CN106192057A - A kind of Multifunctional polyester fiber containing sea mud and preparation method thereof - Google Patents

A kind of Multifunctional polyester fiber containing sea mud and preparation method thereof Download PDF

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CN106192057A
CN106192057A CN201610493452.7A CN201610493452A CN106192057A CN 106192057 A CN106192057 A CN 106192057A CN 201610493452 A CN201610493452 A CN 201610493452A CN 106192057 A CN106192057 A CN 106192057A
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sea mud
extract
powder
mud
aromaticae
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陆建益
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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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • 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
    • D01D5/08—Melt spinning methods
    • 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
    • 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
    • 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
    • D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention provides a kind of Multifunctional polyester fiber containing sea mud and preparation method thereof, the composition of raw materials of this fiber is by weight percentage: polyester slice 70～95%, sea mud powder 2～18%, Fructus Staphyleae Bumaldae seed extract 0.3～2%, Herba Blumeae Aromaticae extract 1～3.5%, arrow root grass extract 1.6～5%, coupling agent 0.1～1.5%.Above-mentioned each raw material is processed by number of ways, is blended, melt spinning method routinely, send into apparatus for melt spinning and carry out co-blended spinning, i.e. obtain the Multifunctional polyester fiber containing sea mud, give off a strong fragrance, skin-friendly is good, both given and there is antibacterial and deodorizing, anti-ultraviolet, acaricide anophelifuge, functions of skin protection and health care, and effective, persistent simultaneously, shown again preferable spinnability, hygroscopicity, breathability, dyeing uniformity and mechanical property, wearability is excellent, wide application.Therefore, sea mud resource is fully used, and has the highest economic worth and the value of environmental protection.

Description

A kind of Multifunctional polyester fiber containing sea mud and preparation method thereof
Technical field
The present invention relates to a kind of Multifunctional polyester fiber containing sea mud and preparation method thereof, belong to Functional Chemical Fibers technology Field.
Background technology
Polyester fiber by the polyester of organic dibasic acid and dihydroxylic alcohols polycondensation through the synthetic fibers of spinning gained.Trade name For terylene, it is called for short PET, is the first big kind of current synthetic fibers.It had both had intensity height, good springiness, heat-resisting, acidproof Alkalescence is good, dimensional stability is high, can pure spin again, also can be with the natural fiber such as cotton, hair, silk, fiber crops and other chemical fibres with arbitrarily The excellent properties such as ratio blending, are heavily used in manufacture clothing, underwear, socks, gym suit, bedding, sanitary dressings etc. Textile.But, polyester fiber there is also that hygroscopicity is poor, antibiotic property is low, uvioresistant performance is strong not, be easily generated electrostatic, be difficult to The deficiencies such as dyeing.People can be infected with in the skin secretions such as many perspiration and environment during wearing or using its textile Dirt, grows various antibacterial and pathogenic bacteria, makes polyster fibre also easily acid by it or alkali while spreading disease by all means Property the effect of metabolite and occur molecular chain degradation, variable color, strength to decline, shorten service life, and it is undesirable smelly to volatilize Taste, the most easily breeds acarid, also can attract mosquito bite.Particularly excess ultraviolet irradiate, make human body skin occur erythema, Dermatitis, pigmentation, accelerate skin aging, pathological changes equivalent risk of burning, serious threat human health even occur.Meanwhile, Substantially shortcoming is there is also in terms of supplementary skin-nourishing, enhancing Skin Cell vigor, anti-ageing skin protection health protection of waiting for a long time.
Breathe freely and skin-protection and health-care about antibacterial and deodorizing, anti-ultraviolet, fragrance, acaricide anophelifuge, moisture absorption although the most many Appear in the newspapers repeatly Deng the research of functional polyalkylene ester fiber, but be mostly based on simple function, there is two or more function Composite polyester fiber is less, can not meet far away people's demand to polyester fiber one-object-many-purposes, at high-performance difference chemical fibre The field of dimension loses competitive advantage.Sea mud is the clay that Coastal beach alluvial is got up, and belongs to secondary clay.China is that coastline is the longest Country, deposited millions of sea mud at Coastal beach, be inexhaustible, back and forth feed, yield your pupil, the most fully Utilize, not only waste resource, also pollute environment.Result of study in recent years shows, sea mud have uniqueness cavernous structure, The characteristics such as specific surface area is big, high adsorption capacity, rich in vitamin A, vitamin C, vitamin E, aminoacid, antibiotics, calcium carbonate And the mineral element such as ferrum, magnesium, zinc, selenium, germanium, simultaneously possibly together with animals and plants remains such as algae class, pasture and water and shell-fish, through too much Year alluvial has formed the organic substances such as the reactive protein to skin beneficiating and polysaccharide, has the antioxidation of uniqueness, antibacterial, health care Therapeutic efficiency [Luo Hongyu etc., " impact of Nutrient Contents In Zhejiang Xiushan Sea Mud On Antioxidant Activity of Environmental Organisms " " ocean and lake Natural pond " the 1st phase in 2008].Also have kill demodex brevis and two kinds of human Demodex of demodex folliculorum effect [Hu Ye etc., " the Xiushan sea mud immersion killing action to human Demodex " " China's parasitology and parasitic disease magazine " the 4th phase in 2011]. At the also early useful sea mud treatment dermopathic application example such as tinea pedis and fungal infection among the people, and effect is preferable.Use sea mud bathing The effect being widely known by the people most be enhance metabolism, the dirt of fine hair hole and toxin are done deep layer cleaning, absorption excess oil and Aging cutin, effectively removes the foul being deposited on skin and hindering alimentation process, to skin hypersensitivity dermatitis, skin ulcer rash, Pruritus etc. have certain curative effect.Additionally, the subcutaneous osmotic of mineral additionally aids alleviation joint and myalgia, to treatment nerve Bitterly, the disease such as arthritis, scapulohumeral periarthritis and body-building, reducing weight and beautifying features are respectively provided with the assosting effect of uniqueness.
It is based on sea mud and human body is had many nutrition, health care and medical values, be subject to the deep processing of sea mud as a raw material To the great attention of country, in recent years, it is special to play with different effects in fields such as bathing, medicine, cosmetics, health product Effect.But owing to sea mud urine smell is highly seasoned, infiltration coefficient is little, and absorbability is low, its effective ingredient is difficult to be fully absorbed by skin, makes Use weak effect.And rich in colloid in sea mud, interlayer has a large amount of inorganic ions to show hydrophilic oleophobic property, thus limit its The application in a lot of field such as chemical fibre.Through retrieval, up to now, the most all do not find that sea mud is implanted polyester slice melts It is spun into the precedent of Multifunctional polyester fiber, also has no that document is reported.
Summary of the invention
The purpose of the present invention, it is simply that provide a kind of Multifunctional polyester fiber containing sea mud in order to solve the problems referred to above And preparation method thereof, the fiber fragrance prepared by the method is pleasant, and skin-friendly is good, has both given and has had antibacterial and deodorizing, anti-simultaneously Ultraviolet, acaricide anophelifuge, functions of skin protection and health care, show again preferable spinnability, hygroscopicity, breathability, dyeing uniformity and Mechanical property, wearability is excellent, and sea mud resource is fully used, and has the highest economic worth and the value of environmental protection.
In order to achieve the above object, the technical solution adopted in the present invention is that a kind of multifunction polyester containing sea mud is fine Dimension, its composition of raw materials is by weight percentage: polyester slice 70～95%, sea mud powder 2～18%, Fructus Staphyleae Bumaldae seed extract 0.3～2%, Herba Blumeae Aromaticae extract 1～3.5%, arrow root grass extract 1.6～5%, coupling agent 0.1～1.5%；Its preparation side Method comprises the following steps:
1. preparing sea mud powder: gather a certain amount of sea mud, add water the mud that prepared solid content is 50～60%, adds sea Mud weight 0.1～the sodium tripolyphosphate of 0.9% and 0.2～the fumaric acid of 3%, stir 1～3h in thermostat water bath, quiet Put 24h, discard basic sediment, pour out upper strata mud, solid-liquid separation, gained solid be scattered in sea mud 3～5 times of weight go from In sub-water, filtering, filter cake is dried at 100 DEG C, pulverizes, and crosses 80～100 mesh sieves, obtains sea mud powder；
2. Fructus Staphyleae Bumaldae seed extract is prepared: gather ripe Fructus Staphyleae Bumaldae seed, roguing, be ground into the powder of 80～100 mesh, molten Solution is in the Acetic acid-sodium acetate buffer of pH4.5, and adds powder weight 0.5～the pectase of 2%, and mix homogeneously, in 40 DEG C Lower concussion cultivation 1～2h, centrifugation, take supernatant vacuum lyophilization, grind, cross 200～300 mesh sieves, obtain Fructus Staphyleae Bumaldae Seed extract；
3. prepare Herba Blumeae Aromaticae extract: gather the Herba Blumeae Aromaticae being dried, clean, dry, be ground into the powder of 80～100 mesh, It is placed in the extraction kettle of supercritical extraction instrument, regulates and controls CO2Flow velocity is 10～20g/min, temperature 25～35 DEG C, pressure 25～ Extracting 1～2h under 50MPa, extract carries out two-stage decompression separation, flash trapping stage still pressure is 12～18MPa, secondary response The pressure of still is 5～9MPa, collects the collection product in flash trapping stage still and the second-order separation still, add in the product powder 6～ The dehydrated alcohol extraction 15min of 10 times of weight, adds the extraction of the dehydrated alcohol containing 6% ammonia of powder 3～9 times of weight 20min, heating concentrates, and dries, is ground into powder, obtains Herba Blumeae Aromaticae extract；
4. arrow root grass extract is prepared: gather the arrow root grass being dried, clean, dry, be transferred to after smashing to pieces with pulverizer carry Take vessel, add, by feed liquid weight ratio 1: 3～12, the ethanol that concentration is 70～90wt%, extract 1～3h at 35～50 DEG C, filter Take filtrate；Filtering residue extracts twice after the same method, merges three filtrates, reduces pressure dense under vacuum 0.06～0.08MPa It is reduced to the extractum of relative density 1.05～1.10 when 60 DEG C, is spray-dried, is ground into powder, obtains arrow root grass extract；
5. weigh sea mud powder by formula, be dissolved in deionized water with the weight ratio of 1: 6～15, at frequency 30KHz, power 250～500W, at temperature 40～50 DEG C, ultrasonic disperse processes, in becoming monolithic layer to peel off state, add the Fructus Staphyleae Bumaldae of formula ratio Seed extract, Herba Blumeae Aromaticae extract, arrow root grass extract, add sea mud grain weight amount 0.1～the Nonyl pheno of 3% Ether, continues ultrasonic disperse 30～50min, filters, and gained solids is vacuum dried at 70～80 DEG C, grinds, and crosses 800～1000 Mesh sieve, obtains sea mud/plant complex；
6. weigh coupling agent by formula, add the dehydrated alcohol dilution of coupling agent 1～3 times of weight, obtain diluent；Then Step sea mud/plant complex 5. is dissolved in dehydrated alcohol with the weight ratio of 1: 1～5, under room temperature after ultrasonic disperse, slow Slowly being added dropwise to above-mentioned diluent, ultrasound condition is continued for 15～50min, after reaction terminates, filters, and the sea mud after filtering/ Plant complex, is vacuum dried at 75～85 DEG C, grinds, and obtains modified sea mud/plant complex；
7. by after the polyester slice mix homogeneously of step modified sea mud/plant complex 6. and formula ratio, routinely Melt spinning method, sends into apparatus for melt spinning and carries out co-blended spinning, prepare the Multifunctional polyester fiber containing sea mud.
Preferred as technique scheme, described coupling agent is maleic anhydride inoculated polypropylene, vinyl triethoxyl One or more in silane, 3-(phenyl amino) propyl trimethoxy silicane, γ-aminopropyltriethoxy diethoxy silane are any The mixture of ratio.
Formula given by said method is to ensure that the present invention produces the basic recipe of desired effect, is the skill of the present invention Art core, however in actual applications, completely can be on the basis of inventive formulation, as required, it is also possible to add toughness reinforcing The additives such as agent, lubricant, antioxidant, dispersant, toner, the requirement of these all common with spinning Fypros is phase With, belong to general knowledge well known in the art, as long as and controlling suitably, also will not the present invention be had a negative impact.
The seed that Fructus Staphyleae Bumaldae seed is Staphyleaceae Fructus Staphyleae Bumaldae in above-mentioned raw materials formula, Fructus Staphyleae Bumaldae has another name called basilima sorbifolia, plant Chemical research shows, Fructus Staphyleae Bumaldae seed is mainly composed of crude protein, total flavones, aminoacid, beta-carotene, vitamin E, vitamin The ore deposits such as B1, vitamin B2, vitamin C, Squalene, linoleic acid, linolenic acid, oleic acid, Palmic acid etc. and potassium, calcium, magnesium, sodium, manganese Prime element [Liu Zheng etc., " Staphylea bumalda DC.seed Analysis of Nutritive Composition and evaluation " " economic forest research " the 3rd phase in 2008].
Herba Blumeae Aromaticae in above-mentioned raw materials formula is the herb of dicotyledon medicine feverfew Herba Blumeae Aromaticae, soft aroma and, have Expelling wind and removing dampness, reducing swelling and alleviating pain, effect of dredge the meridian passage, it is possible to the diseases such as treatment rheumatic arthritis, eczema, skin pruritus.Its chemistry Composition is flavonoid, flavanone, sesquiterpenoids, sterols.According to documents and materials, Herba Blumeae Aromaticae ethanol extraction mainly becomes Divide and have stigmasterol, cupreol, β-daucosterol, caffeic acid, gallic acid, Quercetin and luteolin [Jiang Caiwu etc., " strong medicine The chemical constitution study of Herba Blumeae Aromaticae " " Guangxi Normal University's journal (natural science edition) " the 3rd phase in 2012].
Arrow root grass in above-mentioned raw materials formula is the root of leguminous plant climing property arrow root grass, and sweet in the mouth, micro-puckery, property are put down, rich in Huang The compositions such as ketone, tannin, Polyphenols, saccharide, sterol, alkaloid and amino acids are wherein higher with flavones ingredient content.Have Anti-inflammatory and antalgic, antioxidation, antitumor, sterilization, antiviral, resisting cardiovascular disease, scavenging activated oxygen, improve blood capillary The several functions such as permeability and fragility [Lv Chunping, " arrow root grass total flavones antioxidation study of anti-atherogenic effect research " " Jilin 2009 grades of Ph.D. Dissertation of university "].
In said method, introduce sodium tripolyphosphate, sea mud is processed by fumaric acid, on the one hand sloughs except in sea mud Some heavy metal ion, reduce or remove other harmful substances.Sea mud after another side is acidified removes impurity in micropore More thoroughly, having vacated bigger interlayer, its specific surface area is significantly improved, and interlamellar spacing increases, and absorption property is good.Make simultaneously Heat stability, lubricity, water absorption rate, plasticity, expansion multiple and thixotropy have also been obtained bigger raising
The sea mud that said method obtains/plant complex, natural gentleness, it is with sea mud powder as carrier, loads Fructus Staphyleae Bumaldae seed Extract, Herba Blumeae Aromaticae extract, arrow root grass extract can carry as functional active component, the excellent permeability at tea saponin Under Dong, make Fructus Staphyleae Bumaldae seed extract, Herba Blumeae Aromaticae extract, arrow root grass extract be easier to uniformly penetrating to the inside of sea mud powder and Top layer, and agrology and biological result of study show Fructus Staphyleae Bumaldae seed extract, Herba Blumeae Aromaticae extract, arrow root grass extract with Sea mud powder has the highest affinity, it is possible to enters between sea mud bisque smoothly, defines finer and close structure.And through 70～ 80 DEG C of vacuum drying, make mutual absorption between sea mud powder and Fructus Staphyleae Bumaldae seed extract, Herba Blumeae Aromaticae extract, arrow root grass extract State can quickly be fixed up, and the motion of the rotation of molecule, translation and segment is all subject to the biggest constraint, makes Fructus Staphyleae Bumaldae The active component of seed, Herba Blumeae Aromaticae, arrow root grass and fragrance cannot straight line diffusion, slow down precipitation rate, so that antibacterial and deodorizing, anti- The functions such as ultraviolet, acaricide anophelifuge, fragrance, skin-protection and health-care are greatly prolonged the action time on fiber, each after scrubbed 50 times Plant effect and still reach more than 90%.
In sea mud of the present invention/plant complex preparation process, Fructus Staphyleae Bumaldae seed extract, Herba Blumeae Aromaticae extract, arrow Root grass extract and the combination on nanoscale of the sea mud powder, and by NPE to its surface and edge Modifying, make sea mud/plant complex present oleophilic character, interlamellar spacing becomes big, also drops through coupling agent treatment simultaneously Its surface low can, and the affinity between polyester slice strengthens, effectively improve sea mud/plant complex interface polarity and Chemical micro-environment, reaches nanoscale dispersion and has the good compatibility, adhesion with polyester slice.With single employing coupling agent or NPE processes sea mud/plant complex and compares, and has prominent treatment effect, i.e. coupling agent and nonyl phenol There is synergism in polyoxyethylene ether during processing sea mud/plant composite surface, achieves sea mud/plant well Complex is dispersed in polyester fiber, prevents the possibility that it is reunited, spinnability and mechanical property to be greatly improved.
Present inventor finds under study for action, and with sea mud, Fructus Staphyleae Bumaldae seed, Herba Blumeae Aromaticae, arrow root grass are passed through number of ways Manufacturing process, the sea mud that scientific compatibility is made/plant complex, multiple biological activity and the mutual organic infiltration of pharmacologically active, association Same potentiation, not only makes bioavailability all be improved, and substantial change occurs, and has each independent component and do not possess Property or function, create and be provided simultaneously with the one of the functions such as antibacterial and deodorizing, anti-ultraviolet, acaricide anophelifuge, skin-protection and health-care A little new features, this is the most revealed mistake in prior art.
Present inventor after test of many times research find, sea mud after treatment with Fructus Staphyleae Bumaldae seed extract, Herba Blumeae Aromaticae extract, arrow root grass extract are combined by design proportioning, while collaborative enhancing pharmacologically active, also show collaborative Go flavor and enhancing flavor and the transdermal that are added promote to ooze effect, both can eliminate urine smell taste and foreign odor taste, be more conducive to again infiltration, make functional component and Pharmacologically active can be good at being absorbed through skin surface, enters deep layer and body circulation, increases cell viability, it is achieved to people The total care of body skin.
More unexpected, sea mud powder load Fructus Staphyleae Bumaldae seed extract, Herba Blumeae Aromaticae extract, arrow root grass extract Being dispersed in the inside of polyester fiber and top layer with nano structured unit and be integrally forming securely, each component synergism is dashed forward Going out, antibacterial and deodorizing, anti-ultraviolet, acaricide anophelifuge, fragrance, skin-protection and health-care effect are more preferable.Simultaneously as in incorporation polyester fiber Sea mud/plant complex is nanostructured so that polyester fiber produces crack, hole around nanostructured, it is provided that moisture absorption, Ventilative, dyestuff spreads and the passage of infiltration, and the comfortableness of its fibre, drapability and antistatic behaviour, dyeing uniformity have Bigger improvement, wearability is more excellent.
The present invention innovation by selecting materials, in prescription, proportioning and preparation method, by sea mud, Fructus Staphyleae Bumaldae seed, Herba Blumeae Aromaticae, The active substances that had of raw material such as arrow root grass and nutritive and health protection components compounding after be dispersed among polyester fiber, fragrance is happy People, each component cooperates collaborative onset, plays antibacterial and deodorizing, anti-ultraviolet, acaricide anophelifuge, fragrance, effect of skin-protection and health-care altogether, In its prescription, the physiologically active of each composition is as follows:
The activation of sea mud, adsorption function are extremely strong, the mineral element such as contained antibiotics and ferrum, magnesium, zinc, calcium, selenium, germanium, no It is placed only in skin surface, plays physics uvioresistant, absorb free radical, the effect of promotion active component infiltration, and mineral nitrogen Element permeates in skin, adsorbs the positively charged grease soils in band skin follicle, sweat gland and surface, dead epidermis cell, antibacterial. After the cleaning of the degree of depth, the nutritional labeling discharged more can go deep into skin absorption.
Sea mud has sterilization, antiinflammatory, makes the ability of cell regeneration, can treat skin pruritus, antibacterial infection, red and swollen, tinea Deng, in addition to treatment rheumatic arthritis, myalgia, by the strongest penetration, drive mineral element to transport toward deep skin, Blood circulation promoting, supplements the mineral element needed for skin, allow skin whitening, anti-solarization, tighten up.
Flavone has the effects such as broad-spectrum antiseptic, antiinflammatory, antioxidation, absorption ultraviolet, suppression tyrosinase activity, it is possible to increase The nutrition supply of strong skin and the excretion of metabolite, remove skin surface noxious bacteria, prevent bacterial reproduction.
The antioxidation of Polyphenols, antimutagenic, defying age, bacteriostasis are extremely strong, and can effectively stop that free radical causes is thin The damage to cell membrane of the after birth ester matter peroxidation, has whitening and speckle dispelling, antiinflammatory, protectiving ultraviolet damage, promotion skin generation The effect thanked.
Tannin has antibacterial, antiviral, enzyme inhibition activity and antioxidation, mutation, antiinflammatory and anti-tumor activity, can reduce skin Skin melanin, black speck and freckle, make whitening skin.
Vitamin E have absorb ultraviolet ability, can sun-proof skin care, and can antiinflammatory, antipruritic, skin moistening, delaying skin Old and feeble.
Squalene is good with cutaneous permeability, can improve the oxygen carrying capacity of human body hemoglobin, enhance metabolism, suppression Tyrosinase activity, effectively stop cause in human body skin damnification, short wave ultraviolet, simultaneously allow again some physiological neeies Ultraviolet pass through, the biological function brought into normal play.
Quercetin has the strongest antibacterial work to various pathogens such as staphylococcus aureus, escherichia coli and bacillus pyocyaneus Property, there is certain deodorization.
Reseda have defying age, radioprotective, free radical resisting, antioxidation, antiinflammatory, antiviral, the biological activity such as antibacterial.
Sesquiterpenoids fragrance and refusing to eat insecticidal activity are relatively strong, have anthelmintic parasite killing, antibacterial, antitumor, antiviral, The multiple effect such as immunosuppressant.
Caffeic acid has enhancing immunity anti-inflammatory properties, and can suppress hyaluronidase, and protection collagen protein is from may result in The impact of the free radical of its degraded.
Gallic acid has defying age, sun-proof speckle removing, releases heavy metallic poison, anti-inflammation and promotion skin microcirculation work With.
Vitamin C is a kind of strong antioxidant, and it can protect human body from the damage of free radical, resists black Element produces, and makes whitening skin beautiful.
Cupreol have antiinflammatory, bring down a fever, antiulcer, promote skin metabolism, can anti-sunburn and skin aging Effect.
Linolenic acid can resist free radical, aging resistance, helps to absorb vitamin C and vitamin E, the bullet of strengthening blood circulation Property, reduce the injury of ultraviolet, the collagen protein in protection skin, improve venous engorgement and edema, prevent melanin deposition.
Containing conjugated double bond structures in β-daucosterol molecule, there is reproducibility, free radical can be captured, reduce Cell membrane lipids mistake Oxidation, has antioxidation, antitumor, radioprotective, enhancing immunity and delaying senility function.
Aminoacid is easily absorbed by the skin, and to preventing and treating, xerosis cutis, coarse and wrinkle etc. are effective, also can strengthen skin Resistance against diseases.
The present invention, by the mutual organic infiltration of each effective ingredient in sea mud, Fructus Staphyleae Bumaldae seed, Herba Blumeae Aromaticae, arrow root grass, significantly carries High bioavailability.Inventor, it was unexpectedly observed that the flavone compound use of Fructus Staphyleae Bumaldae seed, Herba Blumeae Aromaticae, arrow root grass, works in coordination with and increases Effect, creates prior art the most antibacterial unexpected, antiinflammatory, antioxidation, defying age, absorption ultraviolet effect.Sea mud removes Outside treatment rheumatic arthritis, myalgia, can block, reflected sunlight, its effective ingredient calcium carbonate and human sweat In lactic acid react, fetid sweat can be eliminated at short notice；Gallic acid is combined with aminoacid, energy regulation of skin pH value, Keeping acid-base balance, make skin elasticity increase, wrinkle reduces, slow down aging；Herba Blumeae Aromaticae extract coordinates with various raw materials, performance Go out to work in coordination with the flavouring being added and go raw meat and smelly eliminating effect；Polyphenol can eliminate free radical, makes whitening skin beautiful；Cupreol is raw with dimension Element C share, and has strong antifeedant activity, can effective expelling mosquito and kill acarid, itch mite and acaricide killing rate are reached 98%；Ore deposit Prime element and Squalene, linoleic acid compatibility, promote ability of oozing strong, can greatly promote the skin absorption of various effective ingredient.Aobvious and Being clear to, the fibre fragrance obtained by the present invention is pleasant, and skin-friendly is good, next to the skin with human body contact just can be formed antibacterial and deodorizing, Slowly release the approach that nutritional labeling is absorbed by human skin while uvioresistant, acaricide anophelifuge, promote health. Especially the diseases such as treatment neuralgia, arthritis, comedo, allergic dermatitis and body-building, reducing weight and beautifying features are respectively provided with uniqueness Assosting effect.After tested: the rate of ultraviolet shield of this fibre reaches 90%, UPF value >=40；To Staphylococcus aureus Bacterium, escherichia coli, Candida albicans etc. have stronger inhibitory action, and bacteriostasis rate is more than 90%.
The polyester fiber of the present invention can be the most knitting, woven or be made into fabric with other natural fibers, chemical fibre blending, Then according to the demand of people, make underwear, shirt, nightwear, T-shirt, gym suit, socks, sheet, bedding etc. next to the skin with human body The various textiles of contact, wide application.And sea mud resource is fully used, provides one for the resource of sea mud and have The direction of advantage, it has the hugest expected economic worth and the value of environmental protection.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described, all bases made according to the disclosure of invention Any equivalent in field, belongs to protection scope of the present invention.
In the present invention, if not refering in particular to, all of equipment, raw material and auxiliary agent etc. are all commercially available or the industry is commonly used , all of percentage ratio, part are unit of weight.
Property indices in following example, all uses following method of testing and standard:
One, antibacterial test: according to standard GB/T/20944.3-2008 " the evaluation third portion of antibacterial textile performance: Succusion " method test, the anti-microbial property of sample is evaluated by bacteriostasis rate, and computing formula is:
Xs=(A-B)/A
In formula: XsFor bacteriostasis rate (%)；A is by average colony number before test agent vibration；B is for average after being vibrated by test agent Clump count, if the average colony number after Zhen Dang is more than the average colony number before vibration, bacteriostasis rate is by 0 calculating.
Two, anti-ultraviolet test: according to standard GB/T/T18830-2009 " evaluation of ultraviolet resistance of fabric ", The ultraviolet using U.S. Labsphere (blue luxuriant and rich with fragrance optics) UV-2000F yarn fabric SPF (sun protection factor) analyser test blend fabric is prevented Protect coefficient UPF and ultraviolet ray transmissivity T.As the UPF ＞ 30 of fabric, during T (UVA) ＜ 5%, this fabric belongs to anti-ultraviolet and produces Product.
Three, anti-demodicid mite performance test: " anti-demodicid mite evaluation methodology and the standard " formulated for 1993 with reference to Japan, uses Proliferation Ability Effect judges test, is pasted onto by fabric sample bottom the glass container of diameter 45mm, highly 15mm, adjusts demodicid mite in acarid feedstuff The quantity of worm, to 20～80/0.1g, takes 0.1g and puts in container, container is put into conditioned process be used for preserve food In airtight plastic ware, put in the calorstat of 25 ± 2 DEG C, after the time needed, sample is washed with water, and uses saline Floatation calculates the mite population of survival.
The computing formula of proliferation inhibition rate is:
Proliferation inhibition rate (%)=(blank test piece survival mite population-mite-proofing and antimicrobial fabric survival mite population)/blank Test piece survival mite population.
Embodiment one
1. pretreatment of raw material
1. preparing sea mud powder: gather the Xiushan Mountain, a certain amount of Zhoushan beach sea mud, add water the mud that prepared solid content is 40%, Add the sodium tripolyphosphate of sea mud weight 0.6% and the fumaric acid of 1.3%, thermostat water bath stirs 1h, stands 24h, discards basic sediment, pours out upper strata mud, solid-liquid separation, and gained solid is scattered in the deionized water of 3 times of weight of sea mud In, filtering, filter cake is dried at 100 DEG C, pulverizes, and crosses 85 mesh sieves, obtains sea mud powder；
2. Fructus Staphyleae Bumaldae seed extract is prepared: gather ripe Fructus Staphyleae Bumaldae seed, roguing, be ground into the powder of 95 mesh, be dissolved in In the Acetic acid-sodium acetate buffer of pH4.5, and add the pectase of powder weight 0.8%, mix homogeneously, shakes at 40 DEG C Cultivate 1h, centrifugation, take supernatant vacuum lyophilization, grind, cross 200 mesh sieves, obtain Fructus Staphyleae Bumaldae seed extract；
3. prepare Herba Blumeae Aromaticae extract: gather the Herba Blumeae Aromaticae being dried, clean, dry, be ground into the powder of 85 mesh, be placed in super In the extraction kettle of critical abstraction instrument, regulate and control CO2Flow velocity is 18g/min, extracts 1h under temperature 25 DEG C, pressure 30MPa, will extraction Thing carries out two-stage decompression separation, and flash trapping stage still pressure is 13MPa, and the pressure of secondary response still is 6MPa, collects flash trapping stage Collection product in still and the second-order separation still, adds the dehydrated alcohol extraction 15min of 8 times of weight of powder in the product, adds Dehydrated alcohol containing the 6% ammonia extraction 20min of 5 times of weight of powder, heating concentrates, and dries, is ground into powder, obtains Herba Blumeae Aromaticae Extract；
4. arrow root grass extract is prepared: gather the arrow root grass being dried, clean, dry, be transferred to after smashing to pieces with pulverizer carry Taking vessel, adding concentration by feed liquid weight ratio 1: 10 is the ethanol of 70wt%, extracts 1.5h, cross leaching filtrate at 35 DEG C；Filtering residue Extract after the same method twice, merge three filtrates, under vacuum 0.06MPa, be evaporated to relative density when 60 DEG C The extractum of 1.05, is spray-dried, is ground into powder, obtains arrow root grass extract.
2. composition of raw materials:
Polyester slice 85kg, sea mud powder 9.5kg, Fructus Staphyleae Bumaldae seed extract 0.5kg, Herba Blumeae Aromaticae extract 2kg, arrow root grass carries Take thing 1.5kg, VTES 0.9kg, γ-aminopropyltriethoxy diethoxy silane 0.6kg.
3. preparation process:
1. weigh sea mud powder 9.5kg, be dissolved in the deionized water of 95kg, at frequency 30KHz, power 450W, temperature 50 C Lower ultrasonic disperse process, in become monolithic layer peel off state, add the Fructus Staphyleae Bumaldae seed extract of 0.5kg, 2kg Herba Blumeae Aromaticae extract Thing, the arrow root grass extract of 1.5kg, add the NPE of 0.095kg, continues ultrasonic disperse 35min, mistake Filter, gained solids is dried at 70 DEG C, grinds, and crosses 1000 mesh sieves, obtains sea mud/plant complex；
2. VTES 0.9kg, γ-aminopropyltriethoxy diethoxy silane 0.6kg is weighed by formula.Add Enter the dehydrated alcohol dilution of 3kg, obtain diluent；Then step 1. sea mud/plant complex is dissolved in the weight ratio of 1: 2.5 In dehydrated alcohol, under room temperature after ultrasonic disperse, being slowly added dropwise into above-mentioned diluent, ultrasound condition is continued for 15min, reaction After end, filter, the sea mud/plant complex after filtering, be vacuum dried at 75 DEG C, grind, obtain modified sea mud/plant Complex；
3. by after the polyester slice mix homogeneously of step modified sea mud/plant complex 2. and 85kg, routinely molten Melting spin processes, send into apparatus for melt spinning and carry out co-blended spinning, concrete spinning technique is FDY technique: spinning temperature be 220～ 260 DEG C, spinning speed is 3500m/min, setting temperature 130～150 DEG C；Prepared specification is 20～300D/12～48f, fracture The multifunction polyester FDY filament containing sea mud of intensity ＞ 3.8cN/dtex；
4. 3. step is contained the multifunction polyester FDY filament of sea mud, uses knitting machine to be woven into fabric, dyeing, then stitch Make underwear, underwear.After tested: the bacteriostasis rate 98.5% of staphylococcus aureus, colibacillary bacteriostasis rate 96.3%, white The bacteriostasis rate 95.7% of candidiasis, UPF value 132, UVA transmitance 2.05%, itch mite and acaricide killing rate are reached 99.5%.
Embodiment two
1. pretreatment of raw material
1. preparing sea mud powder: gather a certain amount of Shandong region tidal flat of Bohai Bay sea mud, the prepared solid content that adds water is 45% Mud, adds the sodium tripolyphosphate of sea mud weight 0.3% and the fumaric acid of 1.5%, stirs in thermostat water bath 1.5h, stands 24h, discards basic sediment, pour out upper strata mud, solid-liquid separation, gained solid dispersion 4 times of weight of sea mud in In deionized water, filtering, filter cake is dried at 100 DEG C, pulverizes, and crosses 100 mesh sieves, obtains sea mud powder；
2. Fructus Staphyleae Bumaldae seed extract is prepared: gather ripe Fructus Staphyleae Bumaldae seed, roguing, be ground into the powder of 100 mesh, be dissolved in In the Acetic acid-sodium acetate buffer of pH4.5, and add the pectase of powder weight 1.1%, mix homogeneously, shakes at 40 DEG C Cultivate 1.5h, centrifugation, take supernatant vacuum lyophilization, grind, cross 250 mesh sieves, obtain Fructus Staphyleae Bumaldae seed extract；
3. prepare Herba Blumeae Aromaticae extract: gather the Herba Blumeae Aromaticae being dried, clean, dry, be ground into the powder of 95 mesh, be placed in super In the extraction kettle of critical abstraction instrument, regulate and control CO2Flow velocity is 15g/min, extracts 1.5h under temperature 35 DEG C, pressure 38MPa, will extraction Taking thing and carry out two-stage decompression separation, flash trapping stage still pressure is 15MPa, and the pressure of secondary response still is 7MPa, collects a fraction Collection product in still and the second-order separation still, adds the dehydrated alcohol extraction 15min of 6 times of weight of powder in the product, then adds Entering the extraction 20min of the dehydrated alcohol containing 6% ammonia of 9 times of weight of powder, heating concentrates, and dries, is ground into powder, obtains Artemisia argyi Receive extract；
4. arrow root grass extract is prepared: gather the arrow root grass being dried, clean, dry, be transferred to after smashing to pieces with pulverizer carry Taking vessel, adding concentration by feed liquid weight ratio 1: 9 is the ethanol of 85wt%, extracts 1h, cross leaching filtrate at 50 DEG C；Filtering residue according to Same method is extracted twice, merges three filtrates, is evaporated to relative density 1.10 when 60 DEG C under vacuum 0.07MPa Extractum, be spray-dried, be ground into powder, obtain arrow root grass extract.
2. composition of raw materials:
Polyester slice 83kg, sea mud powder 11kg, Fructus Staphyleae Bumaldae seed extract 1.2kg, Herba Blumeae Aromaticae extract 1.8kg, arrow root grass Extract 1.7kg, VTES 0.6kg, γ-aminopropyltriethoxy diethoxy silane 0.7kg.
3. preparation process:
1. weigh sea mud powder 11kg, be dissolved in the deionized water of 121kg, at frequency 30KHz, power 380W, temperature 45 C Lower ultrasonic disperse processes, in becoming monolithic layer to peel off state, add the Fructus Staphyleae Bumaldae seed extract of 1.2kg, the Herba Blumeae Aromaticae of 1.8kg and carry Take the arrow root grass extract of thing, 1.7kg, add the NPE of 0.22kg, continue ultrasonic disperse 50min, mistake Filter, gained solids is dried at 80 DEG C, grinds, and crosses 800～1000 mesh sieves, obtains sea mud/plant complex；
2. weigh VTES 0.6kg, γ-aminopropyltriethoxy diethoxy silane 0.7kg by formula, add Enter the dehydrated alcohol dilution of 2.6kg, obtain diluent；Then step 1. sea mud/plant complex is dissolved in the weight ratio of 1: 3 In dehydrated alcohol, under room temperature after ultrasonic disperse, being slowly added dropwise into above-mentioned diluent, ultrasound condition is continued for 30min, reaction After end, filter, the sea mud/plant complex after filtering, be vacuum dried at 85 DEG C, grind, obtain modified sea mud/plant Complex；
3. after step modified sea mud/plant complex 2. being mixed homogeneously with the polyester slice of 83kg, routinely molten Melting spin processes, send into apparatus for melt spinning and carry out co-blended spinning, extruder temperature is 200～260 DEG C, spinning speed be 800～ 1500m/min, drawing temperature is 70～150 DEG C, and drafting multiple is 2～4 times, prepares the short fibre of multifunction polyester containing sea mud Dimension；
4. 3. step is contained multifunction polyester chopped fiber 65kg of sea mud, mixes with cotton fiber or the polyamide staple fibre of 35kg Conjunction is spun into yarn, uses tricot machine to be woven into fabric, dyeing, then is sewn into underwear, underwear.After tested: Staphylococcus aureus The bacteriostasis rate 92.9% of bacterium, colibacillary bacteriostasis rate 90.6%, the bacteriostasis rate 91.5% of Candida albicans, UPF value 97, UVA Transmitance 1.65%, reaches 97% to itch mite and acaricide killing rate.

Claims (2)

1. the Multifunctional polyester fiber containing sea mud, it is characterised in that the composition of raw materials of this fiber is by weight percentage For polyester slice 70～95%, sea mud powder 2～18%, Fructus Staphyleae Bumaldae seed extract 0.3～2%, Herba Blumeae Aromaticae extract 1～ 3.5%, arrow root grass extract 1.6～5%, coupling agent 0.1～1.5%；Its preparation method comprises the following steps:
1. preparing sea mud powder: gather a certain amount of sea mud, add water the mud that prepared solid content is 40～50%, adds sea mud weight Amount 0.1～the sodium tripolyphosphate of 0.9% and 0.2～the fumaric acid of 3%, stir 1～3h in thermostat water bath, stand 24h, discards basic sediment, pours out upper strata mud, solid-liquid separation, and gained solid is scattered in sea mud 3～the deionization of 5 times of weight In water, filtering, filter cake is dried at 100 DEG C, pulverizes, and crosses 80～100 mesh sieves, obtains sea mud powder；
2. Fructus Staphyleae Bumaldae seed extract is prepared: gather ripe Fructus Staphyleae Bumaldae seed, roguing, be ground into the powder of 80～100 mesh, be dissolved in In the Acetic acid-sodium acetate buffer of pH4.5, and add powder weight 0.5～the pectase of 2%, mix homogeneously, shakes at 40 DEG C Swing cultivation 1～2h, centrifugation, take supernatant vacuum lyophilization, grind, cross 200～300 mesh sieves, obtain Fructus Staphyleae Bumaldae seed and carry Take thing；
3. prepare Herba Blumeae Aromaticae extract: gather the Herba Blumeae Aromaticae being dried, clean, dry, be ground into the powder of 80～100 mesh, be placed in In the extraction kettle of supercritical extraction instrument, regulate and control CO2Flow velocity is 10～20g/min, at temperature 25～35 DEG C, pressure 25～50MPa Lower extraction 1～2h, carries out two-stage decompression separation by extract, and flash trapping stage still pressure is 12～18MPa, the pressure of secondary response still Power is 5～9MPa, collects the collection product in flash trapping stage still and the second-order separation still, adds powder 6～10 times of weights in the product The dehydrated alcohol extraction 15min of amount, adds the extraction 20min of the dehydrated alcohol containing 6% ammonia of powder 3～9 times of weight, heating Concentrate, dry, be ground into powder, obtain Herba Blumeae Aromaticae extract；
4. arrow root grass extract is prepared: gather the arrow root grass being dried, clean, dry, after smashing to pieces with pulverizer, be transferred to extractor Ware, adds, by feed liquid weight ratio 1: 3～12, the ethanol that concentration is 70～90wt%, extracts 1～3h at 35～50 DEG C, crosses leaching filter Liquid；Filtering residue extracts twice after the same method, merges three filtrates, is evaporated under vacuum 0.06～0.08MPa The extractum of relative density 1.05～1.10 when 60 DEG C, is spray-dried, is ground into powder, obtains arrow root grass extract；
5. weigh sea mud powder by formula, be dissolved in deionized water with the weight ratio of 1: 6～15, frequency 30KHz, power 250～ At 500W, temperature 40～50 DEG C ultrasonic disperse process, in become monolithic layer peel off state, add formula ratio Fructus Staphyleae Bumaldae seed extract Thing, Herba Blumeae Aromaticae extract, arrow root grass extract, add sea mud grain weight amount 0.1～the NPE of 3%, continues Ultrasonic disperse 30～50min, filters, and gained solids is dried at 70～80 DEG C, grinds, and crosses 800～1000 mesh sieves, obtains sea Mud/plant complex；
6. weigh coupling agent by formula, add the dehydrated alcohol dilution of coupling agent 1～3 times of weight, obtain diluent；Then will step Rapid sea mud/plant complex 5. is dissolved in dehydrated alcohol with the weight ratio of 1: 1～5, under room temperature after ultrasonic disperse, slowly drips Adding above-mentioned diluent, ultrasound condition is continued for 15～50min, after reaction terminates, filters, the sea mud/plant after filtering Complex, is vacuum dried at 75～85 DEG C, grinds, and obtains modified sea mud/plant complex；
7. by after the polyester slice mix homogeneously of step modified sea mud/plant complex 6. and formula ratio, routinely melted Spin processes, sends into apparatus for melt spinning and carries out co-blended spinning, prepare the Multifunctional polyester fiber containing sea mud.
A kind of Multifunctional polyester fiber containing sea mud the most according to claim 1, it is characterised in that described coupling agent is Maleic anhydride inoculated polypropylene, VTES, 3-(phenyl amino) propyl trimethoxy silicane, γ-aminopropyl The mixture of one or more arbitrary proportions in methyldiethoxysilane.
CN201610493452.7A 2016-06-19 2016-06-19 A kind of Multifunctional polyester fiber containing sea mud and preparation method thereof Pending CN106192057A (en)

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CN106619229A (en) * 2017-01-13 2017-05-10 华南理工大学 Oil-tea sunscreen cream and preparation method thereof
CN109371499A (en) * 2018-10-30 2019-02-22 中科纺织研究院（青岛）有限公司 A kind of plant modified dacron fabric and preparation method thereof
CN109487360A (en) * 2018-08-22 2019-03-19 中科纺织研究院（青岛）有限公司 A kind of polyester fiber containing plant extracts
CN110055613A (en) * 2019-04-11 2019-07-26 中科纺织研究院（青岛）有限公司 A kind of Paeonol terylene chips fiber and preparation method thereof
CN110735211A (en) * 2019-11-06 2020-01-31 青岛百草新材料股份有限公司 plant functional seat fabric and preparation method thereof
CN110863252A (en) * 2019-11-06 2020-03-06 百事基材料（青岛）股份有限公司 Plant functional polyester filament and preparation method thereof

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CN105239201A (en) * 2015-08-15 2016-01-13 陆思烨 Toothbrush hair having anti-bacterial and health-caring function and preparation method thereof

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CN106619229B (en) * 2017-01-13 2019-06-18 华南理工大学 A kind of oil tea suncream and preparation method thereof
CN109487360A (en) * 2018-08-22 2019-03-19 中科纺织研究院（青岛）有限公司 A kind of polyester fiber containing plant extracts
EP3748050A4 (en) * 2018-08-22 2021-08-04 Sinotech Academy Of Textile (Qingdao) Co., Ltd. Plant extract-containing polyester fiber
US11174574B2 (en) * 2018-08-22 2021-11-16 Sinotech Academy Of Textile (Qingdao) Co., Ltd. Plant-extract-containing polyester fiber
CN109371499A (en) * 2018-10-30 2019-02-22 中科纺织研究院（青岛）有限公司 A kind of plant modified dacron fabric and preparation method thereof
CN110055613A (en) * 2019-04-11 2019-07-26 中科纺织研究院（青岛）有限公司 A kind of Paeonol terylene chips fiber and preparation method thereof
CN110735211A (en) * 2019-11-06 2020-01-31 青岛百草新材料股份有限公司 plant functional seat fabric and preparation method thereof
CN110863252A (en) * 2019-11-06 2020-03-06 百事基材料（青岛）股份有限公司 Plant functional polyester filament and preparation method thereof
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