CN107012530B - A kind of mosquito repellent nylon-6 fiber and preparation method thereof - Google Patents
A kind of mosquito repellent nylon-6 fiber and preparation method thereof Download PDFInfo
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- CN107012530B CN107012530B CN201710334526.7A CN201710334526A CN107012530B CN 107012530 B CN107012530 B CN 107012530B CN 201710334526 A CN201710334526 A CN 201710334526A CN 107012530 B CN107012530 B CN 107012530B
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- mosquito repellent
- master batch
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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
- D01F6/90—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 polyamides
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Catching Or Destruction (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention provides a kind of mosquito repellent nylon-6 fiber, mosquito repellent master batch is made, then mosquito repellent master batch and nylon-6 fiber are made mosquito repellent polyamide fibre 6 in micro-capsule made from attapulgite and plant mosquito repellent product by mosquito repellent nylon-6 fiber.The present invention also provides a kind of preparation methods of mosquito repellent nylon-6 fiber, include the following steps that by supercritical extraction method, plant mosquito repellent product extract is made in plant mosquito repellent product by (1)；(2) micro-capsule is made in plant mosquito repellent product extract；(3) by the suction-operated of attapulgite, mosquito repellent master batch is made with plant mosquito repellent product micro-capsule；(4) mosquito repellent polyamide fibre 6 is made in mosquito repellent master batch and nylon-6 fiber.The mosquito repellent nylon-6 fiber is more environmentally friendly, safe to the human body.
Description
1st, technical field
The invention belongs to function textile fields, are related to a kind of mosquito repellent nylon-6 fiber and preparation method thereof.
2nd, background technology
With the raising of economic level, people now begin to more pay close attention to the quality of life, for textile, base
This wearability cannot fully meet consumer demand, the function textile of particular utility be assigned, in numerous weavings
Show one's talent in product, favored by consumer.Using Nantural non-toxic material, one is attached to by finishing functions and fabric
It rises, carries out the research and development of natural anophelifuge function textile, make people while clothing is worn, just can easily make mosquito former
Oneself is managed, has not only reduced the probability of disease infection, but also a safe and healthy living environment can be built in a small range.
Attapulgite is a kind of mineral clay with stronger adsorption bleaching ability, and the reserves that I crosses Jiashan county are larger.
Attapulgite is a kind of aqueous alumina magnesia silicate, is occurred with special fibrous crystal.It is 2:The clay of 1 type, i.e., two layers
Oxygen-octahedron presss from both sides one layer of alumina octahedral, replaces a series of crystalline substance there are sectional areas for 0.38 × 0.63nm in lattice structure
Body opening road, internal surface area is larger, therefore with very strong physical absorption and decoloring ability.Main physical and chemical performance and processing performance
Have：Cationic interchangeability, water imbibition, adsorption bleaching, big specific surface area (9.6~36m2/ g) and colloid index and expansion
Hold.Due to the special physicochemical properties and processing performance that attapulgite has, make its oil, chemical industry, building materials, papermaking,
Medicine, agricultural etc. are used widely.
Synthetic fibers due to possess abundant raw material, it is wide in variety, production efficiency is high and wearability is good many advantages, such as, for many years
To be widely used in always in knitting product.Nylon fibre (PA) kind earliest as industrialized production in synthetic fibers, product
Based on long filament, hygroscopicity and wearability are best in synthetic fibers, be mainly used for socks, tire cord, parachute,
The prevalence of shirt and easy dress etc., people also begin to focus on research of the polyamide fibre in terms of functionality.
The current mosquito repellent product used both at home and abroad, mostly uses synthesis repellant, such as Metadelphene or dimethyl phthalate, closes
Environmental protection and safety issue can be all brought into repellent agent.As Chinese invention patent CN201210080003.1 discloses a kind of mosquito repellent
Nylon-6 fiber, after attapulgite is adsorbed dimethyl phthalate, addition 6 resin of additive and polyamide fibre, obtained mosquito repellent chinlon master batch, then with
Chinlon 6 section carry out melt blending spinning mosquito repellent nylon-6 fiber is made, used dimethyl phthalate and chemical addition agent, not environmentally and
To human body, there are potential safety issues.
3rd, invention content
The object of the present invention is to provide a kind of mosquito repellent polyamide fibre, which is existed using the mosquito repellent product of extracted form natural plant
Spinning incorporates nanometer of master batch when processing, and fabric is made to keep duration repelling effect.
In order to achieve the above object, present invention employs following technical solutions：By attapulgite and plant mosquito repellent product system
Mosquito repellent master batch is made in the micro-capsule obtained, then mosquito repellent master batch and nylon-6 fiber are made mosquito repellent polyamide fibre 6.
Further, the plant mosquito repellent product is lemongrass, folium eucalypti, folium artemisiae argyi or peppermint.
Further, in the mosquito repellent polyamide fibre, the weight percent of polyamide fibre 6 is 70~80%, the mosquito repellent master batch
Weight percent be 20~30%；In the mosquito repellent master batch, the weight percent of attapulgite is 50~70%, and plant drives
The weight percent of mosquito product extract is 30%~50%.
Further requirement of the present invention protects a kind of preparation method of mosquito repellent nylon-6 fiber, includes the following steps：
(1) plant mosquito repellent product extract is made by supercritical extraction method in plant mosquito repellent product；
(2) micro-capsule is made in plant mosquito repellent product extract；
(3) by the suction-operated of attapulgite, mosquito repellent master batch is made with plant mosquito repellent product micro-capsule；
(4) mosquito repellent polyamide fibre 6 is made in mosquito repellent master batch and nylon-6 fiber.
Preferably, a kind of preparation method of mosquito repellent nylon-6 fiber, includes the following steps：
(1) plant mosquito repellent product is crushed, be placed in extraction kettle, using 70%~90% ethyl alcohol as entrainer, adjust super face
Boundary CO2Fluid temperature (F.T.), pressure；Extraction temperature is 30 DEG C~50 DEG C, and extracting pressure is 10MPa~40MPa, extraction time for 1~
3h；Extract liquor is collected, centrifugal concentrating is evaporated extract；
(2) suitable gelatin is weighed respectively and Arabic gum adds in the aqueous solution of configuration quality score 1%, at 40~50 DEG C
Stirring and dissolving is complete, then adds in extract, and with 10000~15000r/min emulsifying rates, 5~15min of high speed shear is used
1% aqueous acetic acid adjusts pH=4.0, and ice water is cooled to 5 DEG C, then adjusts pH=9.0 with 1% sodium hydrate aqueous solution,
0.2% formalin is cured, and obtains extract microcapsule；
(3) by attapulgite dispersion in deionized water, after ultrasound 1h after being sufficiently stirred, standing 10min upper strata is poured out to hang
Supernatant liquid removes the remaining magazine of container bottom, 2-3 times repeatedly, adds in suspension of suitable hydrochloric acid after above-mentioned purification, impregnates
It 1-2 days, is subsequently placed in Rotary Evaporators, rotary evaporation is placed on vacuum drying chamber drying.It is then dissolved in absolute ethyl alcohol, adds
Enter extract microcapsule obtained, then mixed liquor rotary evaporation in vacuo, drying crush, mosquito repellent master batch is made；
(4) mosquito repellent master batch/slices of caprone → drying → screw extruding (blending) → filament spinning component filtering → spinning → is blown
Air cooling, which oils, → winding → examines → adds bullet → coiling and molding → draw-teisting → to twist → compressing and washing → afterwards to dry → thermal finalization
→ balance → bucket → packaging → inspection → finished product.
Further, the plant mosquito repellent product described in the preparation method of mosquito repellent nylon-6 fiber is lemon-grass, folium eucalypti, Chinese mugwort
Leaf or peppermint.
The present invention has the following advantages：
(1) the present invention provides a kind of new mosquito repellent nylon-6 fiber, which is utilized natural plants drive
Mosquito product, it is environmentally friendly and safe to the human body.
(2) mosquito repellent master batch is made using attapulgite and plant mosquito repellent product micro-capsule in mosquito repellent nylon-6 fiber of the invention,
The long-acting purpose of sustained release can be reached.
(3) mosquito repellent nylon-6 fiber of the present invention has mosquito walks quickly and keeps away effect well, after placing 120 days, still has to mosquito good
Good walks quickly and keeps away effect.
4th, specific embodiment
The specific embodiment of form by the following examples makees further specifically the above of the present invention
It is bright.But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to following embodiment.
The preparation of 1 lemongrass extract of embodiment
Lemon-grass is crushed, is placed in extraction kettle, using 70~90% ethyl alcohol as entrainer, adjusts supercritical CO2Fluid temperature
Degree, pressure；Extraction temperature is 50 DEG C, extracting pressure 15MPa, extraction time 1.5h；Extract liquor is collected, centrifugal concentrating is evaporated
Extract.
The preparation of 2 mint extract of embodiment
Peppermint is crushed, is placed in extraction kettle, using 70~90% ethyl alcohol as entrainer, adjusts supercritical CO2Fluid temperature (F.T.),
Pressure；Extraction temperature is 50 DEG C, extracting pressure 15MPa, extraction time 2h；Extract liquor is collected, centrifugal concentrating is evaporated extraction
Object.
The preparation of 3 Folium Artemisiae Argyi extract of embodiment
Folium artemisiae argyi is crushed, is placed in extraction kettle, using 70~90% ethyl alcohol as entrainer, adjusts supercritical CO2Fluid temperature (F.T.),
Pressure；Extraction temperature is 40 DEG C, extracting pressure 15MPa, extraction time 2h；Extract liquor is collected, centrifugal concentrating is evaporated extraction
Object.
The preparation of 4 folium eucalypti extract of embodiment
Folium eucalypti is crushed, is placed in extraction kettle, using 70~90% ethyl alcohol as entrainer, adjusts supercritical CO2Fluid temperature (F.T.),
Pressure；Extraction temperature is 60 DEG C, extracting pressure 10MPa, extraction time 4h；Extract liquor is collected, centrifugal concentrating is evaporated extraction
Object.
The preparation of 5 plant extracts micro-capsule of embodiment
Suitable gelatin is weighed respectively and Arabic gum adds in the aqueous solution of configuration quality score 1%, is stirred at 40~50 DEG C
It is complete to mix dissolving, extract made from embodiment 1-4 is then added in, with 10000~15000r/min emulsifying rates, high speed shear
5~15min adjusts pH=4.0 with 1% aqueous acetic acid, and ice water is cooled to 5 DEG C, is then adjusted with 1% sodium hydrate aqueous solution
PH=9.0,0.2% formalin are cured, and obtain the micro-capsule of extract.
The preparation of 6 mosquito repellent chinlon master batch of the present invention of embodiment
Proportioning 1：
| Attapulgite | 70% |
| Lemongrass extract | 30% |
Proportioning 2：
| Attapulgite | 80% |
| Lemongrass extract | 20% |
Proportioning 3：
| Attapulgite | 40% |
| Lemongrass extract | 60% |
Proportioning 4：
| Attapulgite | 50% |
| Mint extract | 50% |
Proportioning 5：
| Attapulgite | 65% |
| Folium Artemisiae Argyi extract | 35% |
Proportioning 6：
| Attapulgite | 60% |
| Folium eucalypti extract | 40% |
By attapulgite dispersion in deionized water, ultrasound 1h after being sufficiently stirred pours out upper strata suspension after standing 10min
Liquid, the removal remaining magazine of container bottom, 2-3 times repeatedly.Suspension of suitable hydrochloric acid after above-mentioned purification is added in, impregnates 1-
It 2 days, is subsequently placed in Rotary Evaporators, rotary evaporation is placed on vacuum drying chamber drying.It is then dissolved in absolute ethyl alcohol, adds in
Extract microcapsule obtained in embodiment 5, then mixed liquor rotary evaporation in vacuo, drying crush, and mosquito repellent master batch is made.
The preparation of 7 mosquito repellent polyamide fibre of the present invention of embodiment
Proportioning 1：
| Polyamide fibre 6 | 80% |
| Lemongrass mosquito repellent master batch | 20% |
Proportioning 2：
| Polyamide fibre 6 | 70% |
| Peppermint mosquito repellent master batch | 30% |
Proportioning 3：
| Attapulgite | 70% |
| Mugwort mosquito repellant master batch | 30% |
Proportioning 4：
Mosquito repellent master batch/slices of caprone → drying → screw extruding (blending) → filament spinning component filtering → spinning → quenching
Oil → winding → examine → add bullet → coiling and molding → draw-teisting → to twist → compressing and washing → afterwards to dry → thermal finalization → balance
→ fall bucket → packaging → inspection → finished product.
8 mosquito repellent polyamide fibre of the present invention of embodiment is to the phobotaxis of mosquito
Test method：Using mosquito as test worm, the phobotaxis of mosquito is measured.Experiment glass box used (70cm × 70cm ×
70cm), centre is divided into two Room of A, B with cardboard.Mosquito repellent polyamide fibre and blank polyamide fibre of the present invention are taken, is respectively sleeved in the burning for filling warm syrup
On cup, the sample of mosquito repellent polyamide fibre of the present invention as made from embodiment 7 is placed on A rooms, blank sample is put in B rooms.Mosquito is passed through
The worm channel of putting of yarn lid is put at random in glass square chest, is sealed and is put insect population.It observes mosquito land to tend to, then revolves mid-board
Turn 90 °, observe the taxis of mosquito, mosquitoes is waited to land substantially after 10min, cardboard is restored as former state, to wait mosquitoes basic again
It falls, the mosquito number of two Room of record A, B calculates mosquito repellent rate, and calculation formula is：Mosquito repellent rate=(B rooms mosquito number-A rooms mosquito number)/B
Room mosquito number × 100%.
Test result：Experimental result is shown in Table 1~6.Mosquito repellent polyamide fibre of the present invention has mosquito walks quickly and keeps away effect well, places
After 120 days, still have to mosquito and good walk quickly and keep away effect.Keep off the weight percent of attapulgite<50% or>When 70%, the present invention
Mosquito repellent polyamide fibre walks quickly and keeps away mosquito effect reduction.
1 mosquito repellent polyamide fibre of the present invention of table (lemongrass, the repelling effect of proportioning 1)
2 mosquito repellent polyamide fibre of the present invention of table (lemongrass, the repelling effect of proportioning 2)
3 mosquito repellent polyamide fibre of the present invention of table (lemongrass, the repelling effect of proportioning 3)
4 mosquito repellent polyamide fibre of the present invention of table (peppermint, the repelling effect of proportioning 4)
5 mosquito repellent polyamide fibre of the present invention of table (folium artemisiae argyi, the repelling effect of proportioning 5)
6 mosquito repellent polyamide fibre of the present invention of table (folium artemisiae argyi, the repelling effect of proportioning 6)
Claims (2)
1. a kind of mosquito repellent nylon-6 fiber, which is characterized in that mosquito repellent is made in micro-capsule made from attapulgite and plant mosquito repellent product
Master batch, then mosquito repellent polyamide fibre 6 is made in mosquito repellent master batch and nylon-6 fiber；
Wherein, the plant mosquito repellent product is lemongrass, folium eucalypti, folium artemisiae argyi or peppermint；
In the mosquito repellent polyamide fibre, the weight percent of polyamide fibre 6 is 70~80%, and the weight percent of the mosquito repellent master batch is
20~30%；In the mosquito repellent master batch, the weight percent of attapulgite is 50~70%, plant mosquito repellent product extract
Weight percent is 30%~50%；
The preparation method of the mosquito repellent nylon-6 fiber, includes the following steps：(1) plant mosquito repellent product is crushed, is placed in extraction
In kettle, using 70%~90% ethyl alcohol as entrainer, supercritical CO is adjusted2Fluid temperature (F.T.), pressure；Extraction temperature is 30 DEG C~50
DEG C, extracting pressure is 10MPa~40MPa, and extraction time is 1~3h；Extract liquor is collected, centrifugal concentrating is evaporated extract； (2)
Suitable gelatin is weighed respectively and Arabic gum adds in the aqueous solution of configuration quality score 1%, it is complete in 40~50 DEG C of stirring and dissolvings
Entirely, extract is then added in, with 10000~15000r/min emulsifying rates, 5~15min of high speed shear is water-soluble with 1% acetic acid
Liquid adjusts pH=4.0, and ice water is cooled to 5 DEG C, then adjusts pH=9.0 with 1% sodium hydrate aqueous solution, and 0.2% formaldehyde is water-soluble
Liquid is cured, and obtains extract microcapsule；(3) by attapulgite dispersion in deionized water, ultrasound 1h, quiet after being sufficiently stirred
Upper strata suspension is poured out after putting 10min, the remaining impurity of container bottom is removed, 2-3 times repeatedly, adds in suitable hydrochloric acid in above-mentioned
Suspension after purification is impregnated 1-2 days, is subsequently placed in Rotary Evaporators, and rotary evaporation is placed on vacuum drying chamber drying；So
After be dissolved in absolute ethyl alcohol, extract microcapsule made from addition by mixed liquor rotary evaporation in vacuo, drying, then crushes, be made
Mosquito repellent master batch；(4) it is mosquito repellent master batch/slices of caprone → drying → screw extruding → filament spinning component filtering → spinning → blowing is cold
But oil → winding → examine → add bullet → coiling and molding → draw-teisting → to twist → compressing and washing → afterwards to dry → thermal finalization → it is flat
Weigh → fall bucket → packaging → inspection → finished product.
2. the preparation method of mosquito repellent nylon-6 fiber as described in claim 1, which is characterized in that include the following steps：(1) will
Plant mosquito repellent product passes through supercritical extraction method, and plant mosquito repellent product extract is made；(2) plant mosquito repellent product is extracted
Micro-capsule is made in object；(3) by the suction-operated of attapulgite, mosquito repellent master batch is made with plant mosquito repellent product micro-capsule；(4) it will drive
Mosquito repellent polyamide fibre 6 is made with nylon-6 fiber in mosquito master batch.
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| CN107523897A (en) * | 2017-09-20 | 2017-12-29 | 浙江恒逸石化有限公司 | A kind of preparation method of health care's polyester fiber |
| CN111304773A (en) * | 2020-04-01 | 2020-06-19 | 百事基材料（青岛）股份有限公司 | Easy-to-dye modified polyamide fiber |
| CN114369907B (en) * | 2021-12-30 | 2023-09-01 | 广东宝创环保新材料制品有限公司 | Medical mask special non-woven fabric with antibacterial function |
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| CN103305953A (en) * | 2012-03-16 | 2013-09-18 | 上海荷叶纺织有限公司 | Mosquito-repelling viscose fiber and preparation method thereof |
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