CN113622091A - Bi-component macrobiosis spun-bonded non-woven fabric containing plant active ingredients and preparation method thereof - Google Patents
Bi-component macrobiosis spun-bonded non-woven fabric containing plant active ingredients and preparation method thereof Download PDFInfo
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- CN113622091A CN113622091A CN202110876615.0A CN202110876615A CN113622091A CN 113622091 A CN113622091 A CN 113622091A CN 202110876615 A CN202110876615 A CN 202110876615A CN 113622091 A CN113622091 A CN 113622091A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/007—Addition polymers
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
- D01D5/23—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool by asymmetrical cooling of filaments, threads, or the like, leaving the spinnerettes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/32—Side-by-side structure; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
- D04H3/147—Composite yarns or filaments
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/13—Physical properties anti-allergenic or anti-bacterial
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- Nonwoven Fabrics (AREA)
Abstract
The invention provides a bi-component macrobiology spun-bonded non-woven fabric containing plant active ingredients and a preparation method thereof, relating to the technical field of macrobiology. The bicomponent macrobiosis spun-bonded non-woven fabric containing the plant active ingredients and the preparation method thereofComprises sol-gel method and calcination method to prepare mesoporous SiO2Nanoparticle, mesoporous SiO2The preparation method comprises the steps of preparing a molecular nest, preparing functional metallocene polypropylene slices containing the molecular nest, preparing functional HMSPP master batches containing the molecular nest, preparing a spun-bonded non-woven fabric containing plant active ingredients and the like. The invention utilizes mesoporous SiO2The nanometer molecular nest, the metallocene polypropylene slices and the HMSPP master batches are combined to be used as a base material, and the plant active ingredient-containing bi-component large-organism spun-bonded non-woven fabric which is good in mechanical property, durable in antibacterial property, soft and free of hair falling is obtained by combining the good antibacterial property of the plant active ingredient.
Description
Technical Field
The invention relates to the technical field of macrobiology, in particular to a preparation method of a bi-component macrobiology spun-bonded non-woven fabric containing plant active ingredients.
Background
For a long time, the physiological and pharmacological actions of tea have been widely noticed, and the records in "Ben Cao Shi Yi" that all the herbs are the herbs of all diseases and tea is the herb of all diseases "show that the health care effect of tea is well accepted since ancient times. The tea contains more than 2000 chemical components, wherein the total number of volatile compounds is about 500, and the functional components mainly comprise polyphenol, polysaccharide, amino acid, protein, alkaloid, vitamin, mineral matter and the like. Tea polyphenol is a general term for polyphenols contained in tea leaves, is considered to be an important substance component of tea leaves for health care, and is the first botanical drug approved by the Food and Drug Administration (FDA) for marketing. Researches show that the active components of the tea can destroy the structure of the bacterial wall membrane, interfere the growth and division of cells, block the synthesis and expression of functional proteins and polysaccharides, induce oxidative stress and other functions.
Orange is the fruit of the plant orange tree of the genus Citrus of the family Rutaceae, the small tree of the genus Citrus, the fruit can be peeled off to eat its pulp, and the pulp can be used as a seasoning or additive for other foods. The orange is rich in crude fiber, pectin, vitamins, flavonoid, plant essential oil and other bioactive substances, and has extremely high comprehensive utilization value.
The isatis root is a traditional Chinese medicine in China, is a dry root of Isatis tinctoria in cruciferae, is recorded in Shen nong Ben Cao Jing, is cold in nature and bitter in taste, and has the effects of clearing heat and removing toxicity, cooling blood and relieving swelling. The composition is widely used for resisting bacteria, viruses, platelet aggregation, endotoxin and the like in clinic, and can enhance the immune function of organisms. The active ingredients of the isatis root contain tryptanthrin and indole derivatives, and the isatis root has good inhibition effect on staphylococcus aureus, staphylococcus epidermidis, bacillus subtilis, sarcina, escherichia coli, typhoid bacillus, streptococcus A, pneumococcus, influenza bacillus and meningococcus. Meanwhile, the active ingredients of the isatis root also have good function of resisting bacterial endotoxin. In addition, the active component of the isatis root is also an important antiviral drug, wherein the active substances such as 4(3H) -quinazolone and the like have the effects of inhibiting infection and proliferation of Coxsackie B3 virus, hemorrhagic fever with renal syndrome virus, encephalitis B virus, mumps virus, herpes simplex virus, hepatitis B virus, influenza A virus and influenza virus.
The honeysuckle flower is the flower bud of Lonicera japonica Thunb, Lonicera confusa Thunb, Lonicera japonica Thunb and Lonicera fulvidraco of Caprifoliaceae, the active ingredients of the honeysuckle flower are mainly chlorogenic acid, isochlorogenic acid, ginkgolic acid, caffeic acid, isoluteolin, luteolin-7-glucoside, beta-sitosterol, stigmasterol, beta-sitosterol-D-G-glucoside, stigmasterol-D-glucoside and volatile oil, and the active ingredients have certain antibacterial effects on Staphylococcus aureus, Staphylococcus albus, hemolyticus, Streptococcus pneumoniae, meningococcus, Salmonella typhi, Salmonella paratyphi, Escherichia coli, Shigella dysenteriae, Proteus, Bordetella pertussis, Pseudomonas aeruginosa, Mycobacterium tuberculosis, cholerae and other gram-positive bacteria and gram-negative bacteria.
The mesoporous silica nanoparticle has unique excellent performances of large specific surface area, uniform and controllable particle size, good biocompatibility, easy functionalization and the like, and is widely used for constructing multifunctional drug carriers. Compared with traditional organic carriers such as micelle, liposome and the like, the mesoporous silica nanoparticle has better stability and larger loading capacity as an inorganic nano material.
Metallocene refers to an organometallic complex compound formed from a transition metal (e.g., zirconium, titanium, hafnium, etc.) and cyclopentadiene, and polypropylene synthesized using a metallocene catalyst is referred to as metallocene polypropylene. The metallocene polypropylene produced by the metallocene catalyst has the advantages of narrow relative molecular mass distribution, smaller microcrystal, excellent impact strength and toughness, good transparency, high glossiness, good radiation resistance and excellent insulating property, and can be well compatible with other various resins. In addition, many novel propylene copolymers such as propylene-styrene random copolymer, propylene-styrene block copolymer, propylene-long chain olefin copolymer, propylene-cycloolefin copolymer, propylene-diene copolymer and the like can be polymerized by the metallocene catalyst.
High Melt Strength (HMSPP) is a polypropylene (PP) material with high melt strength and melt elasticity. The HMSPP can show a certain strain hardening phenomenon during stretching in a molten state, has a wide processing temperature range, and can adapt to processing modes with high requirements on melt strength and strain hardening, such as thermal forming, extrusion foaming, coating, blow molding and the like. In addition, the product prepared from the HMSPP has the characteristics of excellent thermal stability and dimensional stability at high temperature, higher toughness and tensile strength, superior microwave adaptability, good environmental effect, easiness in recycling and the like. Meanwhile, due to the unique structural characteristics of HMSPP, the HMSPP has great advantages in the aspects of mechanical property, crystallization behavior, extensional viscosity and the like compared with the common PP. Furthermore, the melt strength of HMSPP is several times that of ordinary PP with similar flow characteristics; the yield strength, flexural modulus, and heat distortion temperature and melting point of HMSPP are higher than those of ordinary PP with similar melt flow rates in terms of density and melt flow rate.
The spun-bonded non-woven fabric is formed by extruding and stretching a polymer to form continuous filaments, laying the filaments into a web, and then carrying out self-bonding, thermal bonding, chemical bonding or mechanical reinforcement on the web to change the web into the non-woven fabric. The world spunbond nonwoven fabric technology mainly includes lecofier technology of lefen in germany, STP technology in italy, steel making technology in japan, and the like, and particularly, the lefen technology has become the mainstream technology in the world and has been developed into the fourth generation technology. At present, many enterprises are imitated in China, but the core technology of the enterprises is not solved or mastered, so that the domestic equipment manufacturing enterprises are waiting for time to achieve the technical level of the lefen. In order to solve the problems, the invention provides a preparation method of a bi-component macrobiotic spun-bonded non-woven fabric containing plant active ingredients, so that the obtained product has good mechanical properties and good antibacterial performance.
Disclosure of Invention
The invention provides a preparation method of a double-component macrobiosis spun-bonded non-woven fabric containing plant active ingredients, and the preparation method is characterized in that mesoporous SiO2The nano molecular nest, the metallocene polypropylene slices and the HMSPP master batches are combined to be used as a base material, so that the plant active ingredients are better coated, the activity and the antibacterial activity of the plant active ingredients are retained to the maximum extent, and meanwhile, the finished spun-bonded non-woven fabric still has good antibacterial performance after being used or placed for a long time. The preparation method of the bicomponent macrobiosis spun-bonded non-woven fabric containing the plant active ingredients comprises the following steps:
(1) extracting active ingredients of plants:
naturally drying the plant raw materials, removing impurities, crushing and sieving with a 80-mesh sieve to obtain plant raw material powder, accurately weighing 10-30g of the plant raw material powder in a 500mL triangular flask with a plug, adding 200-mL absolute ethyl alcohol, carrying out ultrasonic extraction for 30-60min under the conditions that the temperature is 50-60 ℃ and the power is 100-200W, filtering after extraction is finished, concentrating the filtrate under reduced pressure, and drying to obtain plant active ingredient powder with the powder granularity of 100-200 meshes;
(2) preparation of mesoporous SiO by sol-gel method and calcination method2Nano-particles:
dissolving 2.5g P123 in 100mL hydrochloric acid solution with the concentration of 1.5mol/L, and stirring for 3h in a water bath kettle at 50 ℃ to ensure that the mixture is uniform, clear and transparent; adding 0.5g CTAB, keeping the temperature constant, dropwise adding 5.8mL of Tetraethoxysilane (TEOS) into the solution, gradually rendering the solution white turbid, and continuously stirring for reaction for 20 hours; then adding 0.03g of ammonium fluoride, continuing stirring for 2h, and putting the obtained white turbid liquid into a high-pressure kettle to age for 24h at the temperature of 120 ℃; centrifuging the product, collecting the obtained white solid, drying the white solid in a drying oven at 50 ℃, and calcining the white powder in a muffle furnace at 600 ℃ 6h, grinding the product to obtain the material with the particle size of 100-200nm, the pore diameter of 3-7nm and the specific surface area of 750-820m2(g) mesoporous SiO2A nanoparticle;
(3) mesoporous SiO2Preparation of molecular nest:
respectively mixing 20-50g of plant active ingredient powder and 8-20g of mesoporous SiO2Sequentially adding the nano powder and 0.005-0.05g of dispersing agent into 500mL of deionized water, shearing and dispersing by using a magnetic stirrer under the condition of 100 plus materials and 300r/min to obtain nano composite dispersion liquid containing the plant active ingredients, and volatilizing the solvent of the dispersion liquid to obtain mesoporous SiO with the granularity of 8000 plus materials and 10000 meshes containing the plant active ingredients2Grinding and crushing the molecular nest for later use;
calculating to obtain 65-73% molecular nest carrier prepared in step (3);
the calculation formula of the load amount (D) is as follows:
in the formula: m isaRepresents the mass of the bioactive ingredient in the supernatant, g; m isbRepresenting the mass of the bioactive ingredient in the input system, g; m isdlRepresents the mass of the molecular nest, g;
(4) preparation of the functional metallocene polypropylene chip containing the molecular nest:
respectively vacuum-drying the molecular nest prepared in the step (3) and the metallocene polypropylene slices for 24 hours at the temperature of 120 ℃, then adding the dispersing agent, the antioxidant and the softening agent which have the same dosage as that of the step (3) into a double-screw extruder according to the weight ratio of the molecular nest to the metallocene polypropylene slices of 1:99-199 to carry out mixing granulation, and obtaining the product with Melt Flow Index (MFI) of 15-1800g/10min and relative molecular mass of (8-10) multiplied by 104The functional metallocene polypropylene master batch containing the molecular nest;
(5) preparing a functional HMSPP master batch containing a molecular nest:
respectively vacuum-drying the molecular nest prepared in the step (3) and the HMSPP slices at 120 ℃ for 24h, and then performing molecular dryingThe dispersant, the antioxidant, the softening agent and the degradation agent with the same amount as the dispersant, the antioxidant, the softening agent and the degradation agent in the step (3) are added into a double-screw extruder together for mixing and granulation, wherein the weight ratio of the nest to the HMSPP slices is 1:99-199, the Melt Flow Index (MFI) is 15-40g/10min, and the relative molecular mass is (8-10) multiplied by 104The functional HMSPP master batch containing the molecular nest;
(6) preparation of spunbonded nonwoven containing plant active ingredients:
respectively carrying out vacuum drying on the prepared functional metallocene polypropylene master batch containing the molecular nest and the prepared functional HMSPP master batch containing the molecular nest for 24 hours at 120 ℃; respectively adding the dried functional master batch into two double-screw extruders according to the weight ratio of the functional metallocene polypropylene master batch containing the molecular nest to the functional HMSPP master batch containing the molecular nest being 1:2-3, sequentially adding a dispersing agent, an antioxidant, a softening agent and a flame retardant, heating, melting and mixing, and controlling the temperature difference of two melts to be 10-20 ℃; and (3) entering a spinning box, laying the filaments into a net after filtering, spinning, cooling and air-flow drawing and stretching, and carrying out hot rolling and bonding on the fiber net by an upper press roll, a lower press roll and a rolling mill to form the spunbonded non-woven fabric, so as to obtain the spunbonded non-woven fabric containing the plant active ingredients.
Further, the plant raw material in the step (1) is one or more of tea, orange, isatis root and honeysuckle.
Further, the dispersant in the step (3), the step (4) and the step (5) is one or more of XD-5040, BYK-111, ECO-2500 and DH-5038.
Further, the softening agent in the step (4), the step (5) and the step (6) is one or more of an organic silicon softening agent, sodium octadecyl succinate sulfonate, polyoxyethylene ester, pentaerythritol, sorbitan fatty ester, a tertiary amine softening agent or a quaternary ammonium salt softening agent.
Further, the addition amounts of the dispersing agent, the antioxidant and the softening agent in the step (4), the step (5) and the step (6) are respectively 0.1-1% of the total mass of the mixture.
Further, the antioxidant in the step (5) and the step (6) is one or more of AN antioxidant 1098, AN antioxidant KB-6 and AN antioxidant JADEWIN AN B215.
Further, the degradation agent in the step (5) is organic peroxide, and the addition amount of the degradation agent is 0.1-1% of the total mass of the mixture.
Further, the dispersant in the step (6) is one or more of PT-200E, triethylhexyl phosphoric acid, F-604, sodium dodecyl sulfate and fatty acid polyglycol ester, and the addition amount is 0.1-0.4% of the total mass of the mixture.
Further, the flame retardant in the step (6) is one or more of a magnesium hydroxide flame retardant, an antimony trioxide flame retardant, a zinc borate flame retardant or an aluminum hydroxide flame retardant, and the adding amount of the flame retardant is 0.1-1% of the total mass of the mixture.
Compared with the prior art, the invention has the beneficial technical effects that:
the invention utilizes mesoporous SiO2The nano molecular nest, the metallocene polypropylene slices and the HMSPP master batches are combined to be used as a base material, so that the plant active ingredients are better coated, the activity and the antibacterial activity of the plant active ingredients are retained to the maximum extent, and meanwhile, the finished spun-bonded non-woven fabric still has good antibacterial performance after being used or placed for a long time. Meanwhile, in the preparation process of the bi-component macrobiology spun-bonded non-woven fabric containing the plant active ingredients, due to the fact that the thermal shrinkage temperatures of the two components are different, the two components shrink successively when spun fibers are cooled by air, the bi-component fibers are distributed in parallel and highly spirally curled, and then the manufactured non-woven fabric is soft and does not lose hair.
Detailed Description
The preparation method of the bicomponent macrobiosis spun-bonded nonwoven fabric containing plant active ingredients provided by the invention is further explained by combining the following examples.
Example 1
The preparation method of the bicomponent macrobiotic spun-bonded non-woven fabric containing the plant active ingredients comprises the following steps:
(1) extracting active ingredients of plants:
naturally drying fresh tea and radix isatidis, removing impurities, crushing, sieving with a 80-mesh sieve to obtain mixed powder, accurately weighing 10g of the mixed powder in a 500mL triangular flask with a plug, adding 200mL of absolute ethyl alcohol, carrying out ultrasonic extraction for 30min under the conditions that the temperature is 50 ℃ and the power is 100W, filtering after extraction is finished, concentrating the filtrate under reduced pressure, and drying to obtain plant active ingredient powder with the powder granularity of 100 meshes;
(2) preparation of mesoporous SiO by sol-gel method and calcination method2Nano-particles:
dissolving 2.5g P123 in 100mL hydrochloric acid solution with the concentration of 1.5mol/L, and stirring for 3h in a water bath kettle at 50 ℃ to ensure that the mixture is uniform, clear and transparent; adding 0.5g CTAB, keeping the temperature constant, dropwise adding 5.8mL TEOS into the solution, gradually rendering the solution white turbid, and continuously stirring for reaction for 20 h; then adding 0.03g of ammonium fluoride, continuing stirring for 2h, and putting the obtained white turbid liquid into a high-pressure kettle to age for 24h at the temperature of 120 ℃; centrifugally collecting the product to obtain a white solid, then placing the white solid into a drying oven to be dried at 50 ℃, finally placing white powder into a muffle furnace to be calcined at 600 ℃ for 6h, and grinding the product to obtain mesoporous SiO with the particle size of 100nm, the pore diameter of 7nm and the specific surface area of 750-820m2/g2A nanoparticle;
(3) mesoporous SiO2Preparation of molecular nest:
respectively mixing 20g of plant active ingredient powder and 8g of mesoporous SiO2Sequentially adding the nano powder and 0.005g of dispersing agent into 500mL of deionized water, shearing and dispersing by using a magnetic stirrer at the speed of 100r/min to obtain a nano composite dispersion liquid containing the plant active ingredient, volatilizing a solvent of the dispersion liquid to obtain mesoporous SiO containing the plant active ingredient with the granularity of 8000 meshes and the carrier content of 68 percent2Grinding and crushing the molecular nest for later use;
the dispersant was composed of 0.0025XD-5040 and 0.0025g BYK-111;
(4) preparation of the functional metallocene polypropylene chip containing the molecular nest:
respectively vacuum-drying the molecular nest prepared in the step (3) and the metallocene polypropylene slices at 120 ℃ for 24h, and then adding the molecular nest and the metallocene polypropylene slices together with a dispersant, an antioxidant and a softener according to the weight ratio of 1:99 of the molecular nest to the metallocene polypropylene slicesMixing and granulating in a screw extruder to obtain a Melt Flow Index (MFI) of 955g/10min and a relative molecular mass of 10 multiplied by 104The functional metallocene polypropylene master batch containing the molecular nest;
the dispersing agent is composed of XD-5040 and BYK-111 according to the mass ratio of 1: 1;
the antioxidant is composed of 1098 and an antioxidant KB-6 in a mass ratio of 1: 1;
the softening agent is composed of sodium octadecyl sulfosuccinate and polyoxyethylene ester according to the mass ratio of 1: 1;
the addition amounts of the dispersing agent, the antioxidant and the softening agent are respectively 0.1 percent of the total mass of the mixture;
(5) preparing a functional HMSPP master batch containing a molecular nest:
respectively vacuum-drying the molecular nest and the HMSPP slices prepared in the step (3) for 24 hours at the temperature of 120 ℃, then adding the molecular nest and the HMSPP slices together with a dispersing agent, an antioxidant, a softening agent and a degrading agent into a double-screw extruder according to the weight ratio of 1:99, mixing and granulating to obtain the product with the Melt Flow Index (MFI) of 35g/10min and the relative molecular mass of (8-10) multiplied by 104Functional HMSPP master batch containing molecular nests;
the dispersant is XD-5040 and BYK-111 according to the mass ratio of 1: 1;
the antioxidant is composed of 1098 and an antioxidant KB-6 in a mass ratio of 1: 1;
the softening agent is composed of sodium octadecyl sulfosuccinate and polyoxyethylene ester according to the mass ratio of 1: 1;
the degradation agent is disuccinic acid peroxide;
the addition amounts of the dispersing agent, the antioxidant, the softening agent and the degrading agent are respectively 0.1 percent of the total mass of the mixture;
(6) preparation of spunbonded nonwoven containing plant active ingredients:
respectively carrying out vacuum drying on the prepared functional metallocene polypropylene master batch containing the molecular nest and the prepared functional HMSPP master batch containing the molecular nest for 24 hours at 120 ℃; respectively adding the dried functional master batch into two double-screw extruders according to the weight ratio of 1:2 of the functional metallocene polypropylene master batch containing the molecular nest to the functional HMSPP master batch containing the molecular nest, sequentially adding a dispersing agent, an antioxidant, a softening agent and a flame retardant, heating, melting and mixing, and controlling the temperature difference of two melts to be 10 ℃; entering a spinning box, laying the filaments into a net after filtering, spinning, cooling and air-flow drawing and stretching, and carrying out hot rolling and bonding on the fiber net by an upper compression roller, a lower compression roller and a rolling mill to form a spun-bonded non-woven fabric so as to obtain the spun-bonded non-woven fabric containing plant active ingredients;
the dispersing agent is composed of PT-200E and triethyl hexyl phosphoric acid according to the mass ratio of 1: 1;
the antioxidant is composed of 1098 and an antioxidant KB-6 in a mass ratio of 1: 1;
the softening agent is composed of sodium octadecyl sulfosuccinate and polyoxyethylene ester according to the mass ratio of 1: 1;
the flame retardant consists of a magnesium hydroxide flame retardant and an antimony trioxide flame retardant in a mass ratio of 1: 1;
the addition amounts of the dispersing agent, the antioxidant, the softening agent and the flame retardant are respectively 0.1 percent of the total mass of the mixture.
Example 2
The preparation method of the bicomponent macrobiotic spun-bonded non-woven fabric containing the plant active ingredients comprises the following steps:
(1) extracting active ingredients of plants:
naturally drying fresh radix isatidis and honeysuckle, removing impurities, crushing, sieving with a 80-mesh sieve to obtain plant raw material powder, accurately weighing 30g of the plant raw material powder in a 500mL triangular flask with a plug, adding 300mL of absolute ethyl alcohol, carrying out ultrasonic extraction for 60min under the conditions that the temperature is 60 ℃ and the power is 200W, filtering after extraction is finished, concentrating the filtrate under reduced pressure, and drying to obtain plant active ingredient powder with the powder granularity of 200 meshes;
(2) preparation of mesoporous SiO by sol-gel method and calcination method2Nano-particles:
dissolving 2.5g P123 in 100mL hydrochloric acid solution with the concentration of 1.5mol/L, and stirring for 3h in a water bath kettle at 50 ℃ to ensure that the mixture is uniform, clear and transparent; adding 0.5g CTAB, maintainingGradually adding 5.8mL of TEOS into the solution dropwise at constant temperature, gradually rendering the solution white turbid, and continuously stirring for reaction for 20 h; then adding 0.03g of ammonium fluoride, continuing stirring for 2h, and putting the obtained white turbid liquid into a high-pressure kettle to age for 24h at the temperature of 120 ℃; centrifugally collecting the product to obtain a white solid, then placing the white solid into a drying oven to be dried at 50 ℃, finally placing white powder into a muffle furnace to be calcined at 600 ℃ for 6h, and grinding the product to obtain mesoporous SiO with the particle size of 200nm, the pore diameter of 3nm and the specific surface area of 750-820m2/g2A nanoparticle;
(3) mesoporous SiO2Preparation of molecular nest:
respectively mixing 50g of plant active ingredient powder and 8-20g of mesoporous SiO2Sequentially adding the nano powder and 0.05g of dispersing agent into 500mL of deionized water, shearing and dispersing by using a magnetic stirrer at 300r/min to obtain a nano composite dispersion liquid containing the plant active ingredient, and volatilizing a solvent to obtain 73% mesoporous SiO containing the plant active ingredient with the granularity of 10000 meshes and the carrier amount of 73%2Grinding and crushing the molecular nest for later use;
the dispersant is composed of XD-5040 and DH-5038 according to the mass ratio of 1:1,
(4) preparation of the functional metallocene polypropylene chip containing the molecular nest:
respectively carrying out vacuum drying on the molecular nest prepared in the step (3) and the metallocene polypropylene slices for 24 hours at the temperature of 120 ℃, then adding the dispersing agent, the antioxidant and the softening agent which have the same amount as that of the dispersant, the antioxidant and the softening agent in the step (3) into a double-screw extruder according to the weight ratio of the molecular nest to the metallocene polypropylene slices of 1:199 for mixing and granulation to obtain the product with Melt Flow Index (MFI) of 1200g/10min and relative molecular mass of 8 multiplied by 104The functional metallocene polypropylene master batch containing the molecular nest;
the dispersant is composed of XD-5040 and DH-5038 according to the mass ratio of 1: 1;
the antioxidant consists of KB-6 and AN antioxidant JADEWIN AN B215 in a mass ratio of 1: 1;
the softening agent is composed of polyoxyethylene ester and pentaerythritol in a mass ratio of 1: 1;
the addition amounts of the dispersing agent, the antioxidant and the softening agent are respectively 0.5 percent of the total mass of the mixture;
(5) preparing a functional HMSPP master batch containing a molecular nest:
respectively carrying out vacuum drying on the molecular nest prepared in the step (3) and the HMSPP slices at 120 ℃ for 24h, then adding the dispersing agent, the antioxidant, the softening agent and the degrading agent which are used in the same amount as the step (3) into a double-screw extruder according to the weight ratio of the molecular nest to the HMSPP slices of 1:199 to carry out mixing granulation, and obtaining the product with Melt Flow Index (MFI) of 40g/10min and relative molecular mass of 10 multiplied by 104The functional HMSPP master batch containing the molecular nest;
the dispersant is composed of XD-5040 and DH-5038 according to the mass ratio of 1: 1;
the antioxidant consists of KB-6 and AN antioxidant JADEWIN AN B215 in a mass ratio of 1: 1;
the softening agent is composed of polyoxyethylene ester and pentaerythritol in a mass ratio of 1: 1;
the degradation agent is acetylacetone peroxide;
the addition amounts of the dispersing agent, the antioxidant, the softening agent and the degrading agent are respectively 0.5 percent of the total mass of the mixture;
(6) preparation of spunbonded nonwoven containing plant active ingredients:
respectively carrying out vacuum drying on the prepared functional metallocene polypropylene master batch containing the molecular nest and the prepared functional HMSPP master batch containing the molecular nest for 24 hours at 120 ℃; respectively adding the dried functional master batch into two double-screw extruders according to the weight ratio of 1:3 of the functional metallocene polypropylene master batch containing the molecular nest to the functional HMSPP master batch containing the molecular nest, sequentially adding a dispersing agent, an antioxidant, a softening agent and a flame retardant, heating, melting and mixing, and controlling the temperature difference of two melts to be 20 ℃; entering a spinning box, laying the filaments into a net after filtering, spinning, cooling and air-flow drawing and stretching, and carrying out hot rolling and bonding on the fiber net by an upper compression roller, a lower compression roller and a rolling mill to form a spun-bonded non-woven fabric so as to obtain the spun-bonded non-woven fabric containing plant active ingredients;
the dispersing agent is composed of triethyl hexyl phosphoric acid and fatty acid polyglycol ester according to the mass ratio of 1: 1;
the antioxidant consists of KB-6 and AN antioxidant JADEWIN AN B215 in a mass ratio of 1: 1;
the softening agent is composed of polyoxyethylene ester and pentaerythritol in a mass ratio of 1: 1;
the flame retardant is an aluminum hydroxide flame retardant, and the addition amount of the flame retardant is 0.2 percent of the total mass of the mixture;
the addition amounts of the dispersing agent, the antioxidant and the softening agent are respectively 0.3 percent of the total mass of the mixture.
Comparative example 1
The difference from example 2 is that no plant active ingredient is added.
Comparative example 2
The difference from example 2 is that no molecular nest is used.
Comparative example 3
The difference is that the HMSPP master batch containing the molecular nest is not added in the same way as the example 2.
Comparative example 4
The difference from example 2 is that no functional metallocene polypropylene chips containing molecular nests were added.
Test example 1
The antibacterial properties of the products obtained in examples 1-2 and comparative examples 1-4 of the present invention were tested according to the method specified in GB/T20944.3-2008 "evaluation of antibacterial properties of textiles", and the results are as follows:
the products obtained in examples 1-2 and comparative examples 1-4 were washed with clean water at 25 ℃ for 30 times, 50 times and 70 times, respectively, and then the antibacterial property of the products was tested according to the method specified in GB/T20944.3-2008 "evaluation of antibacterial property of textiles", and the results were as follows:
the principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (9)
1. The preparation method of the bicomponent macrobiotic spun-bonded non-woven fabric containing the plant active ingredients is characterized by comprising the following steps:
(1) extracting active ingredients of plants:
naturally drying the plant raw materials, removing impurities, crushing and sieving with a 80-mesh sieve to obtain plant raw material powder, accurately weighing 10-30g of the plant raw material powder in a 500mL triangular flask with a plug, adding 200-mL absolute ethyl alcohol, carrying out ultrasonic extraction for 30-60min under the conditions that the temperature is 50-60 ℃ and the power is 100-200W, filtering after extraction is finished, concentrating the filtrate under reduced pressure, and drying to obtain plant active ingredient powder with the powder granularity of 100-200 meshes;
(2) preparation of mesoporous SiO by sol-gel method and calcination method2Nano-particles:
dissolving 2.5g P123 in 100mL hydrochloric acid solution with the concentration of 1.5mol/L, and stirring for 3h in a water bath kettle at 50 ℃ to ensure that the mixture is uniform, clear and transparent; adding 0.5g CTAB, keeping the temperature constant, dropwise adding 5.8mL TEOS into the solution, gradually rendering the solution white turbid, and continuously stirring for reaction for 20 h; then adding 0.03g of ammonium fluoride, continuing stirring for 2h, and putting the obtained white turbid liquid into a high-pressure kettle to age for 24h at the temperature of 120 ℃; centrifuging the product, collecting the obtained white solid, drying the white solid in a drying oven at 50 deg.C, calcining the white powder in a muffle furnace at 600 deg.C for 6 hr, and dryingThe product is ground to obtain the material with the particle size of 100-200nm, the pore diameter of 3-7nm and the specific surface area of 750-820m2(g) mesoporous SiO2A nanoparticle;
(3) mesoporous SiO2Preparation of molecular nest:
respectively mixing 20-50g of plant active ingredient powder and 8-20g of mesoporous SiO2Sequentially adding the nano powder and 0.005-0.05g of dispersing agent into 500mL of deionized water, shearing and dispersing by using a magnetic stirrer under the condition of 100 plus materials and 300r/min to obtain nano composite dispersion liquid containing the plant active ingredients, volatilizing the solvent of the dispersion liquid to obtain mesoporous SiO with the granularity of 8000 plus materials and 10000 meshes and the carrier content of 65-73 percent2Grinding and crushing the molecular nest for later use;
(4) preparation of the functional metallocene polypropylene chip containing the molecular nest:
respectively vacuum-drying the molecular nest prepared in the step (3) and the metallocene polypropylene slices for 24 hours at the temperature of 120 ℃, then adding the dispersing agent, the antioxidant and the softening agent which have the same dosage as that of the step (3) into a double-screw extruder according to the weight ratio of the molecular nest to the metallocene polypropylene slices of 1:99-199 for mixing and granulation to obtain the product with the Melt Flow Index (MFI) of 15-1800g/10min and the relative molecular mass of (8-10) multiplied by 104The functional metallocene polypropylene master batch containing the molecular nest;
(5) preparing a functional HMSPP master batch containing a molecular nest:
respectively vacuum-drying the molecular nest and the HMSPP slices prepared in the step (3) for 24 hours at 120 ℃, then adding the dispersing agent, the antioxidant, the softening agent and the degrading agent which are used in the same amount as the step (3) into a double-screw extruder according to the weight ratio of the molecular nest to the HMSPP slices of 1:99-199 to be mixed and granulated, and obtaining the Melt Flow Index (MFI) of 15-40g/10min and the relative molecular mass of (8-10) multiplied by 104The functional HMSPP master batch containing the molecular nest;
(6) preparation of spunbonded nonwoven containing plant active ingredients:
respectively carrying out vacuum drying on the prepared functional metallocene polypropylene master batch containing the molecular nest and the prepared functional HMSPP master batch containing the molecular nest for 24 hours at 120 ℃; respectively adding the dried functional master batch into two double-screw extruders according to the weight ratio of the functional metallocene polypropylene master batch containing the molecular nest to the functional HMSPP master batch containing the molecular nest being 1:2-3, sequentially adding a dispersing agent, an antioxidant, a softening agent and a flame retardant, heating, melting and mixing, and controlling the temperature difference of two melts to be 10-20 ℃; and (3) entering a spinning box, laying the filaments into a net after filtering, spinning, cooling and air-flow drawing and stretching, and carrying out hot rolling and bonding on the fiber net by an upper press roll, a lower press roll and a rolling mill to form the spunbonded non-woven fabric, so as to obtain the spunbonded non-woven fabric containing the plant active ingredients.
2. The method for preparing the bicomponent biont spunbonded nonwoven fabric containing the plant active ingredients as claimed in claim 1, wherein the plant raw material in the step (1) is one or more of tea, orange, isatis root and honeysuckle flower.
3. The method for preparing the bicomponent macrobiosis spunbond nonwoven fabric containing the plant active ingredient as claimed in claim 1, wherein the dispersing agent in the step (3), the step (4) and the step (5) is one or more of XD-5040, BYK-111, ECO-2500 and DH-5038.
4. The method for preparing the two-component macrobiotic spunbonded nonwoven fabric containing plant active ingredients as claimed in claim 1, wherein the softener in the steps (4), (5) and (6) is one or more of silicone softener, sodium stearyl sulfosuccinate, polyoxyethylene ester, pentaerythritol, sorbitan fatty ester, tertiary amine softener or quaternary ammonium salt softener.
5. The method for preparing the plant active ingredient-containing bicomponent macrobiosis spunbond non-woven fabric as claimed in claim 1, wherein the addition amounts of the dispersing agent, the antioxidant and the softening agent in the step (4), the step (5) and the step (6) are respectively 0.1-1% of the total mass of the mixture.
6. The method for preparing the bi-component large biological spunbonded nonwoven fabric containing the plant active ingredients as claimed in claim 1, wherein the antioxidant in the step (5) and the step (6) is one or more of antioxidant 1098, antioxidant KB-6 and antioxidant JADEWIN AN B215.
7. The method for preparing the plant active ingredient-containing bicomponent macrobiosis spunbond nonwoven fabric as claimed in claim 1, wherein the degradation agent in the step (5) is organic peroxide, and the addition amount is 0.1-1% of the total mass of the mixture.
8. The method for preparing the bicomponent macrobiosis spunbond non-woven fabric containing the plant active ingredient as claimed in claim 1, wherein the dispersant in the step (6) is one or more of PT-200E, triethylhexylphosphoric acid, F-604, sodium dodecyl sulfate and fatty acid polyglycol ester, and the addition amount is 0.1-0.4% of the total mass of the mixture.
9. The method for preparing the plant active ingredient-containing bicomponent biolobical spun-bonded nonwoven fabric according to claim 1, wherein the flame retardant in the step (6) is one or more of a magnesium hydroxide flame retardant, an antimony trioxide flame retardant, a zinc borate flame retardant and an aluminum hydroxide flame retardant, and the addition amount is 0.1-1% of the total mass of the mixture.
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