiber.
[0026] 3. The present invention adopts adipic acid dihydrazide and sodium polyacrylate as grinding modifiers to grind and modify diatomaceous earth, which can change the surface properties of diatomaceous earth, increase its hydrophilicity and surface activity, improve the compatibility of diatomaceous earth with bioactive molecules, and enhance the adhesion of diatomaceous earth to fiber matrix; the bioactive molecules obtained by pretreatment are ultrasonically dispersed with the modified diatomaceous earth, and the modified diatomaceous earth is used to adsorb and protect the bioactive molecules, so that the bioactive molecules can better combine with the fiber matrix, thereby improving the comprehensive properties of the fiber such as antibacterial, anti-inflammatory, moisture absorption, and breathability.
[0027] 4. The preparation method of the present invention is simple, low-cost, and suitable for industrial production. The prepared ES large biofiber has excellent biological activity and mechanical properties, and the biological activity is long-lasting and suitable for a variety of application fields, such as medical textiles, sanitary products, personal care products, etc. DETAILED DESCRIPTION
[0028] The technical scheme of the present invention will be further described in detail below in conjunction with specific embodiments. It should be understood that the following embodiments are only exemplary descriptions and explanations of the present invention and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above content of the present invention are included in the scope that the present invention is intended to protect.
[0029] The raw materials used in the examples and comparative examples of the present invention are as follows:
[0030] Chamomile extract, brand Quanao Bio, product number: QAD-01274, purchased from Xi'an Anao Biotechnology Co., Ltd.;
[0031] Tea tree oil, brand Chengfeng, CAS number: 68647-73-4, content: 99%, purchased from Hubei Chengfeng Chemical Co., Ltd.;
[0032] Sodium lignin sulfonate, brand Nengju Chemical, CAS number: 8061-51-6, content: 99%, purchased from Shandong Nengju Chemical Co., Ltd.;
[0033] Polyethylene glycol dimethanesulfonate (MsO-PEG-OMs), brand: Jingpi Technology, CAS number: 52410-74-9, product number: JP0082, content: 99%, purchased from Beijing Jingpi Technology Co., Ltd.;
[0034] Calcined diatomite, brand Chenjin, particle size 325 mesh, purchased from Shijiazhuang Chenjin Mineral Products Co., Ltd.;
[0035] Sodium polyacrylate, brand Nengju Chemical, CAS number: 9003-04-7, content: 99%, purchased from Shandong Nengju Chemical Co., Ltd.;
[0036] Adipic acid dihydrazide, brand Nengju Chemical, CAS number: 1071-93-8, content: 99%, purchased from Shandong Nengju Chemical Co., Ltd.;
[0037] Polyethylene granules (linear low-density polyethylene LLDPE), brand: Sinopec, model: DFDA-7042, purchased from Dongguan Lusheng Plastic Chemical Co., Ltd.;
[0038] Polyester chips, brand China Resources, product name PET, model: CR-8863, purchased from Dongguan Lusheng Plastic Chemical Co., Ltd.
[0039] Examples 1-3 provide an ES large biofiber containing bioactive ingredients and a preparation method thereof, as follows:
[0040] Example 1
[0041] An ES large biological fiber containing biologically active ingredients is prepared by the following method:
[0042] S1. Preparation of biologically active ingredients:
[0043] S11, taking chamomile extract and tea tree oil as biologically active molecules in a mass ratio of 4:1 for later use;
[0044] S12, controlling the mass ratio of the bioactive molecule, sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and 55% ethanol solution to be 5:2:1:17, adding the bioactive molecule, sodium lignin sulfonate and polyethylene glycol dimethanesulfonate to 55% ethanol solution, controlling the stirring speed to be 300 rpm, the stirring temperature to be 45° C., stirring and mixing for 40 minutes until a uniform mixed solution is obtained;
[0045] S13, according to the mass ratio of 3:0.3, the calcined diatomite and the modifier (the modifier includes sodium polyacrylate and adipic acid dihydrazide in a mass ratio of 6.5:1) are mixed and ground for 1h, the grinding pressure is controlled to be 90kPa, the grinding speed is 55rpm, and deionized water (the mass of deionized water is 27 times the mass of the calcined diatomite) is added after grinding and modification, the ultrasonic power is controlled to be 320W, the ultrasonic frequency is 20kHz, and the ultrasonic pre-dispersion is performed for 20min to obtain a dispersion;
[0046] S14, controlling the mass ratio of the dispersion liquid to the mixed liquid to be 1.5:1, adding the dispersion liquid to the mixed liquid and continuing ultrasonic dispersion and mixing for 1 hour, and spray drying to obtain the bioactive component, wherein the spray pressure is 0.4 MPa, the feed rate is 10 mL / min, the inlet air temperature is 40°C, and the drying time is 40 min;
[0047] S2, mixing the bioactive component with polyethylene particles at a mass ratio of 1:10 to obtain a cortex material, and mixing the bioactive component with polyester chips at a mass ratio of 1:22 to obtain a core material;
[0048] S3. Using composite spinning equipment, the skin layer material and the core layer material are respectively fed into two groups of screw extruders in a mass ratio of 1:1 for melt extrusion. The obtained skin layer melt and core layer melt are compounded into filaments through a composite spinning assembly, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber, wherein the spinning box temperature is 250°C, the spinning speed is 1000m / min; the side blowing temperature is 18°C, the side blowing humidity is 80%, and the side blowing rate is 1.2m / s; the stretching multiple is 3.8 times, and the stretching temperature is 70°C.
[0049] Example 2
[0050] An ES large biological fiber containing biologically active ingredients is prepared by the following method:
[0051] S1. Preparation of biologically active ingredients:
[0052] S11, taking chamomile extract and tea tree oil as biologically active molecules at a mass ratio of 5.5:1 for later use;
[0053] S12, controlling the mass ratio of the bioactive molecule, sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and 55% ethanol solution to be 6:3:1:18, adding the bioactive molecule, sodium lignin sulfonate and polyethylene glycol dimethanesulfonate to 55% ethanol solution, controlling the stirring speed to be 400 rpm, the stirring temperature to be 55° C., stirring and mixing for 30 minutes until a uniform mixed solution is obtained;
[0054] S13, according to the mass ratio of 3:0.4, the calcined diatomite and the modifier (the modifier includes sodium polyacrylate and adipic acid dihydrazide in a mass ratio of 7.5:1) are mixed and ground for 1.5h, the grinding pressure is controlled to 80kPa, the grinding speed is 50rpm, and deionized water (the mass of deionized water is 28 times the mass of the calcined diatomite) is added after grinding and modification, the ultrasonic power is controlled to 350W, the ultrasonic frequency is 30kHz, and the ultrasonic pre-dispersion is performed for 15min to obtain a dispersion;
[0055] S14, controlling the mass ratio of the dispersion liquid to the mixed liquid to be 1.8:1, adding the dispersion liquid to the mixed liquid and continuing ultrasonic dispersion and mixing for 1.5 hours, and spray drying to obtain the bioactive component, wherein the spray pressure is 0.5 MPa, the feed rate is 12 mL / min, the inlet air temperature is 45° C., and the drying time is 35 min;
[0056] S2, mixing the bioactive component with polyethylene particles at a mass ratio of 1:12 to obtain a cortex material, and mixing the bioactive component with polyester chips at a mass ratio of 1:25 to obtain a core material;
[0057] S3. Using composite spinning equipment, the skin layer material and the core layer material are respectively fed into two groups of screw extruders in a mass ratio of 1:1.5 for melt extrusion. The obtained skin layer melt and core layer melt are compounded into filaments through a composite spinning assembly, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber, wherein the spinning box temperature is 260°C, the spinning speed is 1400m / min; the side blowing temperature is 20°C, the side blowing humidity is 85%, and the side blowing rate is 1.5m / s; the stretching multiple is 4.6 times, and the stretching temperature is 85°C.
[0058] Example 3
[0059] An ES large biological fiber containing biologically active ingredients is prepared by the following method:
[0060] S1. Preparation of biologically active ingredients:
[0061] S11, taking chamomile extract and tea tree oil as biologically active molecules in a mass ratio of 7:1 for later use;
[0062] S12, controlling the mass ratio of the bioactive molecule, sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and 55% ethanol solution to be 7:4:1:20, adding the bioactive molecule, sodium lignin sulfonate and polyethylene glycol dimethanesulfonate to 55% ethanol solution, controlling the stirring speed to be 500 rpm, the stirring temperature to be 65° C., stirring and mixing for 20 min until a uniform mixed solution is obtained;
[0063] S13, according to the mass ratio of 3:0.5, the calcined diatomite and the modifier (the modifier includes sodium polyacrylate and adipic acid dihydrazide in a mass ratio of 8.5:1) are mixed and ground for 2h, the grinding pressure is controlled to 70kPa, the grinding speed is 45rpm, and deionized water (the mass of deionized water is 30 times the mass of the calcined diatomite) is added after grinding and modification, the ultrasonic power is controlled to 380W, the ultrasonic frequency is 40kHz, and the ultrasonic pre-dispersion is performed for 10min to obtain a dispersion;
[0064] S14, controlling the mass ratio of the dispersion liquid to the mixed liquid to be 2:1, adding the dispersion liquid to the mixed liquid and continuing ultrasonic dispersion and mixing for 2 hours, and spray drying to obtain the bioactive component, wherein the spray pressure is 0.6 MPa, the feed rate is 15 mL / min, the inlet air temperature is 50° C., and the drying time is 30 min;
[0065] S2, mixing the bioactive component with polyethylene particles at a mass ratio of 1:15 to obtain a cortex material, and mixing the bioactive component with polyester chips at a mass ratio of 1:28 to obtain a core material;
[0066] S3. Using composite spinning equipment, the skin layer material and the core layer material are respectively fed into two groups of screw extruders in a mass ratio of 2:2.5 for melt extrusion. The obtained skin layer melt and core layer melt are compounded into filaments through a composite spinning assembly, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber, wherein the spinning box temperature is 270°C, the spinning speed is 1800m / min; the side blowing temperature is 22°C, the side blowing humidity is 90%, and the side blowing rate is 1.8m / s; the stretching multiple is 5.5 times, and the stretching temperature is 100°C.
[0067] In order to verify the comprehensive performance of the ES large biofiber containing bioactive ingredients provided by the present invention, the applicant set up comparative examples 1-4, wherein:
[0068] Comparative Example 1
[0069] An ES large biological fiber containing biologically active ingredients is prepared by the following method:
[0070] S1. Preparation of biologically active ingredients:
[0071] S11, taking chamomile extract and tea tree oil as biologically active molecules in a mass ratio of 4:1 for later use;
[0072] S12, controlling the mass ratio of the bioactive molecule, sodium lignin sulfonate and 55% ethanol solution to be 5:3:17, adding the bioactive molecule and sodium lignin sulfonate to 55% ethanol solution, controlling the stirring speed to be 300 rpm, the stirring temperature to be 45° C., stirring and mixing for 40 minutes until a uniform mixed solution is obtained;
[0073] S13, according to the mass ratio of 3:0.3, the calcined diatomite and the modifier (the modifier includes sodium polyacrylate and adipic acid dihydrazide in a mass ratio of 6.5:1) are mixed and ground for 1h, the grinding pressure is controlled to be 90kPa, the grinding speed is 55rpm, and deionized water (the mass of deionized water is 27 times the mass of the calcined diatomite) is added after grinding and modification, the ultrasonic power is controlled to be 320W, the ultrasonic frequency is 20kHz, and the ultrasonic pre-dispersion is performed for 20min to obtain a dispersion;
[0074] S14, controlling the mass ratio of the dispersion liquid to the mixed liquid to be 1.5:1, adding the dispersion liquid to the mixed liquid and continuing ultrasonic dispersion and mixing for 1 hour, and spray drying to obtain the bioactive component, wherein the spray pressure is 0.4 MPa, the feed rate is 10 mL / min, the inlet air temperature is 40°C, and the drying time is 40 min;
[0075] S2, mixing the bioactive component with polyethylene particles at a mass ratio of 1:10 to obtain a cortex material, and mixing the bioactive component with polyester chips at a mass ratio of 1:22 to obtain a core material;
[0076] S3. Using composite spinning equipment, the skin layer material and the core layer material are respectively fed into two groups of screw extruders in a mass ratio of 1:1 for melt extrusion. The obtained skin layer melt and core layer melt are compounded into filaments through a composite spinning assembly, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber, wherein the spinning box temperature is 250°C, the spinning speed is 1000m / min; the side blowing temperature is 18°C, the side blowing humidity is 80%, and the side blowing rate is 1.2m / s; the stretching multiple is 3.8 times, and the stretching temperature is 70°C.
[0077] Comparative Example 2
[0078] An ES large biological fiber containing biologically active ingredients is prepared by the following method:
[0079] S1. Preparation of biologically active ingredients:
[0080] S11, taking chamomile extract and tea tree oil as biologically active molecules in a mass ratio of 4:1 for later use;
[0081] S12, controlling the mass ratio of the bioactive molecule, polyethylene glycol dimethanesulfonate and 55% ethanol solution to be 5:3:17, adding the bioactive molecule and polyethylene glycol dimethanesulfonate to 55% ethanol solution, controlling the stirring speed to be 300 rpm, the stirring temperature to be 45° C., stirring and mixing for 40 minutes until a uniform mixed solution is obtained;
[0082] S13, according to the mass ratio of 3:0.3, the calcined diatomite and the modifier (the modifier includes sodium polyacrylate and adipic acid dihydrazide in a mass ratio of 6.5:1) are mixed and ground for 1h, the grinding pressure is controlled to be 90kPa, the grinding speed is 55rpm, and deionized water (the mass of deionized water is 27 times the mass of the calcined diatomite) is added after grinding and modification, the ultrasonic power is controlled to be 320W, the ultrasonic frequency is 20kHz, and the ultrasonic pre-dispersion is performed for 20min to obtain a dispersion;
[0083] S14, controlling the mass ratio of the dispersion liquid to the mixed liquid to be 1.5:1, adding the dispersion liquid to the mixed liquid and continuing ultrasonic dispersion and mixing for 1 hour, and spray drying to obtain the bioactive component, wherein the spray pressure is 0.4 MPa, the feed rate is 10 mL / min, the inlet air temperature is 40°C, and the drying time is 40 min;
[0084] S2, mixing the bioactive component with polyethylene particles at a mass ratio of 1:10 to obtain a cortex material, and mixing the bioactive component with polyester chips at a mass ratio of 1:22 to obtain a core material;
[0085] S3. Using composite spinning equipment, the skin layer material and the core layer material are respectively fed into two groups of screw extruders in a mass ratio of 1:1 for melt extrusion. The obtained skin layer melt and core layer melt are compounded into filaments through a composite spinning assembly, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber, wherein the spinning box temperature is 250°C, the spinning speed is 1000m / min; the side blowing temperature is 18°C, the side blowing humidity is 80%, and the side blowing rate is 1.2m / s; the stretching multiple is 3.8 times, and the stretching temperature is 70°C.
[0086] Comparative Example 3
[0087] An ES large biological fiber containing biologically active ingredients is prepared by the following method:
[0088] S1. Preparation of biologically active ingredients:
[0089] S11, taking chamomile extract and tea tree oil as biologically active molecules in a mass ratio of 4:1 for later use;
[0090] S12, controlling the mass ratio of the bioactive molecule, sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and 55% ethanol solution to be 5:2:1:17, adding the bioactive molecule, sodium lignin sulfonate and polyethylene glycol dimethanesulfonate to 55% ethanol solution, controlling the stirring speed to be 300 rpm, the stirring temperature to be 45° C., stirring and mixing for 40 minutes until a uniform mixed solution is obtained;
[0091] S13, according to the mass ratio of 3:0.3, the calcined diatomite and the modifier (the modifier is sodium polyacrylate) were mixed and ground for 1h, the grinding pressure was controlled to 90kPa, the grinding speed was 55rpm, and deionized water (the mass of deionized water was 27 times the mass of the calcined diatomite) was added after grinding and modification, the ultrasonic power was controlled to 320W, the ultrasonic frequency was 20kHz, and the ultrasonic pre-dispersion was performed for 20min to obtain a dispersion;
[0092] S14, controlling the mass ratio of the dispersion liquid to the mixed liquid to be 1.5:1, adding the dispersion liquid to the mixed liquid and continuing ultrasonic dispersion and mixing for 1 hour, and spray drying to obtain the bioactive component, wherein the spray pressure is 0.4 MPa, the feed rate is 10 mL / min, the inlet air temperature is 40°C, and the drying time is 40 min;
[0093] S2, mixing the bioactive component with polyethylene particles at a mass ratio of 1:10 to obtain a cortex material, and mixing the bioactive component with polyester chips at a mass ratio of 1:22 to obtain a core material;
[0094] S3. Using composite spinning equipment, the skin layer material and the core layer material are respectively fed into two groups of screw extruders in a mass ratio of 1:1 for melt extrusion. The obtained skin layer melt and core layer melt are compounded into filaments through a composite spinning assembly, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber, wherein the spinning box temperature is 250°C, the spinning speed is 1000m / min; the side blowing temperature is 18°C, the side blowing humidity is 80%, and the side blowing rate is 1.2m / s; the stretching multiple is 3.8 times, and the stretching temperature is 70°C.
[0095] Comparative Example 4
[0096] An ES large biological fiber containing biologically active ingredients is prepared by the following method:
[0097] S1. Preparation of biologically active ingredients:
[0098] S11, taking chamomile extract and tea tree oil as biologically active molecules in a mass ratio of 4:1 for later use;
[0099] S12, controlling the mass ratio of the bioactive molecule, sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and 55% ethanol solution to be 5:2:1:17, adding the bioactive molecule, sodium lignin sulfonate and polyethylene glycol dimethanesulfonate to 55% ethanol solution, controlling the stirring speed to be 300 rpm, the stirring temperature to be 45° C., stirring and mixing for 40 minutes until a uniform mixed solution is obtained;
[0100] S13, according to the mass ratio of 3:0.3, the calcined diatomite and the modifier (the modifier is adipic acid dihydrazide) were mixed and ground for 1h, the grinding pressure was controlled to 90kPa, the grinding speed was 55rpm, and deionized water (the mass of deionized water was 27 times the mass of the calcined diatomite) was added after grinding and modification, the ultrasonic power was controlled to 320W, the ultrasonic frequency was 20kHz, and the ultrasonic pre-dispersion was performed for 20min to obtain a dispersion;
[0101] S14, controlling the mass ratio of the dispersion liquid to the mixed liquid to be 1.5:1, adding the dispersion liquid to the mixed liquid and continuing ultrasonic dispersion and mixing for 1 hour, and spray drying to obtain the bioactive component, wherein the spray pressure is 0.4 MPa, the feed rate is 10 mL / min, the inlet air temperature is 40°C, and the drying time is 40 min;
[0102] S2, mixing the bioactive component with polyethylene particles at a mass ratio of 1:10 to obtain a cortex material, and mixing the bioactive component with polyester chips at a mass ratio of 1:22 to obtain a core material;
[0103] S3. Using composite spinning equipment, the skin layer material and the core layer material are respectively fed into two groups of screw extruders in a mass ratio of 1:1 for melt extrusion. The obtained skin layer melt and core layer melt are compounded into filaments through a composite spinning assembly, and then cooled and stretched by side blowing to obtain the required ES large bio-fiber, wherein the spinning box temperature is 250°C, the spinning speed is 1000m / min; the side blowing temperature is 18°C, the side blowing humidity is 80%, and the side blowing rate is 1.2m / s; the stretching multiple is 3.8 times, and the stretching temperature is 70°C.
[0104] Performance testing
[0105] The comprehensive properties of the ES large biological fibers in Examples 1-3 of the present invention and Comparative Examples 1-4 were tested respectively, as follows:
[0106] Tensile fracture performance: Tested in accordance with the provisions of standard GB / T14337-2008;
[0107] Antibacterial performance: Tested in accordance with the provisions of standard GB / T 20944.3-2008, test bacteria Escherichia coli (washing standard GB / T 8629-2001);
[0108] Water absorption performance: ES large biological fiber is woven into ES fabric according to the conventional method, and the fabric is cut into 3 small pieces, and its initial mass (M1) is recorded. It is put into a beaker filled with water and soaked in it for 1 hour. After taking it out, the water on the surface of the fabric is absorbed with filter paper until no water drops naturally drip. Its mass (M2) is weighed, and the water absorption rate is calculated. The average of the 3 results is taken, and the water absorption rate is calculated by the following formula: M = (M2-M1) / M1, where M is the water absorption rate, M1 is the dry weight of the fabric, and M2 is the weight of the fabric after water absorption;
[0109] Breathability: ES large biological fiber was woven into ES fabric according to conventional methods and tested with reference to the provisions of standard GB / T5453-1997. The test results are shown in Table 1 below.
[0110] Table 1:
[0111]
[0112] It can be seen from the data shown in Table 1 above that the comprehensive performance of the ES large biological fibers obtained in Examples 1-3 of the present invention is significantly better than that in Comparative Examples 1-4. The ES large biological fibers obtained in the present invention have excellent biological activity and mechanical properties, good moisture absorption and air permeability, and long-lasting antibacterial properties.
[0113] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, and these simple modifications all belong to the protection scope of the present invention. In addition, the various embodiments of the present invention can also be combined arbitrarily, as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.
Claims
1. A method for preparing ES large biofiber containing bioactive ingredients, characterized in that: The following steps are involved: S1. Preparation of biologically active ingredients: The bioactive molecules, sodium lignin sulfonate, and polyethylene glycol dimethanesulfonate are added to an ethanol solution and stirred evenly to obtain a mixed solution; the calcined diatomaceous earth is ground and modified, and then ultrasonically pre-dispersed with deionized water to obtain a dispersion solution; the dispersion solution is then added to the mixed solution and ultrasonically dispersed and mixed for 1-2 hours, and then spray-dried to obtain the dispersion solution; S2, mixing the bioactive component and the polyethylene particles evenly to obtain the cortex material, and mixing the bioactive component and the polyester slices evenly to obtain the core material; S3, using composite spinning equipment, feeding the skin layer material and the core layer material into two sets of screw extruders for melt extrusion, and the obtained skin layer melt and core layer melt are compounded into filaments through composite spinning components, and then cooled and stretched by side blowing to obtain the desired ES large bio-fiber; The bioactive molecules in step S1 include chamomile extract and tea tree oil in a mass ratio of 4-7:1; The grinding and modification of the calcined diatomite in step S1 specifically refers to: grinding the calcined diatomite and the modifier according to the mass ratio of 3:0.3-0.5 for 1-2 hours, controlling the grinding pressure to 70-90 kPa and the grinding speed to 45-55 rpm; The modifier comprises sodium polyacrylate and adipic acid dihydrazide in a mass ratio of 6.5-8.5:
1.
2. The method for preparing ES large biofiber containing bioactive ingredients according to claim 1, characterized in that: In the step S1, the mass ratio of the bioactive molecule, sodium lignin sulfonate, polyethylene glycol dimethanesulfonate and ethanol solution is 5-7:2-4:1:17-20.
3. The method for preparing ES large biofiber containing bioactive ingredients according to claim 1, characterized in that: In the step S1, the mass ratio of the calcined diatomite to the deionized water is 1:27-30; the mass ratio of the dispersion to the mixed solution is 1.5-2:
1.
4. The method for preparing ES large biofiber containing bioactive ingredients according to claim 1, characterized in that: In step S2, the mass ratio of the bioactive component to the polyethylene particles is 1:10-15; the mass ratio of the bioactive component to the polyester chips is 1:22-28.
5. The method for preparing ES large biofiber containing bioactive ingredients according to claim 1, characterized in that: In step S3, the mass ratio of the skin layer material to the core layer material is 1-2:1-2.
5.
6. The method for preparing ES large biofiber containing bioactive ingredients according to claim 1, characterized in that: In step S3, the spinning box temperature is 250-270°C, the spinning speed is 1000-1800m / min; the side blowing temperature is 18-22°C, the side blowing humidity is 80-90%, and the side blowing rate is 1.2-1.8m / s; the drafting multiple is 3.8-5.5 times, and the drafting temperature is 70-100°C.
7. An ES large biofiber containing biologically active ingredients, characterized in that: The ES large biological fiber containing biologically active ingredients is prepared by the preparation method of any one of claims 1-6.
Citation Information
Patent Citations
ES large biofibers containing active ingredients of dried orange peel, orange and pomelo and preparation method of ES large biofibers
CN112779627A
Contact cold sensory fiber, textile product, and method for producing the same
JP2002235278A